JP6552245B2 - Polishing composition and method for producing polished article - Google Patents

Description

  The present invention relates to a polishing composition and a method for producing a polished article.

  Conventionally, a polishing process using a polishing composition is performed on the surface of a material such as a metal, a semimetal, a nonmetal, or an oxide thereof. As the polishing composition, generally used is a composition containing abrasive grains according to the material of the object to be polished and the purpose of polishing. Patent documents 1-4 are mentioned as technical literature about a constituent for polish containing an abrasive grain.

Unexamined-Japanese-Patent No. 2004-263074 Japanese Patent Application Publication No. 2007-300070 JP, 2011-161570, A JP, 2013-069929, A

  By the way, for example, in the polishing of a magnetic disk substrate, it is required to finish the surface with higher quality for higher capacity, and defect suppression at a level which has not been considered as a problem conventionally is required. Therefore, when the surface after polishing by the polishing composition containing colloidal silica derived from the alkali silicate-containing liquid was analyzed in detail, among the defects detected on the surface after polishing, the fine particles attached to the surface It became clear that the cause was caused by various film-like substances. It has been found that this film-like substance is inevitably contained in the colloidal silica derived from the alkali silicate-containing liquid derived from the raw material of the colloidal silica. Further, it has been found that the constituent material of the film-like substance is a silicate compound that can contain a small amount of alkali metal.

  Unless colloidal silica derived from an alkali silicate-containing liquid (hereinafter also referred to as “silica S”) is used, defects due to adhesion of the film-like substance do not occur. Then, it is possible to replace with silica S and to use the silica particle obtained by the other manufacturing method (The manufacturing method which does not use the alkali-silicate containing liquid as a raw material). However, such silica particles are generally expensive. Further, some silica S have various characteristics (for example, average particle diameter, particle shape, etc.), and some silica particles obtained by other production methods cannot be substituted.

  This invention is made | formed in view of this situation, and it aims at providing the polishing composition which can implement | achieve a higher quality surface using the colloidal silica originating in the alkali silicate containing liquid. . Another object of the present invention is to provide a method for producing a polishing product and a polishing method using the polishing composition. Another related object is to provide a film-like substance adhesion preventing agent for preventing the film-like substance from adhering, a defect reducing method using the film-like substance adhesion preventing agent, and a method for producing a polished article.

  According to this specification, there is provided a polishing composition comprising colloidal silica derived from an alkali silicate-containing solution, and a film-like substance anti-adhesion agent having a silica adsorption rate AS in water of 20% or more. According to a polishing composition containing such a film-like substance adhesion inhibitor (hereinafter also referred to as "inhibitor B"), colloidal silica (silica S) derived from an alkali silicate-containing liquid is used, and a film-like form It is possible to realize a high-quality surface in which defects due to material adhesion are suppressed.

  According to a preferred embodiment of the polishing composition disclosed herein, the film-like substance adhesion preventing agent is a polyoxyethylene having a polyoxyethylene chain and an end group ether-bonded to the end of the polyoxyethylene chain. Including derivatives. According to such a polishing composition, defects due to adhesion of a film-like substance can be effectively suppressed. The polyoxyethylene derivative preferably has 6 to 20 moles of ethylene oxide added in the polyoxyethylene chain. Moreover, it is preferable that the said end group is a hydrocarbon group or a halogenated hydrocarbon group. The terminal group preferably has 1 to 20 carbon atoms.

  The HLB value of the film-like substance adhesion inhibitor is preferably 11 or more. Polishing composition containing the said film-form substance adhesion prevention agent tends to have high dispersibility. Therefore, it is possible to effectively exhibit the polishing action on the object to be polished, and efficiently obtain a high quality surface in which the adhesion of the film-like substance is prevented.

  The polishing composition disclosed herein preferably has a content of the film-like substance adhesion inhibitor of 0.1 mmol / L or more and 5 mmol / L or less. According to such a polishing composition, it is possible to effectively exhibit the polishing action on the object to be polished, and it is possible to efficiently obtain a high-quality surface in which adhesion of a film-like substance is prevented.

  The polishing composition disclosed herein preferably has a pH of 5 or less. According to such a polishing composition, it is possible to effectively exhibit the polishing action on the object to be polished, and it is possible to efficiently obtain a high-quality surface in which adhesion of a film-like substance is prevented.

  The polishing composition disclosed herein typically contains a film-like substance having a thickness of less than 100 nm. Film-like substances of such size are particularly difficult to remove with precision from compositions containing silica S. Therefore, in the polishing composition containing such a film-like substance, it is particularly meaningful to apply the technique disclosed herein to prevent the adhesion of the film-like substance.

  The polishing composition disclosed herein is suitable as a polishing composition for polishing a magnetic disk substrate, for example. In the field of magnetic disk substrates, a surface with fewer defects is required for high capacity and high reliability. Therefore, the magnetic disk substrate can be a preferable application target of the technology disclosed herein.

  The polishing composition disclosed here is suitable as a polishing composition for polishing a glass material. The above-mentioned film-like substance tends to be particularly easy to adhere to the glass material as described later and to be difficult to remove. Therefore, it is particularly meaningful to apply the technique disclosed herein to prevent adhesion of the film-like substance. Among glass materials, application to a glass substrate is preferable, and for example, it is suitable for use in polishing glass substrates such as a glass substrate for a magnetic disk (glass magnetic disk substrate) and a glass substrate for a photomask.

  According to this specification, there are also provided any polishing composition disclosed herein, and supplying the above polishing composition to a polishing object to polish the polishing object. A method of making an abrasive article is provided, including. According to this production method, it is possible to produce an abrasive having a high-quality surface that enjoys the advantages of the use of silica S and is highly suppressed in defects due to adhesion of film-like substances.

  According to this specification, there is also provided a polishing method comprising polishing an object to be polished using any of the polishing compositions disclosed herein. According to this polishing method, it is possible to realize a high-quality surface in which the advantages of using silica S are enjoyed and defects due to adhesion of the film-like substance are highly suppressed.

  According to this specification, there is also provided a method of reducing defects present on a surface after polishing in polishing using a polishing composition containing silica S. The method for reducing defects includes a film-like substance adhesion preventing agent having a silica adsorption ratio AS in water of 20% or more in a polishing composition containing the silica S, and an object to be polished using the polishing composition. Including polishing. According to the defect reduction method, defects present on the surface after polishing can be significantly reduced by the effect of the film-like substance adhesion inhibitor.

  According to this specification, there is also provided a film-like substance adhesion inhibitor (inhibitor B) which prevents the adhesion of the film-like substance contained in the colloidal silica derived from the alkali silicate-containing liquid to the object to be polished. The film-like substance adhesion preventing agent is characterized by a silica adsorption rate AS in water of 20% or more. According to the film-like substance adhesion preventing agent, it is possible to obtain an abrasive with reduced defects caused by the adhesion of the film-like substance.

  According to this specification, the step (1) of polishing the object to be polished with the polishing composition containing silica S, and the polishing with the surface treatment solution containing the film-like substance adhesion preventing agent satisfying the silica adsorption rate AS There is provided a method for producing an abrasive comprising the step (2) of subjecting an object to a surface treatment in this order. According to this manufacturing method, it is possible to obtain an abrasive with reduced defects caused by the adhesion of the film-like substance.

It is a SEM image which shows a film-like substance.

  Hereinafter, preferred embodiments of the present invention will be described. Note that matters other than matters specifically mentioned in the present specification and necessary for the implementation of the present invention can be grasped as design matters of those skilled in the art based on the prior art in this field. The present invention can be implemented based on the contents disclosed in the present specification and common technical knowledge in the field.

<Composition for polishing SB>
The polishing composition disclosed herein includes colloidal silica (silica S) derived from an alkali silicate-containing liquid, and a film-like substance adhesion inhibitor (inhibitor B) having a silica adsorption rate AS of 20% or more in water. And is characterized by including. Hereinafter, the polishing composition containing silica S and the inhibitor B may be described as "polishing composition SB".

  Here, “colloidal silica derived from an alkali silicate-containing liquid” refers to colloidal silica produced using an alkali silicate-containing liquid (for example, sodium silicate-containing liquid starting from silica sand) as a raw material. In general, colloidal silica (silica S) produced by such a method inevitably contains a film-like substance derived from the raw material. Therefore, the above-mentioned film-like material is unavoidably contained in the polishing composition containing silica S unless the intentional and appropriate treatment for excluding the above-mentioned film-like material is performed with high accuracy. That is, the polishing composition disclosed herein typically contains a film-like substance together with silica S. Moreover, when the polishing composition disclosed herein contains a film-like substance, it can be inferred from the fact that the polishing composition contains silica S.

In the art disclosed herein, whether or not the composition contains a film-like substance can be evaluated by the following method. That is, the dispersion sample containing the composition to be evaluated is filtered through a membrane filter with a pore size of 0.2 μm. At this time, the amount of the dispersion sample to be filtered by the membrane filter is set to 30 mg on the basis of the solid content per 1 cm ² of the filtration area of the membrane filter. If the dispersion sample cannot be passed through a membrane filter with a pore size of 0.2 μm, before filtering the dispersion sample with a membrane filter with a pore size of 3 times or more (that is, a membrane filter with a pore size of 0.6 μm or more) in advance. Processing can be performed. As the membrane filter having a pore diameter of 0.2 μm, for example, a polycarbonate membrane filter (trade name “K020A-047A” manufactured by ADVANTEC) can be used.
The dispersion sample is filtered through a membrane filter having a pore size of 0.2 μm, and the residue on the membrane filter is observed with a scanning electron microscope (SEM). Observations are made on randomly selected 12.7 μm × 9.5 μm × 100 fields of view. If it is difficult to distinguish, zoom and check as necessary. And when the presence of a film-like substance is recognized in those visual fields, it is evaluated that the composition contains a film-like substance. When the film-like substance is not present in the 100 fields of view, it is evaluated that the composition does not substantially contain the film-like substance.

  In the technique disclosed herein, the target for evaluating whether or not the film-like substance is contained according to the above method is the polishing composition, as well as the production of the polishing material such as the cleaning solution, surface treatment solution, rinse solution, etc. Any composition that can be used in the process can also be included. In addition, a material that can be used as a raw material for producing such a composition, such as an aqueous dispersion of colloidal silica derived from an alkali silicate-containing liquid, can also be an object of evaluation by the above method.

(Film-like substance)
For example, as shown in FIG. 1, the film-like substance is a minute film (in other words, a thin piece or a thin film) typically having a rectangular shape (specifically, a rectangular shape). The film-like substance is often present in the form of a rectangle, and its thickness L _T is usually less than about 100 nm (typically less than about 50 nm). Usually, the long side length L _L of the film-like substance is about 0.5 μm or more, and the short side length L _S is about 0.1 μm or more. Therefore, depending on the ratio of the long side to the short side, the shape of the film-like substance may be expressed as a strip, a band, or the like.

  When a polishing composition containing such a film-like substance is supplied to the object to be polished, the surface of the object to be polished can come into surface contact with the surface of the film-like substance. At this time, when the surface of the object to be polished is in close contact with the surface of the film-like substance, a state in which the film-like substance is continuously staying at a specific position on the object to be polished, that is, adhesion (sticking) of the film-like substance occurs. The film-like substance adhering to the surface of the object to be polished by such surface contact has a thin and flat shape, and the alkali cleaning liquid or the like can be obtained by a general method such as scrubbing or applying ultrasonic waves. Even if it is washed with water, it remains on the surface of the object to be polished, and as a result, it may cause convex defects. Also, for example, even if the condition of chemical cleaning is made stricter and the film-like substance on the surface of the object to be polished is removed, the film-like substance adheres to the portion of the object to be polished to which the film Since the amount of surface removal by chemical cleaning is smaller compared to the non-adhered part (non-adhered part), it can also cause convex defects. It is one of the main problems to be solved in the art disclosed herein to suppress convex defects (typically, convex defects having a substantially flat shape (such as a tabular shape)) caused by such a film-like substance. is there.

