JP5286940B2 - Slurry feeder - Google Patents

Description

  The present invention relates to a slurry supply apparatus for supplying a slurry, which is a mixed polishing liquid, to a chemical mechanical polishing (CMP) apparatus for planar processing of a semiconductor substrate surface in semiconductor manufacturing.

  2. Description of the Related Art In recent years, a CMP method as a microfabrication technique for high integration and high performance of a semiconductor device includes a mixed polishing liquid (hereinafter referred to as a slurry) in which a plurality of polishing stock solutions having different components are mixed, and an object to be polished. Is a polishing method in which the chemical action between the two and the mechanical action of the abrasive grains are combined, and the planarization of the interlayer insulating film, the formation of the metal plug, the embedded metal wiring type in the semiconductor manufacturing apparatus process, particularly in the multilayer wiring forming process It is an indispensable process.

  As a polishing apparatus used in this CMP, a disk-shaped polishing surface plate having a polishing cloth affixed to the surface, and a plurality of wafers that hold one surface of the wafer to be polished and abut the other surface of the wafer against the polishing cloth A wafer holding head and a head driving mechanism for rotating the wafer holding head relative to the polishing surface plate are provided, and polishing is performed by supplying a slurry containing abrasive grains between the polishing cloth and the wafer.

  Slurries are usually abrasive dispersions (mechanical polishing components) such as metal oxides, chemical polishing components comprising an oxidizing agent such as hydrogen peroxide or an alkali such as KOH, a dispersion aid, a pH adjuster, a diluent, etc. Contains. In the CMP method, it is extremely important to maintain the accuracy of the mixing ratio and supply amount of a plurality of polishing stock solutions such as abrasive dispersions having different slurry components and hydrogen peroxide, and to prevent aggregation and sedimentation. In addition, in order to stabilize the polishing rate and improve the accuracy of flattening, the particle size or particle size distribution of the abrasive grains in the slurry supplied to the flattening step must be stable, and other impurities and foreign matters can be prevented from being mixed. Is also an important factor. As dispersion aids, organic substances such as surfactants and organic acids are often used. Here, the fact that the concentration of a chemical polishing component such as an oxidizing agent is stable is also an important factor for improving the flattening accuracy.

  Moreover, since the pH of the abrasive dispersion and slurry is neutral, the composition sufficiently allows the growth of aerobic microorganisms. Although the preparation of the slurry and the operation of supplying the slurry to the polishing apparatus are continuously performed, it is inevitable that aerobic microorganisms are present in the abrasive dispersion. When microorganisms reach the polishing apparatus, the wafer polishing performance is adversely affected. In addition, with the passage of time, on the inner wall of the supply line of the abrasive dispersion liquid, and the supply line to the polishing apparatus of the slurry after mixing a plurality of polishing stock solutions such as abrasive dispersion liquid and hydrogen peroxide having different components, It has been confirmed that microorganisms adhere and propagate and partially form a lump. In particular, there is a tendency for aerobic microorganisms to locally adhere, multiply and agglomerate at the bent portions of the abrasive dispersion supply line and the slurry supply line. Further, when a resin material such as PFA (perfluoroalkyl copolymer) is used for the piping of each supply line, the above tendency becomes more prominent.

  As described above, when microorganisms adhere to the inner wall portion of the abrasive dispersion supply line and propagate and become partially agglomerated, the flow resistance of the abrasive dispersion supply line increases, This results in a decrease in the feed rate of the grain dispersion. Furthermore, the mixing ratio of the abrasive dispersion and the hydrogen peroxide solution varies, making it difficult to control to a predetermined component ratio.

  Furthermore, when a flow meter is used, the accuracy of flow rate measurement due to the adhesion of microorganisms decreases, and it becomes difficult to control the flow rate to a predetermined component ratio. In addition, when a mixer is used, microorganisms adhere to the mixing promoting member and the inner wall and propagate, and uniform mixing cannot be performed in the mixer. In addition, when microorganisms adhere to the inner wall of the slurry supply line and grow, the flow resistance increases with respect to the flow of the slurry, resulting in a decrease in the amount of slurry supplied to the polishing equipment, and the accuracy of the supply amount. Can't keep up.