The major axis L _L of the film-like substance is usually 0.5 μm or more. Therefore, a typical shape of the film-like substance mentioned here includes a shape having a thickness of less than 100 nm and a major axis L _L of 0.5 μm or more. The major axis L _L of the film-like substance is typically about 0.7 μm or more, and may be, for example, about 1 μm or more. A film-like substance having a longer diameter L _L (length) that is greater than or equal to a predetermined size tends to have a strong adhesive force because it has a large area that can come into contact with the surface of the object to be polished. Therefore, the application effects of the technology disclosed herein can be exhibited better. The upper limit of the long diameter L _L is not particularly limited, but is usually 5 μm or less, and typically 3 μm or less. When the long diameter L _L is reduced, it becomes increasingly difficult to accurately remove the film-like substance from the polishing composition containing the silica S, and therefore, the significance of application of the technique disclosed herein is increased. The technique disclosed here allows a polishing composition to contain a film-like substance and can effectively prevent adhesion of the film-like substance, so that a film having a major axis L _L of a predetermined value or less. It can be preferably applied to the solid substance.

Minor _{L S} of the film-like material is generally 0.1μm or more, typically at about 0.2μm or more, can be, for example, approximately 0.3μm or more. A film-like substance having a short diameter L _S (width) greater than or equal to a predetermined value tends to have a strong adhesive force because it has a large area that can contact the surface of the object to be polished. Therefore, the application effects of the technology disclosed herein can be suitably exhibited. The upper limit of the minor diameter L _S is not particularly limited, but is usually 1.5 μm or less, and typically 1 μm or less. As the minor diameter L _S becomes smaller, it becomes increasingly difficult to precisely remove the film-like substance from the polishing composition containing silica S, and the application significance of the technology disclosed herein becomes greater. The technology disclosed herein allows the polishing composition to contain a film-like substance and can effectively prevent adhesion of the film-like substance, so that the short diameter L _S is not more than a predetermined value. It can preferably be applied to film-like substances.

When the film-like substance has a rectangular shape, the major axis L _L is taken as the long side. Since the film-like substance does not necessarily have a rectangular shape, in such a case, the longest diameter may be set to the long diameter L _L for convenience. When the film-like substance has a rectangular shape, the short diameter L _S is taken as the short side. In the film-like materials other than rectangular, the longest distance across the length in the direction perpendicular to the major axis L _L may be the minor axis L _S.

The thickness _{L T} of the film-like material, typically 50nm or less, for example, at approximately 30nm or less, typically is approximately 20nm or less. If the thickness L _T of the film-like material is reduced, since the film-like material from the polishing composition containing silica S be accurately removed becomes increasingly difficult, to apply the significance of the art disclosed herein increases . The art disclosed herein, the polishing composition SB may be suitably implemented in a manner that includes a film-like material having the thickness L _T. The lower limit of the thickness L _T is not particularly limited, but is usually about 3 nm or more, for example, 5 nm or more.

Although not particularly limited, the ratio of the major axis L _L to the thickness L _T of the film-like substance (L _L / L _T ) is greater than about 10 and 15 or more (eg, 50 or more, typically 100 or more). Is preferred. Since the film-like substance satisfying the above ratio (L _L / L _T ) is thin and has a large area, it tends to have a strong adhesion to the object to be studied. Therefore, in the polishing composition containing such a film-like substance and polishing using the composition, it is particularly significant to apply the technique disclosed herein.

  It is known that the above film-like substance is generated at least secondary to the production of colloidal silica using an alkali silicate-containing liquid (for example, a sodium silicate-containing liquid) as a raw material. Therefore, the said film-form substance is a component which can be unavoidably contained in the composition containing the colloidal silica obtained by the said manufacturing method at least.

(Silica S)
The polishing composition SB disclosed herein contains colloidal silica (silica S) derived from an alkali silicate-containing solution. The polishing composition SB may contain one type of silica S alone, or may contain two or more types (for example, two or more types having different particle diameters, particle shapes, etc.) in combination. Good.

  The above polishing composition SB typically contains silica S as an abrasive. Here, "include as abrasive grains" means being contained in a mode that can exert the polishing action on the object to be polished. The abrasive grains in the polishing composition SB may be substantially composed of silica S, or may be composed of a combination of silica S and other abrasive grains. Here, that the abrasive grains are substantially composed of silica S means that 95 wt% or more (typically 98 wt% or more) of the abrasive grains is composed of silica S. The same is true for other types of abrasive grains.

  Polishing composition SB disclosed here is not limited to the one containing silica S as abrasive grains. In other words, the polishing composition SB disclosed herein may contain silica S for purposes other than abrasive grains, and silica S as abrasive grains and silica S contained for purposes other than abrasive grains. And both may be included. It is because the said film-form substance may be included in the composition containing silica S regardless of the function of the silica S and the purpose of use. According to the technology disclosed herein, it is possible to suppress defects (for example, convex defects due to the adhesion of the film-like substance) caused by the film-like substance regardless of the function and purpose of use of the silica S.

  Hereinafter, although the aspect which mainly utilizes silica S as an abrasive grain is mainly demonstrated, the technical thought disclosed by this specification is not limited to this aspect.

  The silica S contained in the polishing composition SB disclosed herein may be in the form of primary particles, or may be in the form of secondary particles in which a plurality of primary particles are aggregated. Further, silica S in the form of primary particles and those in the form of secondary particles may be mixed.

  The particle shape of silica S is not particularly limited, and may be, for example, spherical or non-spherical. Specific examples of the non-spherical shape include peanut shape (i.e., shape of peanut shell), wedge shape, shape with projections (e.g., gold palm sugar shape), rugby ball shape, and the like. From the viewpoint of reducing the surface roughness, silica S having a nearly spherical shape can be preferably used.

  The average primary particle diameter D1 of the silica S is not particularly limited, but is preferably 5 nm or more, more preferably 8 nm or more, still more preferably 10 nm or more, for example 12 nm or more, from the viewpoint of polishing efficiency and the like. Moreover, from the viewpoint that a smoother surface can be easily obtained, D1 is preferably 100 nm or less, more preferably 80 nm or less, and even more preferably 50 nm or less. The technique disclosed herein is also preferable in an embodiment using silica S having D1 of 30 nm or less (more preferably 25 nm or less, more preferably less than 25 nm, for example, less than 20 nm) from the viewpoint of easily obtaining a higher quality surface. It can be implemented.

In the technology disclosed herein, the average primary particle diameter D1 of silica S and other particles refers to the average particle diameter based on the BET method. The average primary particle diameter D1 can be calculated from the specific surface area S (m ² / g) measured by the BET method according to the formula D1 (nm) = 2727 / S. The specific surface area can be measured using, for example, a surface area measuring device manufactured by Micromeritex Corporation, a trade name “Flow Sorb II 2300”.

  The average secondary particle diameter D2 of the silica S is not particularly limited, but is preferably 5 nm or more, more preferably 8 nm or more, still more preferably 10 nm or more, for example 12 nm or more, from the viewpoint of polishing rate. Further, from the viewpoint of obtaining a more smooth surface, the above D2 is suitably 200 nm or less, preferably 150 nm or less, more preferably 100 nm or less, and further preferably 80 nm or less. The technique disclosed herein is also preferable in an embodiment using silica S having D2 of 50 nm or less (more preferably 30 nm or less, more preferably less than 25 nm, for example, less than 20 nm) from the viewpoint of easily obtaining a higher quality surface. It can be implemented.

  In the technology disclosed herein, the average secondary particle diameter D2 of silica S and other particles is, for example, model “UPA-UT151” manufactured by Nikkiso Co., Ltd., using an aqueous dispersion of the measurement object as a measurement sample. It can be measured by the dynamic light scattering method used.

  D2 of silica S is generally equal to or greater than D1 (D2 / D1 ≧ 1) and is typically larger than D1 (D2 / D1> 1). Although not particularly limited, it is appropriate that D2 / D1 of silica S is usually in the range of 1.0 to 3.0, from the viewpoint of the polishing effect and the surface smoothness after polishing. The range of 0-2.5 is preferable and the range of 1.0-2.3 is more preferable. From the viewpoint of obtaining higher surface smoothness, silica S having D2 / D1 of 1.0 to 2.0 (more preferably 1.0 to 1.5, for example 1.0 to 1.4) is preferably used. obtain. In addition, D2 / D1 of the silica S used in the Example mentioned later is 1.1-1.4 in all.

  Although not particularly limited, the average value (average aspect ratio) of the major axis / minor axis ratio of silica S is preferably 1.01 or more, more preferably 1.05 or more (for example 1.1 or more). By increasing the average aspect ratio, a higher polishing rate can be achieved. The average aspect ratio of the silica S is preferably 3.0 or less, more preferably 2.0 or less, and still more preferably 1.5 or less from the viewpoint of surface roughness reduction and the like. The polishing composition disclosed herein contains silica S having an average aspect ratio of less than 1.25 (eg, 1.20 or less, typically less than 1.15) by including the film-like substance anti-adherent. Even in the mode of use, convex defects due to adhesion of the film-like substance can be effectively reduced. Therefore, according to this aspect, it is possible to achieve both the reduction of the surface roughness and the reduction of the convex defects at a high level.

  The shape (outer shape) and average aspect ratio of the silica S can be grasped by, for example, observation with an electron microscope. As a specific procedure for grasping the average aspect ratio, for example, using a SEM, a predetermined number (for example, 200) of abrasive particles capable of recognizing the shape of independent particles is the smallest that circumscribes each particle image. Draw a rectangle. For the rectangle drawn for each particle image, the value obtained by dividing the length of the long side (major axis value) by the length of the short side (minor axis value) is the major axis / minor axis ratio (aspect ratio). Calculated as). An average aspect ratio can be obtained by arithmetically averaging the aspect ratios of the predetermined number of particles.

  The density of the silica S is preferably 1.5 or more, more preferably 1.6 or more, and still more preferably 1.7 or more. By increasing the density of silica, the polishing rate can be improved when polishing an object to be polished. From the viewpoint of reducing scratches generated on the surface (surface to be polished) of the object to be polished, silica particles having a density of 2.3 or less are preferable. As the density of the abrasive grains (typically silica), a value measured by a liquid displacement method using ethanol as a displacement liquid can be adopted.

  Silica S in the technology disclosed herein is manufactured using an alkali silicate-containing liquid as a raw material as described above. Such a composition containing silica S (for example, any polishing composition disclosed herein) may contain an alkali metal derived from a raw material (for example, an alkali metal such as Na, K, Li, etc.). A composition comprising silica S may typically comprise Na.

(solvent)
The polishing composition SB disclosed herein typically contains water as a solvent in which the silica S is dispersed (hereinafter, used in the meaning of a medium including a solvent and a dispersion medium). As water, ion exchange water (deionized water), pure water, ultrapure water, distilled water or the like can be preferably used.

  Polishing composition SB disclosed here may further contain an organic solvent (lower alcohol, lower ketone, etc.) that can be uniformly mixed with water, if necessary. Usually, 90 vol% or more of the solvent contained in the polishing composition is preferably water, and more preferably 95 vol% or more (typically 99 to 100 vol%) is water.

(Film-like substance adhesion inhibitor)
The film-like substance adhesion inhibitor (inhibitor B) in the technology disclosed herein is characterized by a silica adsorption rate AS in water of 20% or more. In the following, "silica adsorption rate AS in water" may be simply referred to as "silica adsorption rate AS". The silica adsorption rate AS in this specification is measured by the following method.

[Method of measuring silica adsorption rate AS]
(I) In ion-exchanged water, 73 g / L of colloidal silica (manufactured by JGC Catalysts & Chemicals Co., Ltd., product name “Spherica # 300”) having an average primary particle diameter D1 (specific surface area equivalent particle diameter) of 280 nm is measured. A dispersion X containing 1 mmol / L of a certain film-like substance adhesion inhibitor (inhibitor B) and adjusted to pH 3.0 with sulfuric acid (H ₂ SO ₄ ) and sodium hydroxide (NaOH) is prepared. After the dispersion X was allowed to stand at 25 ° C. for 24 hours, a high-speed cooling centrifuge (manufactured by Beckman Coulter, apparatus name “Avanti HP-301”, rotor name “JA-30.50”, and the following solution Y: The same is applied to the measurement.) Is centrifuged at a temperature of 25 ° C. and a rotational speed of 20000 rpm for 20 minutes, and the supernatant X is taken out. The total organic carbon (TOC) of the supernatant X is measured with a TOC meter (manufactured by Shimadzu Corporation, apparatus name “TOC-5000A”, the same applies to the measurement of the supernatant Y below), and this is defined as X (ppm). .
(Ii) A solution Y adjusted to pH 3.0 is prepared in the same manner as the dispersion X is prepared except that the colloidal silica is not used. The solution Y is allowed to stand at 25 ° C. for 24 hours, and then centrifuged at a temperature of 25 ° C. and a rotational speed of 20000 rpm for 20 minutes using a high-speed cooling centrifuge, and the supernatant Y is taken out. The total organic carbon (TOC) of the supernatant Y is measured by a TOC meter, which is taken as Y (ppm).
(Iii) Based on X and Y obtained by the measurement of the above (i) and (ii), the silica adsorption rate AS is calculated by the following equation: AS = (Y−X) / Y × 100;

The colloidal silica (product name “Spherica # 300” manufactured by JGC Catalysts & Chemicals Co., Ltd.) used in the method for measuring the silica adsorption rate AS is colloidal silica derived from an alkali silicate-containing liquid, and is an inhibitor. It is a measurement reagent which provides a SiO ₂ surface for evaluating the adsorption easiness of B on silica. Therefore, the silica S used in the polishing composition disclosed herein is not limited to the colloidal silica used in the above measurement method. However, utilization of the colloidal silica used in the above measurement method as a component of the polishing composition is not hindered.

Although it does not specifically limit, the reason that the inhibitor B disclosed here can contribute to adhesion prevention of a film-like substance is considered as follows, for example. That is, the silica adsorption ratio AS indicates that the larger the value, the easier the substance is to be adsorbed to silica (SiO ₂ ) in water. Therefore, it can be said that the inhibitor B having a silica adsorption rate AS of 20% or more has a property of being easily adsorbed to the film-like substance in water. The inhibitor B adsorbed on the film-like substance can exert a function of preventing adhesion between the film-like substance and the object to be polished by being interposed between the film-like substance and the object to be polished. It is considered that this effectively prevents the adhesion of the film-like substance to the object to be polished. In particular, when the object to be polished is a glass material such as a glass substrate, the inhibitor B easily adheres to the object to be polished, so that the film B and the object to be polished are adhered to each other by the inhibitor B. It can interfere more effectively. Therefore, the application effects of the technology disclosed herein can be exhibited better.

  The type, composition, and the like of the inhibitor B are not particularly limited as long as the silica adsorption rate AS is equal to or higher than the lower limit value described above. For example, the inhibitor B may be an ionic compound (cationic compound, anionic compound or amphoteric compound) that can be at least partially ionized in water to become a cation or an anion. Further, the inhibitor B may be a nonionic compound. A nonionic compound can be suitably employed as the inhibitor B because a suitable silica adsorption rate AS can be easily obtained. In particular, nonionic compounds can be preferably selected as the inhibitor B used under acidic (for example, pH 5 or less, preferably 4 or less) conditions.

  From the viewpoint of achieving a higher film material adhesion preventing effect, the silica adsorption ratio AS of the inhibitor B is preferably 25% or more, more preferably 50% or more (eg 60% or more, typically 70%) More preferably 80% or more (for example, 90% or more). According to the inhibitor B having a large silica adsorption rate AS, the effect of preventing the adhesion of the film-like substance tends to be exhibited better.

  A suitable example of the inhibitor B disclosed herein is a polyoxyethylene derivative. Here, the polyoxyethylene derivative means a compound containing a polyoxyethylene structure (polyoxyethylene chain). For example, a polyoxyethylene derivative that is a nonionic compound can be suitably employed. Examples of such polyoxyethylene derivatives include polyoxyethylene alkyl ether, polyoxyethylene alkyl aryl ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene fatty acid ester, polyoxyethylene alkylamine Etc.

  When the inhibitor B disclosed herein is a polyoxyethylene derivative, the ethylene oxide (EO) addition molar number of the compound may be 2 or more, and is not particularly limited. Generally, polyoxyethylene derivatives having an EO addition mole number of 4 to 30 are preferred because a suitable silica adsorption rate is easily obtained. Further, from the viewpoint of dispersibility in water, the number of moles of EO added to the polyoxyethylene derivative is preferably 6 to 20, more preferably 8 to 20, and still more preferably 10 to 20. In a preferred embodiment, the inhibitor B having an EO addition mole number of 12 to 20 (more preferably 14 to 20, typically 16 to 20, for example, 18 to 20) can be used.

  When the inhibitor B disclosed here is a polyoxyethylene derivative, the inhibitor B preferably has a hydrophobic group in addition to the polyoxyethylene chain. In a preferred embodiment, the hydrophobic group is attached to the end of the polyoxyethylene chain. According to the structure of the inhibitor B, the effect of preventing the adhesion of the film-like substance tends to be exhibited better. By this, the convex defect resulting from adhesion of a film-like substance can be reduced, and a better surface quality abrasive can be realized.

  Preferable examples of the hydrophobic group include a hydrocarbon group and a halogenated hydrocarbon group. Examples of the hydrocarbon group include an alkyl group, an alkenyl group, an alkadienyl group, an alkatrienyl group, an alkynyl group, a cycloalkyl group, a bicycloalkyl group, a tricycloalkyl group, a cycloalkenyl group, a cycloalkadienyl group, and an aryl group. , An aralkyl group, an alkoxy group and an alkoxyalkyl group. The halogenated hydrocarbon group may be one in which some or all of the hydrogen atoms in the hydrocarbon groups listed above are substituted with halogen atoms such as F, Cl, Br and the like. For example, the inhibitor B in which the hydrophobic group is a hydrocarbon group is preferable. The hydrophobic group is preferably an aliphatic group, and more preferably a chain aliphatic group.

  The number of carbon atoms of the hydrophobic group (for example, alkyl group) is not particularly limited, and may be 1 to 36, for example. The carbon number is usually suitably 4 or more, preferably 6 or more, more preferably 8 or more, for example 10 or more. When the carbon number of the hydrophobic group is increased, the adsorptivity to silica tends to be improved. This is preferable from the viewpoint of preventing the film-like substance from adhering to the object to be polished. The carbon number of the hydrophobic group is usually 32 or less, preferably 28 or less, more preferably 24 or less, still more preferably 22 or less, for example 20 or less. When the carbon number of the hydrophobic group is decreased, the solubility or dispersibility of the inhibitor B in water tends to be improved. This is preferable from the viewpoint of the dispersion stability of the polishing composition containing the inhibitor B. In a preferred embodiment, a polyoxyethylene derivative having 12 to 24 (e.g. 14 to 20) carbon atoms of the hydrophobic group may be employed as the inhibitor B. According to such an inhibitor B, a better film-like substance adhesion preventing effect can be exhibited.

  The technique disclosed here can be preferably implemented in an embodiment in which the inhibitor B is polyoxyethylene alkyl ether (hereinafter, sometimes referred to as POE alkyl ether). As the EO addition mole number of the above-mentioned POE alkyl ether, the EO addition mole number which can be adopted in the above-mentioned polyoxyethylene derivative can be applied. For example, an inhibitor B of 6 to 20 (more preferably 10 to 20, more preferably 12 to 20, more preferably 14 to 20, typically 16 to 20, eg 18 to 20) moles of EO added It can be used. The structure and carbon number of the alkyl group in the POE alkyl ether can be the same as in the case where the hydrophobic group that can be employed in the polyoxyethylene derivative is an alkyl group. For example, the alkyl group is a chain alkyl group having 1 to 20 carbon atoms (typically 8 to 20, preferably 10 to 20, more preferably 12 to 20, and further preferably 14 to 20) (for example, a linear alkyl group). Inhibitor B is preferred.

  The inhibitor B in the art disclosed herein may be any one of the compounds as described above, or may be a mixture of two or more.

  The HLB (Hydrophile-Lipophile Balance) value of the inhibitor B disclosed herein is not particularly limited. From the viewpoint of solubility or dispersibility in water, an inhibitor B having an HLB value of 11 or more can be preferably employed. The HLB value is more preferably 12 or more, still more preferably 13 or more (for example 14 or more), and particularly preferably 15 or more, from the viewpoint of exhibiting the adhesion preventing effect of the film-like substance better. The upper limit of the HLB value of the inhibitor B is not particularly limited, but is usually 19 or less, preferably 18 or less, more preferably 17 or less (for example, 16 or less). The inhibitor B having an HLB value in the range described above tends to exhibit a suitable silica adsorption rate AS, and can preferably exhibit the effect of preventing the film-like substance from adhering to the object to be polished. In addition, when the polishing composition disclosed here contains a plurality of types of inhibitors B having different HLB values, the HLB value is a weighted average (weight basis) of the HLB values of each inhibitor B. .

  The molecular weight of the inhibitor B is not particularly limited, and can be, for example, about 200 to 5,000. From the viewpoint of obtaining a good film adhesion preventing effect, the molecular weight of the inhibitor B is usually 400 or more, preferably 500 or more, more preferably 600 or more, and still more preferably 700 or more (eg, 800 or more). Further, from the viewpoint of polishing efficiency, the molecular weight of the inhibitor B is suitably 4000 or less, preferably 3000 or less, more preferably 2500 or less, and still more preferably 2000 or less (e.g. 1500 or less).

  The content of the inhibitor B in the polishing composition disclosed herein (the total amount of the inhibitors B in the case of containing a plurality of types of inhibitor B) is not particularly limited, and it is desired depending on the purpose of use and mode of use. It can set suitably so that the effect of this may be acquired. In a preferred embodiment, the content of the inhibitor B in the polishing composition can be, for example, 0.001 mmol / L or more, and usually 0.01 mmol from the viewpoint of exhibiting the effect of preventing adhesion of a film-like substance better. / L or more is suitable, preferably 0.1 mmol / L or more, more preferably 0.2 mmol / L or more, and further preferably 0.3 mmol / L or more (for example, 0.5 mmol / L or more). Further, the content of the inhibitor B in the polishing composition can be, for example, 100 mmol / L or less, and from the viewpoint of polishing efficiency etc., usually 10 mmol / L or less, and 5 mmol / L or less. Is preferable, and 3 mmol / L or less is more preferable.

  Although the content is not particularly limited, the content of the inhibitor B with respect to 100 g of silica S can be, for example, 0.01 mmol or more, and is usually 0. 05 mmol or more is suitable, 0.1 mmol or more is preferable, and 0.3 mmol or more is more preferable. Further, the content of the inhibitor B with respect to 100 g of silica S can be, for example, 10 mmol or less, and usually 5 mmol or less is preferable from the viewpoint of polishing efficiency and the like, and 3 mmol or less is preferable. The inhibitor B disclosed herein can exhibit a good film material adhesion preventing effect even in an embodiment in which the content relative to 100 g of silica S is, for example, 1 mmol or less.