  The adhesion and propagation of microorganisms in the abrasive dispersion supply line and the slurry supply line increase with the use time of the slurry supply apparatus, and there is a risk that the flow path may be blocked, particularly at the bent portion of the supply line. . For this reason, it becomes difficult to control to a predetermined mixing ratio and to make the supply amount of slurry to the polishing apparatus constant.

  In addition, when a part of the microbial lump is peeled off as small pieces or particles due to the adhesion or propagation of microorganisms, and this reaches the polishing apparatus as a foreign substance, it has a serious adverse effect on the polishing performance of the wafer. It will be different.

  In order to solve the above-mentioned problems caused by aerobic microorganisms, a bactericide is conventionally added to the abrasive dispersion, but it is in a situation where no aerobic microorganisms can be eliminated. For this reason, the following is known, in which a slurry supply device is provided with an abrasive dispersion supply line and a part of the slurry supply line provided with microbial contamination prevention means such as heating and cooling unit means.

An apparatus for supplying a polishing fluid containing a CMP slurry material to a polishing apparatus, the first storage means storing a first polishing fluid, and the second storing a second polishing fluid. Storage means, means for mixing the first polishing fluid and the second polishing fluid, the first storage means, the second storage means, and the mixing means from any of these storage means Cooling of the polishing fluid, heating by microwave irradiation, provided in any part of the piping for feeding the polishing fluid to the means and the piping for feeding the polishing fluid obtained by mixing, It is provided with a means for preventing microbial contamination by irradiation of cytotoxic electromagnetic waves and / or sound waves (for example, Patent Document 1).
JP 2003-197576 A

  However, what is described in Patent Document 1 described above always quickly grasps and confirms the presence / absence of microorganisms in the polishing fluid, the tendency of microorganisms to propagate, and the actual effects of driving the microorganism contamination prevention means. I can't. For this reason, there is a problem in stable polishing of the wafer in the polishing apparatus. Further, the microorganism contamination preventing means is always driven regardless of the presence or absence of microorganisms in the polishing fluid. For this reason, even if the microorganisms are not present in the polishing fluid, the microorganism contamination preventing means is driven, and there is a problem in energy saving.

  The present invention solves the above-described conventional problems, and an object thereof is to provide a slurry supply apparatus that can always maintain stable polishing in a polishing apparatus.

The slurry supply apparatus of the present invention comprises a microorganism detecting means for detecting microorganisms in any part from a supply line of a polishing stock solution to a supply line to a polishing apparatus for a slurry that is a mixed liquid of the plurality of polishing stock solutions ,
A cleaning means for cleaning at least a part of the polishing stock solution from the supply line to the supply line to the polishing apparatus for the slurry, which is a mixed solution of the plurality of polishing stock solutions, includes a detection value of microorganisms by the microorganism detection means. Based on the above, the at least a part of the polishing stock solution from the supply line to the supply line to the polishing apparatus of the slurry that is a mixed solution of the plurality of polishing stock solution is washed with pure water, after washing with pure water,
A tetramethylammonium hydroxide (TMAH) liquid is supplied to at least a part of a supply line from the supply line of the polishing stock solution to a polishing apparatus for slurry, which is a mixed polishing stock solution of the plurality of polishing stock solutions, and is supplied to the supply line. After being discharged for a period of time, hydrogen peroxide water is supplied and discharged for a predetermined time in the supply line.
A slurry supply apparatus in which at least a part from the supply line of the polishing stock solution to the supply line to the polishing apparatus for slurry, which is a mixed liquid of the plurality of polishing stock solutions, is an abrasive dispersion supply line made of a resin material . Is.

According to the slurry supply apparatus of the present invention, it is possible to always maintain stable polishing in the polishing apparatus. In addition, the cells of microorganisms attached and propagated by the TMAH solution can be dissolved, and further, the detachment of the microorganisms by the reaction between the TMAH solution and the hydrogen peroxide solution can be promoted, so that it can be reliably removed and washed.