(Abrasive grains other than silica S)
The polishing composition SB disclosed herein may contain abrasives other than the silica S. The material and properties of the abrasive grains other than silica S are not particularly limited, and can be appropriately selected according to the purpose of use and usage of the polishing composition. As abrasive grains other than silica S, any of inorganic particles, organic particles, and organic-inorganic composite particles can be used. Specific examples of inorganic particles include silica particles, alumina particles, ceria particles, titania particles, zirconia particles, chromium oxide particles, magnesium oxide particles, manganese dioxide particles, zinc oxide particles, oxide particles such as bengara particles; silicon nitride particles And nitride particles such as boron nitride particles; carbide particles such as silicon carbide particles and boron carbide particles; diamond particles; carbonates such as calcium carbonate and barium carbonate; Specific examples of the organic particles include polymethyl methacrylate (PMMA) particles and poly (meth) acrylic acid particles (here, (meth) acrylic acid is a generic term for acrylic acid and methacrylic acid). And polyacrylonitrile particles. Abrasive grains other than silica S may be used alone or in combination of two or more.

  As abrasive grains other than silica S, inorganic particles are preferable, and particles made of metal or metalloid oxide are particularly preferable. The abrasive grains may be silica particles. Examples of silica particles other than silica S (that is, silica particles other than colloidal silica derived from an alkali silicate-containing liquid; hereinafter also referred to as “silica NS”) include those other than the method using an alkali silicate-containing liquid as a raw material. Colloidal silica (for example, alkoxide method colloidal silica) manufactured by a method, dry method silica (for example, fumed silica), etc. are mentioned.

  Although not particularly limited, as the abrasive grains other than silica S, those satisfying one or more of preferable average primary particle diameter D1, average secondary particle diameter D2 and D2 / D1 in silica S described above are preferably employed. It can.

  Although not particularly limited, the proportion of silica S in the abrasive grains contained in the polishing composition SB disclosed herein is typically 50% by weight or more, preferably 75% by weight or more, and more preferably It is 90% by weight or more, more preferably 95% by weight or more. The technique disclosed here can be preferably implemented in an aspect in which the abrasive grains are substantially composed of silica S. In addition, regardless of the content of the silica S, as long as a film-like substance can be contained, the application effect of the technology disclosed herein can be exhibited. Therefore, in the technique disclosed herein, the proportion of silica S in the abrasive grains contained in the polishing composition is less than 50% by weight, for example, 25% by weight or less, or 10% by weight or less, or 5% by weight or less. Certain embodiments can also be preferably implemented.

(PH)
The pH of the polishing composition SB is not particularly limited. The pH of the polishing composition SB can be, for example, pH 12.0 or less (typically, pH 1.0 to 12.0), and pH 10.0 or less (typically, pH 1.0 to 10.0). ) May be used. In a preferred embodiment, the pH of the polishing composition SB can be pH 7.0 or less (eg, pH 1.0 to 7.0), and pH 6.0 or less (typically pH 1.2 to 6.0). For example, it is more preferable to set it as pH1.2-5.5), and it is further more preferable to set it as pH5.0 or less (for example, pH1.5-5.0). The pH of the polishing composition SB is, for example, pH 4.5 or less (typically, pH 2.0 to 4.5, preferably pH 2.5 to 4.3, more preferably pH 2.5 to 4.0). be able to. The pH can be preferably applied to a polishing liquid (for example, a polishing liquid for polishing) used for polishing a glass material such as a glass magnetic disk substrate. In polishing of a glass material, in order to obtain a more smooth surface, the pH range of the polishing composition SB is more than pH 2.5 (typically, the pH range is more than 2.5 and 4.3 or less, For example, pH can be preferably employed in the range of more than 2.5 and 3.8 or less. In order to adjust the pH, a pH adjustor described later can be used as needed.

(Other ingredients)
The polishing composition SB disclosed herein is a pH adjuster such as an acid or an alkali agent, an oxidizing agent, a chelating agent, a surfactant, a water-soluble polymer, an antibacterial agent, as long as the effects of the present invention are not significantly hindered. You may further contain the well-known additive which can be used for polishing compositions (for example, polishing composition for magnetic disk substrates), such as a rust agent, antiseptic | preservative, and an antifungal agent, as needed. The technology disclosed herein may also be practiced in a mode in which the polishing composition SB is substantially free of additives such as an oxidizing agent, a water-soluble polymer, a surfactant, and a chelating agent. The polishing composition SB having such a composition is suitable, for example, as a polishing composition used in the polishing of a glass material (glass magnetic disk substrate etc.). Polishing composition SB disclosed here may be substantially composed of, for example, silica S and a film-like substance that can be unavoidably contained, a solvent, an inhibitor B, and a pH adjuster.

  Examples of the acid that can be contained in the polishing composition SB include carbonic acid, hydrochloric acid, nitric acid, phosphoric acid, hypophosphorous acid, phosphorous acid, phosphonic acid, sulfuric acid, boric acid, hydrofluoric acid, orthophosphoric acid, pyrroline. Inorganic acids such as acids, polyphosphoric acids, metaphosphoric acids and hexametaphosphoric acids; and organic acids such as organic carboxylic acids, organic phosphonic acids and organic sulfonic acids, but not limited thereto. As an organic acid, a C1-C18 thing is preferable and a C1-C10 thing is more preferable. Specific examples of organic acids include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, enanthic acid, caprylic acid, pelargonic acid, capric acid, lauric acid, myristic acid, palmitic acid, margaric acid, stearic acid, Saturated carboxylic acids such as nicotinic acid; unsaturated carboxylic acids such as crotonic acid, oleic acid, linoleic acid, linolenic acid, ricinolenic acid; oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, maleic acid, fumaric acid, Saturated and unsaturated dicarboxylic acids such as itaconic acid and iminodiacetic acid; hydroxycarboxylic acids such as glycolic acid, lactic acid, malic acid, citric acid, tartaric acid, gluconic acid and mandelic acid; methanesulfonic acid, ethanesulfonic acid and benzene Sulfonic acid, p-toluenesulfonic acid, 10-camphorsulfonic acid, isethion , Acid taurine; methyl acid phosphate, ethyl acid phosphate, ethyl glycol acid phosphate, isopropyl acid phosphate, phytic acid, phosphonic acids such as 1-hydroxyethylidene-1,1-diphosphonic acid; and the like. Preferred acids from the viewpoint of polishing efficiency include inorganic acids such as sulfuric acid and phosphoric acid. By using a carboxylic acid such as maleic acid or citric acid (for example, a polyvalent carboxylic acid having two or more carboxy groups), the effect of the inhibitor B tends to be exhibited better. By using organic acids such as maleic acid, citric acid, and isethionic acid, higher smoothness tends to be realized. Further, for example, in a polishing composition used for polishing a glass material, an acid having a low oxidizing power (for example, an acid having a standard redox potential of 0.5 V or less with respect to a standard hydrogen electrode, specifically, sulfuric acid, citric acid, etc.) Can be preferably employed. The acid may be used in the form of a salt with the acid. The acid salt is not particularly limited, and examples thereof include salts with suitable metals and ammonium. An acid and its salt can be used individually by 1 type or in combination of 2 or more types.

  In the embodiment including the acid, the content of the acid in the polishing composition SB (the total content thereof in the embodiment including a plurality of acids) can be appropriately set so as to obtain a desired pH. Although the content is not particularly limited, the content of the acid can be, for example, 0.1 g / L or more, preferably 0.5 g / L or more, more preferably 1 g / L or more from the viewpoint of polishing rate etc. More preferably, it is 5 g / L or more. In addition, from the viewpoint of storage stability of the polishing composition SB, the content is appropriately 70 g / L or less, preferably 50 g / L or less, for example 30 g / L or less.

  Examples of the alkali agent include alkali metal salts (including hydroxide salts, hereinafter the same), alkaline earth metal salts or ammonium salts. Preferable examples include potassium hydroxide, potassium carbonate, potassium bicarbonate, sodium carbonate, ammonium carbonate, potassium phosphate, potassium hydrogen phosphate, sodium phosphate, sodium hydrogen phosphate, ammonium hydrogen phosphate, potassium citrate, Potassium oxalate, ammonium hydrogen oxalate, potassium tartrate, sodium potassium tartrate, ammonium tartrate, ammonium hydrogen tartrate, potassium bromate, potassium sorbate, potassium chlorate, potassium perchlorate, calcium nitrate, potassium gluconate, potassium succinate, Potassium fluoride, calcium fluoride, ammonium fluoride, potassium periodate, potassium ferricyanide, ammonium acetate, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutyl hydroxide Ammonium and the like. Of these, potassium hydroxide, potassium carbonate, potassium bicarbonate, sodium carbonate, ammonium carbonate, potassium phosphate, potassium hydrogen phosphate, sodium phosphate, sodium hydrogen phosphate, and ammonium hydrogen phosphate are more preferable. Such an alkali agent can be used individually by 1 type or in combination of 2 or more types.

  In the embodiment including the alkaline agent, the content of the alkaline agent (the total content thereof in the embodiment including the plurality of alkaline agents) can be appropriately set so as to obtain a desired pH. Although it does not specifically limit, content of an alkaline agent can be 0.1 g / L or more, for example. The content is preferably 0.5 g / L or more, more preferably 1 g / L or more, and still more preferably 5 g / L or more from the viewpoint of polishing rate and the like. Further, from the viewpoint of storage stability and the like of the polishing composition, the content is suitably 70 g / L or less, preferably 50 g / L or less, for example 30 g / L or less.

  In a preferred embodiment, the above-mentioned acids and alkaline agents can be used in combination so that pH buffering can be exerted. Although not particularly limited, as such a buffer system, for example, a combination of a weak acid such as citric acid and sodium citrate and its strong base salt, a strong acid such as sulfuric acid and ammonium sulfate, and its weak base salt, A combination of these can be used.

  Examples of the oxidizing agent include, but are not limited to, peroxide, nitric acid or a salt thereof, peroxo acid or a salt thereof, permanganic acid or a salt thereof, chromic acid or a salt thereof, and the like. As such an oxidizing agent, one type may be used alone, or two or more types may be used in combination as appropriate. Specific examples of the oxidizing agent include hydrogen peroxide, nitric acid, iron nitrate, aluminum nitrate, peroxodisulfuric acid, periodic acid, bromic acid, perchloric acid, hypochlorous acid, persulfuric acid, and salts thereof (for example, sodium salt) , Potassium salt, ammonium salt) and the like. Examples of preferred oxidizing agents include hydrogen peroxide, iron nitrate, peroxodisulfuric acid and nitric acid. Such an oxidizing agent can effectively act as a polishing accelerator by being typically used in combination with the above-mentioned acid. For example, such an oxidizing agent may be preferably used in a polishing composition used for polishing a metal material (for example, a nickel phosphorous plated magnetic disk substrate).

  In the embodiment including the oxidizing agent, the content of the oxidizing agent in the polishing composition SB (when the plurality of oxidizing agents are included, the total content thereof) may be, for example, 0.01 g / L or more. it can. The content is preferably 0.1 g / L or more, more preferably 0.5 g / L or more from the viewpoint of polishing rate and the like. Further, from the viewpoint of economy and the like, the content of the oxidizing agent is suitably 100 g / L or less, preferably 75 g / L or less, more preferably 60 g / L or less.

  The polishing composition SB disclosed herein can be preferably practiced in a mode in which the polishing composition contains substantially no oxidizing agent. For example, when the polishing object is a silicon wafer, if the polishing composition contains an oxidizing agent, the surface of the polishing object is oxidized by supplying the composition to the polishing object. This is because an oxide film is generated, which may lower the polishing rate. In addition, even when the object to be polished is a glass material (for example, a glass magnetic disk substrate), an oxidizing agent is usually unnecessary. For example, the polishing composition SB that substantially does not contain at least any of hydrogen peroxide, sodium persulfate, ammonium persulfate, and sodium dichloroisocyanurate is preferable. In addition, that polishing composition does not contain an oxidizing agent substantially means not containing an oxidizing agent at least intentionally. Therefore, the molar concentration of the oxidizing agent in the polishing composition is, for example, 0.0005 mol / L or less, preferably 0.0001 mol / L or less, more preferably 0.00001, which is derived from the raw materials and the production process. A polishing composition which inevitably contains an oxidizing agent of mol / L or less, particularly preferably 0.000001 mol / L or less) is the concept of a polishing composition substantially free of the oxidizing agent mentioned herein. Can be included.

  The polishing composition SB disclosed herein may contain a water-soluble polymer. By including the water-soluble polymer, the surface roughness (for example, the surface roughness of the magnetic disk substrate) after polishing with the polishing composition can be further reduced. Examples of water-soluble polymers include cellulose derivatives, starch derivatives, polymers containing oxyalkylene units, polymers containing nitrogen atoms, vinyl alcohol polymers, polymers having sulfonic acid groups, acrylic polymers and the like. Specific examples include hydroxyethyl cellulose, pullulan, random copolymer or block copolymer of ethylene oxide and propylene oxide, polyvinyl alcohol, polyisoprene sulfonic acid, polyvinyl sulfonic acid, polyallyl sulfonic acid, polyisoamylene sulfonic acid. Polystyrene sulfonic acid or a salt thereof, polyacrylic acid or a salt thereof, polyvinyl acetate, polyethylene glycol, polyvinyl pyrrolidone, polyacryloylmorpholine, polyacrylamide and the like. The water-soluble polymers can be used alone or in combination of two or more. The technique disclosed herein can be preferably practiced even in a mode in which the polishing composition SB is substantially free of a water-soluble polymer.

  In the embodiment including the water-soluble polymer, the content of the water-soluble polymer in the polishing composition SB (in the embodiment including a plurality of water-soluble polymers, the total content thereof) is, for example, 0.01 g / L. It can be more than. The content is preferably 0.05 g / L or more, more preferably 0.08 g / L or more, and still more preferably 0.1 g / L or more, from the viewpoint of surface smoothness and the like. Further, from the viewpoint of polishing rate and the like, the content is suitably 10 g / L or less, preferably 5 g / L or less, for example 1 g / L or less.

The polishing composition SB disclosed herein can optionally include a surfactant (typically, a water-soluble organic compound having a molecular weight of less than 1 × 10 ⁴ ). The use of the surfactant can improve the dispersion stability of the polishing composition SB. The surfactant is not particularly limited, and one or more kinds selected from known nonionic surfactants, anionic surfactants, cationic surfactants and amphoteric surfactants can be used. . The polishing composition SB disclosed herein can be preferably practiced even in an embodiment substantially free of a surfactant as an optional component.

  Examples of preservatives and fungicides include isothiazoline compounds, p-hydroxybenzoic acid esters, phenoxyethanol and the like.

(Polishing liquid)
In the art disclosed herein, the polishing composition is typically supplied to the object to be polished in the form of a polishing liquid containing the polishing composition and used for polishing the object to be polished. The polishing liquid may be prepared, for example, by diluting (typically diluting with water) any of the polishing compositions disclosed herein. Or you may use polishing composition as polishing liquid as it is. That is, the concept of the polishing composition in the technology disclosed herein is used as a polishing liquid diluted with a polishing liquid (working slurry) that is supplied to a polishing object and used for polishing the polishing object. Both concentrated liquid (polishing liquid stock solution) are included. Another example of the polishing liquid containing the polishing composition disclosed herein is a polishing liquid prepared by adjusting the pH of the composition.

  The content of the abrasive grains in the polishing liquid is not particularly limited, but is usually 0.01% by weight or more, preferably 0.05% by weight or more, more preferably 0.1% by weight or more, and still more preferably 0.15% by weight or more (eg, 1% by weight or more, typically 3% by weight or more). By increasing the abrasive content, higher polishing rates can be achieved. From the viewpoint of economy, the content is usually 30% by weight or less, preferably 25% by weight or less, and more preferably 20% by weight or less. The content may be 15% by weight or less, for example, 10% by weight or less, and may be 5% by weight or less (further, 2% by weight or less, eg 1% by weight or less). .

(Concentrate)
The polishing composition disclosed herein may be in a concentrated form (that is, in the form of a polishing liquid concentrate) before being supplied to the object to be polished. The polishing composition in such a concentrated form is advantageous from the viewpoints of convenience, cost reduction, etc. during production, distribution, storage and the like. The concentration rate can be, for example, about 2 to 100 times in terms of volume, and usually about 2 to 50 times is appropriate. The concentration ratio of the polishing composition according to a preferred embodiment is, for example, 2 to 10 times.

  Thus, the polishing composition in the form of a concentrated liquid can be used in such a manner that a polishing liquid is prepared by diluting at a desired timing and the polishing liquid is supplied to a polishing object. The dilution can be typically performed by adding the aforementioned solvent to the concentrated solution and mixing. Moreover, when the said solvent is a mixed solvent, you may add and dilute only some components among the structural components of this solvent, and add the mixed solvent which contains those structural components in the amount ratio different from the said solvent. May be diluted. Further, as described later, in a multi-component type polishing composition, a part of the agents may be diluted and then mixed with other agents to prepare a polishing liquid, and a plurality of agents were mixed. Later, the mixture may be diluted to prepare a polishing liquid.

  The content of abrasive grains in the concentrated liquid can be, for example, 50% by weight or less. From the viewpoint of the stability of the polishing composition (for example, the dispersion stability of the abrasive grains), the filterability, etc., usually, the content is preferably 45% by weight or less, more preferably 40% by weight or less . In a preferred embodiment, the abrasive content may be 30% by weight or less, or 20% by weight or less (eg, 15% by weight or less). In addition, the content of the abrasive can be, for example, 0.5% by weight or more, preferably 1% by weight or more, and more preferably, from the viewpoint of convenience and cost reduction in production, distribution, storage, etc. Is 3% by weight or more (for example, 5% by weight or more).

  The polishing composition disclosed herein may be of one-part type or multi-part type such as two-part type. For example, the part A containing some components of the constituents of the polishing composition and the part B containing the remaining components may be mixed and used for polishing a polishing object. Part A and part B may be mixed in advance, may be mixed in the middle of a supply line that reaches the object to be polished, or may be mixed on the surface of the object to be polished or just before that. Although not particularly limited, for example, the polishing composition SB disclosed herein is used for polishing an object to be polished by mixing Part A containing silica S and Part B containing the inhibitor B. Can be configured as follows. Part A can be a dispersion typically containing silica S and a solvent. The part B may be a solution or dispersion containing the inhibitor B and a solvent, and may consist essentially of the inhibitor B.

<Polished object>
The polishing composition disclosed herein can be applied to the polishing of polishing objects having various materials and shapes. The material of the object to be polished is, for example, a metal or semimetal such as silicon, aluminum, nickel, tungsten, copper, tantalum, titanium, stainless steel, or an alloy thereof, and a thin film used for semiconductor wiring using these materials. A glassy material such as quartz glass, aluminosilicate glass, glassy carbon, a ceramic material such as alumina, silica, sapphire, silicon nitride, tantalum nitride or titanium carbide; a compound semiconductor substrate such as silicon carbide, gallium nitride or gallium arsenide Material; resin material such as polyimide resin; etc., but is not limited thereto. Moreover, the grinding | polishing target object comprised with the several material of these may be sufficient. The shape of the object to be polished is not particularly limited. The polishing composition disclosed herein can be preferably applied to polishing a polishing object having a flat surface such as a plate shape or a polyhedron shape.

  The technique disclosed here can be preferably applied to polishing of a glass material. Here, "grinding of the glass material" refers to polishing of the object to be polished in which at least a part of the surface to be polished is made of the glass material, and the whole is made of the glass material In particular, polishing of the glass substrate is included. Examples of the glass material include aluminosilicate glass, soda lime glass, soda aluminosilicate glass, aluminoborosilicate glass, borosilicate glass, quartz glass, and crystallized glass. As examples of crystallized glass, the main crystal phase is spodumene, mullite, aluminum borate crystal, β-quartz solid solution, α-quartz, cordierite, enstatite, celsian, wollastonite, anorthite, forsterite, lithium Examples thereof include metasilicate and lithium disilicate. The polishing composition disclosed herein is suitable for use in polishing a glass substrate such as a magnetic disk glass substrate (glass magnetic disk substrate) and a photomask glass substrate.

  The technology disclosed herein can be preferably applied to the polishing of a glass material containing silicic acid (hereinafter also referred to as "silicic acid-containing glass material"). The film-like substance is a silicate compound that can contain a small amount of an alkali metal as described above. In a glass material containing silicic acid, the film-like substance is particularly easy to adhere, and once attached, the film-like substance is removed. hard. Moreover, since the film-like substance and the silicic acid-containing glass material have such similar compositions, it is difficult to set chemical treatment conditions for removing only the film-like substance without damaging the silicic acid-containing glass material. That is, if the chemical treatment conditions for removing the film-like substance are strict, the surface quality of the silicic acid-containing glass material (polishing object) tends to decrease. Therefore, in the polishing of silica-containing glass materials, it is particularly significant to apply the technology disclosed herein to prevent the adhesion of film-like substances. For example, application to a glass substrate having a surface made of a silicate-containing glass material is preferable, and application to a glass magnetic disk substrate that requires a high level of defect reduction is particularly preferable.

  The polishing composition disclosed herein is preferably applied to the polishing of a magnetic disk substrate because it can highly reduce surface defects (in particular, convex defects having a substantially flat shape (such as a trapezoidal shape)) after polishing. It can be done. For example, it is suitable for use in polishing a glass magnetic disk substrate made of a glass material such as aluminosilicate glass or a magnetic disk substrate (Ni-P substrate) having a nickel phosphorus plating layer on the surface of an aluminum alloy. Application to the polishing of glass magnetic disk substrates is particularly preferred. The aluminosilicate glass here may include those having a crystal structure and those subjected to chemical strengthening treatment. The chemical strengthening treatment may be performed after polishing.

<Polishing method>
The polishing composition SB disclosed herein is particularly suitable for polishing (precision polishing) of an object to be polished. Therefore, this specification provides a method for producing an abrasive, including a polishing step using the polishing composition SB. The polishing object to be polished with the polishing composition SB may be a polishing object obtained through processes such as lapping (rough polishing), grinding, and plating. Although polishing composition SB contains silica S and therefore typically contains a film-like substance, adhesion of the film-like substance to the object to be polished can be suppressed by inhibitor B. In other words, the above-mentioned inhibitor B can function as a harmless agent of the film-like substance that can be contained in the polishing composition SB. Thereby, while enjoying the advantages of using silica S, it is possible to prevent the occurrence of convex defects due to the adhesion of the film-like substance and to realize a higher quality surface. Moreover, according to the manufacturing method of the polishing article including the polishing process using polishing composition SB, the polishing article which has a high quality surface can be manufactured efficiently.

  Polishing composition SB can be particularly preferably used for final polishing of an object to be polished because convex defects can be highly reduced on the surface after polishing. Therefore, according to this specification, a method for producing a polished article including a final polishing step using the polishing composition SB (for example, a method for producing a glass magnetic disk substrate or other magnetic disk substrate) is provided. In addition, final polishing refers to the last polishing process (namely, process which does not perform additional polishing after the process) in the manufacturing process of an object. However, it is acceptable to perform a surface treatment step using a surface treatment liquid described later as a step after the final polishing step using the polishing composition SB.