1st invention is equipped with the microorganisms detection means which detects microorganisms in any site | part from the supply line of polishing stock solution to the supply line to the polishing apparatus of the slurry which is a mixed liquid of the said several polishing stock solution , The said grinding | polishing A cleaning means for cleaning at least a part from the supply line of the stock solution to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing apparatus, based on the detection value of microorganisms by the microorganism detection means, At least a part of the polishing stock solution from the supply line to the slurry supply line to the polishing apparatus, which is a mixed solution of the plurality of polishing stock solutions, is washed with pure water, washed with pure water, and then the polishing stock solution At least part of the supply line from the supply line to the polishing apparatus for slurry, which is a mixed polishing stock solution of the plurality of polishing stock solutions, includes tetramethylammonium hydroxide. (TMAH) liquid is supplied, stays in the supply line for a predetermined time and is discharged, and then supplies hydrogen peroxide water, stays in the supply line for a predetermined time and discharges, and supplies the polishing stock solution from the supply line. The slurry supply apparatus is an abrasive dispersion supply line in which at least a part of the slurry, which is a mixed liquid of the polishing stock solution, reaches a supply line to the polishing apparatus .

By supplying the TMAH solution after washing with pure water, the TMAH solution can directly contact and infiltrate the microorganism, so that the cells of the microorganism can be dissolved and sterilized in a shorter time, and the TMAH solution is supplied. Then, by staying in the supply line for a predetermined time, the TMAH liquid, which is an organic strong alkaline substance, is sufficiently in contact with the microorganisms that adhere to and propagate on the inner wall even in the bent part of the supply line, and a part of which is agglomerated. It can penetrate and sterilize and sterilize the cells of microorganisms more reliably. The change of pH to the alkali side by the supply of TMAH solution causes the microorganisms to be negatively charged, and the inner wall of the particle dispersion supply line made of resin material This also causes physical detachment of microorganisms due to the electrical repulsive action of the TMAH liquid. After the TMAH liquid is retained for a predetermined time and discharged, hydrogen peroxide water is supplied and retained in the supply line for a predetermined time. Then, the TMAH liquid which is a strong alkaline substance adhering to and remaining on the inner wall of the supply line and the hydrogen peroxide solution react and foam, and the microorganisms dissolved by the TMAH liquid are separated from the inner wall and sterilized on the inner wall of the supply line. Can be promoted more.
In addition, when microorganisms are detected by the microorganism detecting means, it is possible to respond quickly so as not to adversely affect the polishing apparatus. Therefore, it is possible to always maintain stable polishing in the polishing apparatus.
In addition, it is possible to prevent a change in flow rate due to an increase in flow resistance in the polishing fluid supply path due to the growth of microorganisms, and to stabilize the mixing ratio. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.
In addition, the cells of microorganisms that have adhered and propagated by tetramethylammonium hydroxide (TMAH) solution should be dissolved, and the removal of microorganisms by the reaction between the TMAH solution and hydrogen peroxide solution should be promoted to ensure removal and washing. Can do. Therefore, it is possible to prevent a change in flow rate due to an increase in flow resistance in the polishing fluid supply path due to the propagation of microorganisms, and to stabilize the mixing ratio. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.
In addition, tetramethylammonium hydroxide solution, which is an organic strong alkali substance, sufficiently contacts and penetrates microorganisms that have adhered to and propagated on the inner wall at the bent part of the supply line and partly become agglomerated. Microbial cells can be lysed and sterilized.
Also, the tetramethylammonium hydroxide solution, which is a strong alkaline substance that remains attached to the microorganisms on the inner wall of the supply line, reacts with the hydrogen peroxide solution to foam, and the microorganisms dissolved by the tetramethylammonium hydroxide solution from the inner wall It is possible to further promote peeling and sterilization of the inner wall of the supply line.

  According to a second invention, in the first invention, the microorganism detection means is provided at a plurality of portions from the supply line of the polishing stock solution to the supply line of the slurry, which is a mixed liquid of the plurality of polishing stock solutions, to the polishing apparatus. A slurry supply device characterized by the above.