  The polishing composition SB disclosed herein may also be used in a polishing step upstream of final polishing. Here, the polishing process upstream of the final polishing refers to a pre-polishing process between the rough polishing process and the final polishing process. The preliminary polishing step typically includes at least a primary polishing step, and may further include a second, third,... Polishing step. The polishing composition disclosed herein may be used, for example, in a polishing step performed immediately before final polishing.

  Although not particularly limited, the polishing step using the polishing composition SB can be performed, for example, as follows. That is, a polishing liquid containing any one of the polishing composition SB disclosed herein is prepared. The preparation of the polishing liquid may include preparing the polishing liquid by performing operations such as concentration adjustment (for example, dilution), pH adjustment and the like on the polishing composition. Or you may use the said polishing composition as polishing liquid as it is. Also, in the case of a multi-component polishing composition, to prepare the above-mentioned polishing liquid, mixing the agents, diluting one or more agents before the mixing, and after the mixing Diluting the mixture, etc. can be included.

  Next, the polishing liquid is supplied to the object to be polished and polished by a conventional method. As a polisher, a well-known polisher according to the shape of a grinding | polishing target object and the grinding | polishing objective can be employ | adopted suitably. For example, in the case of polishing a glass substrate, the glass substrate that has undergone the lapping process is set in a polishing machine, and a polishing liquid is supplied to the surface (surface to be polished) of the glass substrate through the polishing pad of the polishing machine. Typically, while supplying the polishing liquid continuously, the polishing pad is pressed against the surface of the glass substrate to relatively move (for example, rotate) the two. The type of polishing pad is not particularly limited. For example, any of non-woven fabric type, suede type, those containing abrasive grains, those not containing abrasive grains, etc. may be used. The use of a polishing pad that does not contain abrasive grains is preferable, and a suede type polishing pad is particularly preferable.

  A rinse treatment may be performed following the completion of the supply of the polishing liquid. This rinse treatment is typically performed by supplying a rinse liquid to the surface to be polished instead of the polishing liquid. The rinse solution is not particularly limited, but, for example, water can be preferably used. Alternatively, a rinse solution may be used which contains the same components as the polishing solution except that it contains no silica S or other solid content.

  In a preferred embodiment, the rinsing liquid used for the rinsing treatment may contain the inhibitor B. Therefore, according to the present specification, the rinsing liquid contains any of the inhibitor B disclosed herein, Is provided with a rinse solution further containing a solvent (eg, water). Moreover, the composition for the rinse liquid preparation containing the said inhibitor B is provided. The rinsing liquid can be preferably used in a mode in which the rinsing liquid is supplied to a polishing object following a polishing liquid containing silica S (a polishing liquid containing the inhibitor B or a polishing liquid not containing the inhibitor B). . With the rinse solution having such a composition, it is possible to prevent the film-like substance in the polishing solution that may remain at the start of the rinse treatment from adhering to the object to be polished. In addition, the film-like substance removed from the object to be polished by the rinsing process can be prevented from reattaching to the object to be polished. Therefore, the use of the above-mentioned rinse liquid can reduce the convex defect by adhesion of a film-like substance.

  In the case where the rinse liquid contains the inhibitor B, the content of the inhibitor B (the total amount thereof when a plurality of types of the inhibitor B is contained) is not particularly limited. For example, the content (concentration) of the inhibitor B that can be applied to the polishing composition SB can also be employed in the rinse solution.

  The pH of the rinse solution is not particularly limited. For example, the pH that can be applied to the polishing composition SB can also be employed in the rinse liquid. For the adjustment of the pH, the same pH adjuster as the polishing composition SB can be used as needed. In a preferred embodiment, the rinse solution may be approximately neutral (e.g., pH 6 to pH 8). The rinse liquid may have a composition substantially composed of the inhibitor B and water.

  The matters disclosed by this specification further include a rinsing method for rinsing a polishing object using a rinsing liquid containing any of the inhibitor B disclosed herein, and polishing including the rinsing treatment. A method and a method of producing an abrasive, and a defect reduction method including the above-mentioned rinse treatment are included.

  The method of producing an abrasive product disclosed herein can further include a polishing step (hereinafter, also referred to as “step (P)”) performed prior to a polishing step using the polishing composition SB. According to the aspect including the step (P), the effect of shortening the time required for the entire polishing step and enhancing the productivity of the abrasive can be realized. Also, by performing the step (P), for example, defects (eg, dent defects) present at the start of the polishing step can be efficiently eliminated. The step (P) may be one polishing step using one type of polishing composition, or may include two or more polishing steps performed using two or more types of polishing compositions in sequence. Good.

  The polishing composition (hereinafter also referred to as “polishing composition (P)”) used in the step (P) is not particularly limited. For example, as the abrasive, any of abrasives other than silica S and silica S exemplified as materials usable for the polishing composition SB can be used. When the polishing composition (P) contains silica S, the silica S may be the same as or different from the silica S contained in the polishing composition SB. The difference between the silica S contained in the polishing composition (P) and the silica S contained in the polishing composition SB is, for example, a difference in one or more of the particle diameter, particle shape, density and other characteristics. obtain.

The average primary particle size D1 _P of the abrasive grains contained in the polishing composition (P) is preferably equal to the average primary particle size D1 _S silica S contained in the polishing composition SB or more. For example, D1 _P / D1 _S can be 1 to 100, and usually 2 to 50 is appropriate. In a preferred embodiment, as the abrasive grains contained in the polishing composition (P), those having a D1 _{P of} about 10 nm to 1000 nm (more preferably 20 nm to 700 nm, more preferably 30 nm to 500 nm) can be preferably employed.

  When the polishing composition (P) contains silica particles as abrasive grains, any of silica S and silica NS can be used as the silica particles. Although not particularly limited, silica particles having an average primary particle diameter D1 of about 10 nm to 1000 nm (more preferably 20 nm to 700 nm, still more preferably 30 nm to 500 nm, for example, 30 nm to 200 nm) of the polishing composition (P) are used. It can preferably be employed as an abrasive. Silica particles having an average primary particle diameter D1 of 1 to 50 times (more preferably 1.5 to 30 times, for example, 2 to 20 times) of silica S contained in polishing composition SB are preferred.

  When the polishing composition (P) contains silica particles as abrasive grains, the shape (outer shape) of the silica particles is not particularly limited, and may be spherical or non-spherical. Specific examples of the non-spherical shape include a peanut shape (that is, a shape of peanut shell), a cocoon shape, a shape with a protrusion (for example, a confetti shape), a rugby ball shape, and the like. The silica particles may be used alone or in combination of two or more of different shapes. Especially, the silica particle which has a peanut shape, a bowl shape, and a shape with a protrusion is preferable, and a silica particle with a protrusion is more preferable.

  When a grinding | polishing target object is a glass material, a ceria, a zirconia, a titania, and a silica are illustrated as an abrasive grain which can be preferably used for polishing composition (P). Of these, ceria and silica are preferable. As ceria, particles having an average primary particle diameter D1 of about 10 nm to 1000 nm (more preferably 30 nm to 700 nm, still more preferably 100 nm to 500 nm) can be preferably used.

  The abrasive grain content in the polishing composition (P) is not particularly limited. For example, the same abrasive content as that of the above-described polishing liquid or concentrate can be applied to the content of abrasives in the polishing composition (P).

  The polishing composition (P) typically contains a solvent for dispersing the abrasive grains as described above. As the solvent, the same solvent as the polishing composition SB can be preferably used.

  The pH of the polishing composition (P) is not particularly limited, and may be, for example, pH 12.0 or less (typically, pH 1.0 to 12.0), and pH 10.0 or less (typically, pH 1 or less). 0 to 10.0). In a preferred embodiment, the polishing composition (P) may have a pH of 9.0 or less (for example, pH 2.0 to 9.0), and pH 8.0 or less (typically pH 2.5 to 8). 0.0, for example, pH 3.0 to 8.0) is more preferable. The pH can be preferably applied in the production of a glass substrate such as a glass magnetic disk substrate. When ceria is used as the abrasive, the pH of the polishing composition (P) can be, for example, pH 3.0 to 9.0, may be pH 4.0 to 8.0, and further, pH 5.0 to 5.0 It may be 7.5. For the adjustment of the pH, the same pH adjuster as the polishing composition SB can be used as needed.

  The polishing composition (P) may contain, if necessary, the same known additive (for example, a water-soluble polymer) as the polishing composition SB. When a water-soluble polymer is included as an additive, the amount used is usually suitably 0.05 g / L to 20 g / L, and preferably 1 g / L to 10 g / L. The art disclosed herein can be preferably practiced in a mode in which the polishing composition (P) is substantially free of an oxidizing agent. The polishing composition (P) having such a composition can be preferably employed, for example, in a mode in which the object to be polished is a glass material (such as a glass magnetic disk substrate). In a preferred embodiment, the polishing composition (P) may be substantially composed of abrasive grains, a solvent, a pH adjuster (for example, an acid), and a water-soluble polymer optionally used.

  The step (P) uses a polishing machine having a polishing pad and supplies a polishing solution containing a polishing composition (P) between the polishing object set in the polishing machine and the polishing pad. It can be preferably implemented in a mode in which the object to be polished and the polishing pad are relatively moved. As a polisher, a well-known polisher according to the shape of a grinding | polishing target object and the grinding | polishing objective can be employ | adopted suitably. The kind of polishing pad used for the step (P) is not particularly limited. For example, any of non-woven fabric type, suede type, those containing abrasive grains, those not containing abrasive grains, etc. may be used. The use of a polishing pad that does not contain abrasive grains is preferable, and a suede type polishing pad is particularly preferable. A rinse treatment may be performed following the completion of the supply of the polishing liquid.

  The film-like substance adhesion inhibitor (inhibitor B) disclosed herein can be preferably used as a component of a polishing composition containing silica S as described above. By including the inhibitor B in the polishing composition containing the silica S, the film-like substance that can be contained in the above composition can be rendered harmless. More specifically, adhesion of the film-like substance to the object to be polished can be prevented, and convex defects caused by the film-like substance can be reduced. Therefore, according to this specification, there is provided a method for detoxifying the film-like substance, wherein the polishing composition containing silica S and the film-like substance contains the inhibitor B.

Surface treatment solution
The inhibitor B disclosed herein can also be preferably used as a component of a surface treatment liquid for treating an object to be polished. Examples of the object to be treated which is the treatment object of the surface treatment liquid containing the inhibitor B (hereinafter also referred to as "surface treatment liquid B") include an object to be polished which may have a film-like substance attached to the surface. As a suitable example of such an object to be polished, polishing was performed using a polishing composition containing silica S (a polishing composition containing an inhibitor B or a polishing composition containing no inhibitor B). A polishing object is mentioned. According to the surface treatment using the surface treatment liquid B, when the surface treatment liquid B contains the inhibitor B, the reattachment of the film-like substance removed from the object to be treated to the object to be polished is suppressed. obtain. As a result, the film-like substance can be efficiently removed from the surface of the object to be polished. Therefore, according to the surface treatment liquid B, convex defects caused by the film-like substance can be effectively reduced in the polished object after the surface treatment.

  Here, the "surface treatment" performed by the surface treatment solution (surface treatment solution B) containing the inhibitor B generally refers to the treatment performed by applying the surface treatment solution to the surface of the object to be polished. It is a concept. The surface treatment here may be a treatment grasped as cleaning, rinsing, polishing, etc. of the polishing object as long as the effect of removing the film-like substance that may exist on the surface of the polishing object from the surface can be exhibited.

  The surface treatment liquid B disclosed herein typically contains a solvent in which the inhibitor B is dissolved or dispersed. As the solvent, those similar to the solvents which can be used for the polishing composition SB can be preferably used. One preferred example of the solvent used for the surface treatment liquid B is water.

  The content of the inhibitor B in the surface treatment solution B (the total amount of the inhibitors B in the case of containing plural types of the inhibitor B) is not particularly limited, and a desired effect is obtained depending on the purpose of use, mode of use, etc. Can be set as appropriate. In a preferred embodiment, the content of the inhibitor B in the surface treatment liquid B can be, for example, 0.001 mmol / L or more, and from the viewpoint of exhibiting the effect of preventing adhesion of a film-like substance better, usually 0. It is suitable to set it as 01 mmol / L or more, 0.1 mmol / L or more is preferable, and 0.3 mmol / L or more (for example, 0.5 mmol / L or more) is more preferable. Further, the content of the inhibitor B in the surface treatment liquid can be, for example, 1000 mmol / L or less, and from the viewpoint of economy, it is usually preferably 500 mmol / L or less, and 100 mmol / L or less. Is more preferred. In a preferred embodiment, the content of the inhibitor B in the surface treatment liquid can be 10 mmol / L or less, and can be 5 mmol / L or less, and further 3 mmol / L or less.

  The surface treatment liquid disclosed herein may include particles. The particles to be included in the surface treatment liquid are not particularly limited, and any of abrasive grains other than silica S and silica S exemplified as materials that can be used for the polishing composition SB can be used. The above particles may be used alone or in combination of two or more. From the viewpoint of improving the surface quality after the surface treatment, it is preferable that the surface treatment liquid does not substantially contain a film-like substance. Therefore, the surface treatment liquid preferably does not contain silica S. In other words, when particles are included in the surface treatment liquid, the particles are preferably selected from particles other than silica S.

  As a suitable example of the particles that can be included in the surface treatment liquid, silica particles other than silica S (silica NS) can be mentioned. The surface treatment liquid having such a composition can effectively remove the film-like substance from the object to be polished by the action of the silica NS by containing the silica NS having a composition similar to the film-like substance. Further, since the surface treatment liquid containing silica NS can be made to have a composition substantially free of the film-like substance, the situation where the film-like substance derived from the surface treatment liquid adheres to the object to be polished can be avoided. Can.

  Silica NS is preferably selected from the group consisting of alkoxide colloidal silica and dry silica. Examples of dry process silica here include silica (fumed silica) obtained by burning a silane compound such as silicon tetrachloride or trichlorosilane in a hydrogen flame, or the reaction between metal silicon and oxygen. The silica produced by Among them, alkoxide silica colloidal silica is preferred as the preferable silica NS. Alkoxide Method Colloidal silica is a colloidal silica produced by a hydrolysis condensation reaction of an alkoxysilane. As the above alkoxysilane, usually, tetraalkoxysilane (for example, tetraethoxysilane, tetramethoxysilane, etc.) is used. Silica NS can be used alone or in combination of two or more. In the surface treatment liquid according to a preferred embodiment, the particles contained in the surface treatment liquid are substantially composed of silica NS.

  When the surface treatment liquid B contains particles, the average primary particle diameter D1, the average secondary particle diameter D2, and D2 / D1 of the particles are not particularly limited. For example, preferable D1, D2 and D2 / D1 in the above-mentioned silica S can be preferably applied also to particles to be included in the surface treatment liquid. Further, when the surface treatment liquid B contains particles, the content of the particles is not particularly limited. For example, the same abrasive content as that of the polishing liquid or the concentrated liquid described above can be applied to the particle content of the surface treatment liquid B.

  The surface treatment liquid B may further contain known additives similar to the polishing composition SB as needed. The technology disclosed herein can also be preferably practiced in the mode in which the surface treatment liquid B is substantially free of an oxidizing agent. The surface treatment liquid B having such a composition can be preferably employed, for example, in a mode in which the object to be polished is a glass material (glass magnetic disk substrate etc.). The surface treatment liquid B disclosed herein is, for example, a composition substantially composed of an inhibitor B and a solvent; a composition substantially composed of an inhibitor B, a solvent and a pH adjuster: the inhibitor B, a solvent And a composition substantially consisting of a surfactant; a composition substantially consisting of an inhibitor B, a solvent, a pH adjuster and a surfactant; and the like.

  The pH of the surface treatment solution B is not particularly limited. For example, the pH that can be applied to the polishing composition SB can also be employed in the surface treatment liquid B. For the adjustment of the pH, the same pH adjuster as the polishing composition SB can be used as needed. In a preferred embodiment, the surface treatment solution B may be substantially neutral (eg, pH 6 to pH 8).

  The surface treatment using the surface treatment solution B can be performed in various modes in which the film-like substance can be removed from the surface of the object to be polished by the treatment.

  As a preferred embodiment of the surface treatment, a polishing machine having a polishing pad is used, and the surface treatment solution B is supplied between the polishing object set in the polishing machine and the polishing pad, and There is an aspect of moving the polishing pad relative to the polishing pad. As a polisher, a well-known polisher according to the shape of a grinding | polishing target object and the grinding | polishing objective can be employ | adopted suitably. The type of polishing pad used is not particularly limited. For example, any of non-woven fabric type, suede type, those containing abrasive grains, those not containing abrasive grains, etc. may be used. The use of a polishing pad that does not contain abrasive grains is preferable, and a suede type polishing pad is particularly preferable. Following completion of the supply of the surface treatment solution B, a rinse treatment with a rinse solution (for example, water) not containing the inhibitor B may be performed.

  As another embodiment of the surface treatment using the surface treatment solution B, an embodiment wherein the surface of the object to be polished is polished with an abrasive tape in the presence of the surface treatment solution B; the surface of the object to be polished in the presence of the surface treatment solution B A mode of cleaning with a wiping tape; a mode of scrub cleaning the surface of the object to be polished in the presence of the surface treatment liquid B with a sponge made of polyvinyl alcohol (PVA) or the like; These treatments may be performed in a state where the polishing object is immersed in the surface treatment liquid B. As another aspect of the surface treatment process, an embodiment in which the object to be polished is immersed in the surface treatment solution B and ultrasonic waves are applied; a mode in which the surface treatment solution B with high pressure is sprayed onto the surface of the object to be polished; These can be performed singly or in combination of two or more. For example, scrubbing and sonication may be performed sequentially or in parallel.

  Although not particularly limited, the surface treatment using the surface treatment solution B is, for example, rinse treatment in a polishing process using a polishing composition containing silica S; following a polishing process using a polishing composition containing silica S Cleaning treatment performed; polishing step performed as the next step of the polishing step using the polishing composition containing silica S; and the like. According to this specification, for example, in the step (1) of polishing the object to be polished with the polishing composition containing silica S, and the surface treatment liquid (surface treatment solution B) containing the inhibitor B, the surface is polished There is provided a method for producing a polished article, which comprises the processing step (2) in this order.

  In the above manufacturing method, the step (1) is the last step of the polishing step using the polishing composition containing silica S (typically, the polishing step using the polishing composition containing a film-like substance) Is preferred. After the step (1), a polishing step using a polishing composition containing no silica S may be further performed. The polishing step performed after step (1) may be performed before step (2) or may be performed after step (2). It is preferable not to arrange another polishing step between the step (1) and the step (2) from the viewpoint of suppressing the expansion of the influence of the film-like substance which can adhere to the surface of the object to be polished in the step (1). In the case where the manufacturing method disclosed herein comprises a polishing step performed after step (1) (preferably after step (2)), the polishing step does not contain silica S, and in step (1) It is preferable to carry out using the polishing composition containing the abrasive grain whose average primary particle diameter is smaller than the used silica S.

  The technique disclosed here can be preferably implemented in a mode in which the surface of the object to be polished is not dried between the end of step (1) and the start of step (2). That is, it can be preferably implemented in a mode in which the surface of the object to be polished is kept wet from the end of the step (1) to the start of the step (2). By this, it is suppressed that the film-like substance which can adhere in a process (1) strongly adheres to the grinding | polishing target object surface, and it exists in the tendency for a film-like substance to be easy to be removed in a process (2). Therefore, an abrasive having a better surface quality can be produced.

<Composition set>
According to this specification, there is provided a set of compositions for producing an abrasive, the set comprising the first composition and the second composition. In the above-mentioned composition for producing an abrasive product, the first composition and the second composition are stored separately from each other, and are typically mixed and used. The set of compositions for producing an abrasive product disclosed herein may further include, as the set contents, a third composition separately stored from the first composition and the second composition.

  The first composition constituting the composition set for manufacturing an abrasive product includes silica S, and preferably further includes a solvent. This first composition is typically a composition comprising a film-like substance. The first composition can be used as it is or diluted with a suitable solvent (for example, water) to prepare a polishing composition.

  The second composition constituting the composition set for manufacturing an abrasive is typically a composition that does not substantially contain a film-like substance. This second composition preferably comprises a pH adjuster. Thus, storing silica S and a pH adjuster separately is advantageous from the viewpoint of storage stability of the first composition. The second composition may further comprise a solvent suitable for dissolving or diluting the pH adjusting agent. When the second composition is in the form of a solution, the solution preferably contains no insoluble matter such as particles. The second composition can be used in the preparation of the polishing composition as it is, or dissolved in an appropriate solvent (for example, water) or diluted with the solvent. For example, the polishing composition can be prepared by mixing the first composition and the second composition by a conventional method. In addition, the second composition may be added to the polishing composition containing the first composition at any time.

  In a preferred embodiment of the set of compositions for producing an abrasive product disclosed herein, the first composition or the second composition can contain the inhibitor B. Both the first composition and the second composition may contain the inhibitor B at the same or different concentrations. Thus, by including the inhibitor B in at least one of the first composition and the second composition, the preparation operation of the polishing composition containing the inhibitor B can be simplified.

  In another preferable embodiment of the above composition set for manufacturing an abrasive, the inhibitor B may be contained in the set content as a third composition stored separately from the first composition and the second composition. Good. The composition set of such a configuration is easy to use because the usage mode and concentration of the inhibitor B are high. The third composition may contain the inhibitor B alone, or may be a solution containing the inhibitor B and a suitable solvent. When the third composition is in the form of a solution, the solution preferably contains no insoluble matter such as particles.

  The third composition may be used for preparing the polishing composition as it is, or dissolved in or diluted with a suitable solvent (eg, water). For example, the polishing composition can be prepared by mixing the first composition, the second composition, and the third composition in a conventional manner. In addition, the third composition is added to the polishing composition containing the first composition (which may be the polishing composition containing the first composition and the second composition, and the same applies in the following) at any timing. It is also good. For example, the third composition may be added to the polishing composition after the supply of the polishing composition containing the first composition to the object to be polished is started. As another use mode, the third composition is used as it is or after being dissolved in an appropriate solvent (for example, water) or diluted with the solvent after the polishing step with the polishing composition containing the first composition. The aspect used for preparation of a surface treatment liquid is mentioned.