  Thereby, in the supply line from the polishing stock solution supply line to the polishing apparatus for the slurry, which is a mixed solution of the plurality of polishing stock solutions, a site where microorganisms are present or a breeding site can be specified.

  According to a third invention, in the first invention, the polishing stock solution or the slurry is microorganisms from a plurality of portions from the supply line of the polishing stock solution to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing apparatus. The slurry supply device is characterized in that it is led out by a detection means.

  Thereby, in the supply line from the supply line of the polishing stock solution to the polishing apparatus for the slurry, which is a mixed solution of the plurality of polishing stock solutions, the number of microorganism detecting means is reduced and the site where the microorganisms are present or the breeding site is specified. Can do.

  According to a fourth aspect of the present invention, there is provided the slurry supply apparatus according to any one of the first to third aspects, further comprising an informing unit for informing a detection value by the microorganism detecting unit.

  Accordingly, the presence / absence of microorganisms and the number of microorganisms in the supply line from the polishing stock solution supply line to the polishing apparatus for slurry, which is a mixed solution of the plurality of polishing stock solutions, are constantly grasped and promptly corresponding to this. Treatment can be performed.

  According to a fifth aspect of the present invention, in any one of the first to fourth aspects, at least a part of the polishing stock solution from a supply line to a supply line to a polishing apparatus for slurry, which is a mixed solution of the plurality of polishing stock solutions, is provided. The slurry supply apparatus includes a sterilizing unit that sterilizes microorganisms and drives the sterilizing unit based on detection of microorganisms by the microorganism detecting unit.

  Accordingly, it is possible to prevent the discharge of microorganisms to the polishing apparatus, to prevent a change in flow rate due to an increase in flow resistance in the polishing fluid supply path due to the propagation of microorganisms, and to stabilize the mixing ratio. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.

A sixth invention provides the abrasive dispersion liquid supply according to any one of the first to fifth inventions, wherein the TMAH liquid, the hydrogen peroxide solution, and the pure water are supplied from the opposite direction (reverse direction) to the flow of the abrasive dispersion liquid. The slurry supply device is supplied to the line and flows .

Thus, during cleaning, abrasive dispersion, TMAH solution, hydrogen peroxide, a container for receiving the purified water can also Rukoto more to simplify the overall structure by replacing.

Example 1
Hereinafter, the slurry supply apparatus of Example 1 of this invention is demonstrated, referring FIGS. FIG. 1 is a basic configuration diagram of a slurry supply apparatus according to a first embodiment of the present invention, FIG. 2 is a basic configuration diagram of a microorganism detecting means, and FIG. 3 is a first step at the time of cleaning for discharging an abrasive dispersion by supplying pure water. FIG. 4 is a configuration diagram of the slurry supply apparatus showing the state of the second step at the time of cleaning to supply the TMAH liquid, and FIG. 5 is a configuration at the time of cleaning to discharge the TMAH liquid by supplying nitrogen gas. FIG. 6 is a configuration diagram of the slurry supply apparatus showing the state of the third step, FIG. 6 is a configuration diagram of the slurry supply apparatus showing the state of the fourth step at the time of cleaning for supplying hydrogen peroxide, and FIG. FIG. 8 is a block diagram of the slurry supply apparatus showing the state of the fifth step during cleaning for discharging hydrogen water, and FIG. FIG. 9 shows the present invention. It is a basic configuration diagram of another slurry feeder.

  In FIG. 1, first, the basic configuration of the slurry supply apparatus will be described. A predetermined amount of polishing stock solution 2 is stored in the abrasive dispersion container 1, and nitrogen gas is dispersed from the nitrogen gas supply line 3 through the on-off valve 4 in the abrasive dispersion container 1. Pressurize the upper surface of the liquid 2. An abrasive dispersion supply pipe 6 is provided in the abrasive dispersion container 1 and communicates with the abrasive dispersion supply line 7. The nitrogen gas supply line 3 and the abrasive dispersion liquid supply line 7 are fixed to the detachable member 5 and configured to be detachable from the abrasive dispersion container 1. The abrasive dispersion 2 is a slurry stock solution for slurry containing fine abrasive particles such as silica, ceria, alumina, zirconia, and manganese dioxide. The abrasive dispersion supply pipe 6 may be configured integrally with the abrasive dispersion supply line 7.