Note that the matters disclosed by this specification include the following.
<1> A film-like substance adhesion preventing agent contained in a polishing composition containing colloidal silica derived from an alkali silicate-containing liquid,
Including a film-like substance adhesion preventive agent having a silica adsorption rate AS of 20% or more,
A film-like substance adhesion inhibitor, which reduces defects caused by adhesion of a film-like substance in polishing using the above-mentioned polishing composition.
<2> A step (1) of polishing an object to be polished with a polishing composition containing colloidal silica derived from an alkali silicate-containing solution,
A method for producing a polished article, comprising the step (2) of surface-treating the object to be polished with a surface treatment liquid containing a film-like substance adhesion preventing agent having a silica adsorption rate AS of 20% or more in this order.
<3> The production method according to <2>, wherein the polishing composition in the step (1) contains the film-like substance.
<4> The production method according to <2> or <3>, wherein the surface treatment liquid in the step (2) does not substantially contain the film-like substance.
<5> A surface treatment agent used for a polishing object treated (for example, polished) with a colloidal silica-containing liquid containing colloidal silica derived from an alkali silicate-containing liquid, and the silica adsorption rate AS is 20% or more. A surface treatment agent comprising a film-like substance adhesion inhibitor.
<6> A surface treatment liquid used for a polishing object treated (typically polished) with a colloidal silica-containing liquid containing colloidal silica derived from an alkali silicate-containing liquid, A surface treatment liquid comprising a surface treatment agent and a solvent capable of dissolving or dispersing the surface treatment agent.
<7> A polishing composition used for polishing the polishing object after the step of polishing the polishing object using a polishing composition containing colloidal silica derived from an alkali silicate-containing liquid,
Polishing composition containing the film-form substance adhesion preventing agent whose silica adsorption rate AS is 20% or more, and an abrasive grain (preferably abrasive grains other than the colloidal silica derived from an alkali silicate containing liquid).
<8> A composition (a) and a composition (b) stored separately from each other,
The composition (a) contains colloidal silica derived from an alkali silicate-containing solution,
The composition set for abrasives manufacture which the said composition (b) contains the film-like substance adhesion inhibiting agent whose silica adsorption rate AS is 20% or more.

  The following examples illustrate some of the embodiments of the present invention, but are not intended to limit the present invention to those shown.

The contents of the additives used in the following Examples and Comparative Examples are as follows. The numbers in parentheses indicate the number of moles of ethylene oxide (EO) added to the polyoxyethylene chain.
N1: Polyoxyethylene (20) stearyl ether N2: Polyoxyethylene (20) lauryl ether N3: Polyoxyethylene (6) Isodecyl ether N4: Polyoxyethylene (9) Isodecyl ether N5: Polyoxyethylene (7) Stearyl ether N6: polyoxyethylene (10) behenyl ether N7: polyethylene glycol (weight average molecular weight about 600)
N8: polyoxyethylene (2) sodium lauryl ether sulfate N9: lauryl trimethyl ammonium chloride

  The number of carbons of the alkyl group of the additives N1 to N9 (alkyl chain length; the number of carbons of the alkyl group having the largest number of carbons when having a plurality of alkyl groups), the EO addition mole number, the HLB value, Tables 1 and 2 show the silica adsorption rate AS measured by the above method.

Experimental example 1
<Preparation of polishing composition>
Example 1
An aqueous dispersion containing colloidal silica having an average primary particle diameter D1 of 17 nm, derived from an alkali silicate-containing liquid, sulfuric acid as a pH adjuster, additive N1, and ion-exchanged water are mixed, and the colloidal silica is mixed. A polishing composition having the composition shown in Table 1 was prepared, which contains as abrasive grains. The amount of the aqueous dispersion, pH adjuster and additive used was adjusted so that the concentration of the abrasive grains was 12.6% by weight, the pH was 3.0, and the additive content was 1 mmol / L. .

(Examples 2 to 8)
A polishing composition having the composition shown in Table 1 was prepared in the same manner as in Example 1 except that the pH adjusting agent and additives shown in Table 1 were used.

(Comparative example 1)
A polishing composition having the composition shown in Table 1 was prepared in the same manner as in Example 1 except that the additive N1 was not used.

<Polishing of glass substrate>
Using the polishing compositions of Examples 1 to 7 and Comparative Examples 1 to 3 as they were as polishing liquids, 65 mm (about 2.5 inches) diameter magnetic disk aluminosilicate glass substrates were polished under the following conditions. As the above-mentioned glass substrate, what was pre-polished using a pre-polishing composition containing ceria (CeO ₂ ) abrasive grains having an average primary particle diameter D1 of 300 nm was used.

(Polishing conditions)
Polishing device: Double-sided polishing device manufactured by Speedfam, model "9B-5P"
Polishing pad: Suede pad Polishing pressure: 130 g / cm ²
Upper platen rotation speed: 13rpm
Lower surface plate rotation speed: 40 revolutions / minute Polishing solution supply rate: 15 mL / minute (flow)
Polishing fluid temperature: 25 ° C
Polishing time: 10 minutes

The polished substrate was washed under the following conditions and dried. Then, the following evaluation was performed.
(Washing conditions)
The substrate after polishing is immersed in an alkaline cleaning solution (“CSC-102B” available from Speed Pham Clean System Co., Ltd. diluted 200 times on a volume basis) to which 120 kHz ultrasonic waves are applied. After scrub cleaning with PVA sponge in pure water to which sonic waves were applied, and then immersed in ion-exchanged water to which 950 kHz ultrasonic waves were applied, it was pulled up into an isopropyl alcohol (IPA) atmosphere and dried.

<Evaluation>
(Polishing rate)
The polishing rate was calculated based on the weight difference of the glass substrate before and after polishing and the density of the glass substrate. The results are shown in Table 1 in terms of relative values with 100% of Comparative Example 1.

(Surface roughness)
The surface roughness Ra (nm) of the polished surface was measured using an atomic force microscope (AFM; trade name “D3100 Nano Scope V”, manufactured by Veeco) under the conditions of a measurement region of 1 μm × 1 μm. The results are shown in Table 1 in terms of relative values with 100% of Comparative Example 1.

(Defect assessment)
The surface of the glass substrate according to each example was inspected with an inspection apparatus “Candela OSA7100” manufactured by KLA Tencor, and the location of defects in a predetermined area (area where the radial position from the disk center was 20 mm to 31 mm) was detected. Next, after the glass substrate was re-cleaned under the above-described cleaning conditions, the same region as before the re-cleaning was similarly examined to detect the location of the defect. And the defect detected in the same position as rewashing in the test | inspection after rewashing was counted as a "residual defect". The results are shown in Table 1 in terms of relative values with 100% of Comparative Example 1. The large number of residual defects means that there are many defects due to strong deposits that can not be removed even by rewashing.

  As shown in Table 1, in polishing with a polishing composition containing colloidal silica (silica S) as abrasive grains, according to Examples 1 to 8 using additives N1 to N4, comparative examples containing no additives Compared to 1, it was confirmed that residual defects were significantly reduced. Moreover, according to the polishing composition of Examples 1-8, it became clear that surface roughness can be reduced more, maintaining the polishing rate substantially comparable to the comparative example 1. FIG.

Experimental example 2
<Preparation of polishing composition>
(Examples 9 and 10)
A polishing composition having the composition shown in Table 2 was prepared in the same manner as in Example 1 except that colloidal silica derived from an alkali silicate-containing liquid and having an average primary particle diameter D1 of 12 nm or 25 nm was used as abrasive grains. .

(Examples 11 and 12)
A polishing composition having the composition shown in Table 2 was prepared in the same manner as in Example 1 except that the content of the additive was 0.1 mmol / L or 5 mmol / L.

(Example 13)
A polishing composition having the composition shown in Table 2 was prepared in the same manner as in Example 1 except that a pH adjuster was used so that the pH was 5.0.

(Comparative Examples 2-6)
A polishing composition having the composition shown in Table 2 was prepared in the same manner as in Example 1 except that the additives shown in Table 2 were used.

<Polishing and evaluating glass substrates>
The glass substrates were polished in the same manner as in Experimental Example 1 using the polishing compositions of Examples 9 to 13 and Comparative Examples 2 to 6 as they were in the polishing liquid. After the glass substrate after polishing was washed and dried in the same manner as in Experimental Example 1, the residual defects were evaluated in the same manner. The results are shown in Table 2. Table 2 also shows the evaluation results of Comparative Example 1 in Experimental Example 1.

  As shown in Table 2, according to the polishing compositions of Examples 9 to 13 containing colloidal silica (silica S) as abrasive grains and additive N1, the particle size of these silica S and additive content It was also confirmed that residual defects can be clearly reduced also at pH and pH. The polishing rates in Examples 12 and 13 were lower than those in the other examples.

  On the other hand, the additive N5 and the additive N6 have low dispersion stability of the dispersion X at the time of measuring the silica adsorption rate AS, and the silica adsorption rate AS could not be measured appropriately. In addition, the polishing compositions of Comparative Examples 2 and 3 using these additives N5 and N6 had significantly more residual defects than Comparative Example 1. Further, in Comparative Examples 4 to 6 using the additives N7 to N9 having a silica adsorption rate AS of less than 20%, the effect of reducing the residual defects is not recognized as compared with Comparative Example 1, or the residual defects increase. It was a tendency to.

  Specific examples of the present invention have been described in detail above, but these are merely examples and do not limit the scope of the claims. The art set forth in the claims includes various variations and modifications of the specific examples illustrated above.

Claims (8)

A polishing composition used for polishing a magnetic disk substrate or a photomask substrate, comprising:
Colloidal silica derived from a solution containing an alkali silicate,
A film-like substance adhesion inhibitor having a silica adsorption rate AS of at least 20% in water,
Including
Substantially free of oxidants,
The film-like substance adhesion inhibitor comprises a polyoxyethylene derivative,
The polyoxyethylene derivative has a polyoxyethylene chain having an ethylene oxide addition mole number of 6 to 20, and a hydrophobic group,
The film-like substance adhesion inhibitor has an HLB value of 11 or more,
The polishing composition , wherein a content of the film-like substance adhesion preventing agent is 0.1 mmol / L or more and 5 mmol / L or less . The polyoxyethylene derivative is, possess said polyoxyethylene chain, and a terminal group ether bonded to the terminal of the polyoxyethylene chain,
The polyoxyethylene derivative is, before SL terminal groups a hydrocarbon group or halogenated hydrocarbon group der is, the number of carbon atoms of the end groups Ru 20 der polishing composition according to claim 1. Polishing composition of Claim 1 or 2 whose pH is 5 or less. The polishing composition according to any one of claims 1 to 3 , comprising a film-like substance having a thickness of less than 100 nm. A polishing composition comprising: preparing the polishing composition according to any one of claims 1 to 4 , and supplying the polishing composition to a polishing object to polish the polishing object. Production method. A polishing method comprising polishing an object to be polished using the polishing composition according to any one of claims 1 to 4 . A method of reducing defects present on a surface after polishing using a polishing composition in the polishing of a magnetic disk substrate or a photomask substrate ,
Comprising the step of polishing a workpiece by using the polishing composition,
The polishing composition is
Colloidal silica derived from a solution containing an alkali silicate,
A film-like substance adhesion inhibitor having a silica adsorption rate AS of at least 20% in water,
Including
Substantially free of oxidants,
The film-like substance adhesion inhibitor comprises a polyoxyethylene derivative,
The polyoxyethylene derivative has a polyoxyethylene chain having an ethylene oxide addition mole number of 6 to 20, and a hydrophobic group,
The film-like substance adhesion inhibitor has an HLB value of 11 or more,
The defect reduction method , wherein the content of the film-like substance adhesion inhibitor in the polishing composition is 0.1 mmol / L or more and 5 mmol / L or less . A method for producing a polished article by polishing a magnetic disk substrate or a photomask substrate,
Polishing the object to be polished with a polishing composition containing colloidal silica derived from an alkali silicate-containing solution;
Wherein the step of treating the surface of the polishing target surface treatment solution containing the full Irumu matter adhesion inhibitor and (2) in this order,
The polishing composition is substantially free of an oxidizing agent,
The film-like substance adhesion preventing agent prevents adhesion of a film-like substance contained in colloidal silica derived from an alkali silicate-containing liquid to an object to be polished, and has a silica adsorption rate AS of 20% in water. That's it,
The film-like substance adhesion inhibitor comprises a polyoxyethylene derivative,
The polyoxyethylene derivative has a polyoxyethylene chain having an ethylene oxide addition mole number of 6 to 20, and a hydrophobic group,
The film-like substance adhesion inhibitor has an HLB value of 11 or more,
Content of the said film-like substance adhesion prevention agent in the said composition for grinding | polishings is a manufacturing method of the polished article which is 0.1 mmol / L or more and 5 mmol / L or less .