The abrasive dispersion 2 is supplied to the mixed storage container 11 through the on-off valve 8 and the three-way switching valve 10 of the abrasive dispersion supply line 7. The abrasive dispersion supply line 7 is installed with a plurality of bent portions 9 in the mounted state. A slurry 12 which is a mixed polishing liquid of abrasive dispersion 2 and a hydrogen peroxide solution and pure water described later is stored in the mixed storage container 11.

A hydrogen peroxide solution (H ₂ O ₂ ) 14 as a polishing stock solution is stored in the hydrogen peroxide solution container 13, and nitrogen gas is supplied from the nitrogen gas supply line 15 through the opening / closing valve 16 into the hydrogen peroxide solution container 13. The upper surface of the hydrogen peroxide solution 14 is pressurized. A supply pipe 18 is provided in the hydrogen peroxide solution container 13 and communicates with a hydrogen peroxide solution supply line 19. Further, the nitrogen gas supply line 15 and the hydrogen peroxide solution supply line 19 are fixed to the detachable member 17 and configured to be detachable from the hydrogen peroxide solution container 13. The hydrogen peroxide solution 14 is supplied to the mixed storage container 11 through the open / close valve 20 of the hydrogen peroxide solution supply line 19.

  Pure water which is a polishing stock solution for dilution is supplied from the pure water supply line 21 to the mixed storage container 11 through the pure water branch line 22 and the open / close valve 23. A circulation line 24 is formed in the mixed storage container 11 to promote mixing in the mixed storage container 11 by driving a pump 25 and prevent sedimentation of abrasive grains.

  The slurry 12 is supplied from the mixed storage container 11 to the slurry mixed storage container 28 through the slurry supply line 26 and the on-off valve 27 by a drop pressure, and a predetermined amount of the slurry 29 is stored. A circulation line 30 is formed in the slurry mixing storage container 28, and the mixing is promoted in the slurry mixing storage container 28 by driving the pump 31, and the settling of abrasive grains is prevented. The slurry 29 is supplied to the polishing apparatuses 34 and 37 by driving the slurry supply lines 32 and 35 connected to the circulation line 30 and the pumps 33 and 36.

  A predetermined amount of tetramethylammonium hydroxide liquid 39 (hereinafter referred to as a TMAH liquid) is stored in a TMAH liquid container 38, and a TMAH liquid supply line 40 opened in the TMAH liquid container 38 is provided with a three-way switching valve. 41, an on-off valve 42, a three-way switching valve 43, and a cleaning liquid supply line 44 are connected to the three-way switching valve 10. The TMAH solution 39 is an organic strong alkali substance, and is prepared by diluting a TMAH stock solution to a concentration of 25 percent with ultrapure water.

  Nitrogen gas is pressurized from the nitrogen gas supply line 45 through the on-off valve 46 to pressurize the upper surface of the TMAH liquid 39 in the TMAH liquid container 38. A branch line 47 branched from the nitrogen gas supply line 45 is connected to the TMAH liquid supply line 40 via an on-off valve 48.

  A predetermined amount of hydrogen peroxide solution 50 is stored in the hydrogen peroxide solution container 49, and a hydrogen peroxide solution supply line 51 opened in the hydrogen peroxide solution container 49 is connected to the three-way switching valve 41. Nitrogen gas is pressurized from the nitrogen gas supply line 52 through the on-off valve 53 to pressurize the upper surface of the hydrogen peroxide solution 50 in the hydrogen peroxide solution container 49. A branch line 54 branched from the nitrogen gas supply line 52 is connected to a hydrogen peroxide solution supply line 51 via an on-off valve 55.

  A branch line 56 branched from the pure water supply line 21 connects pure water to the three-way switching valve 10 via an on-off valve 57.

  Further, in the basic configuration of FIG. 1, each of the abrasive dispersion supply line 7 and the circulation lines 24 and 30 is provided with a microorganism detecting means 200 and a sterilizing means 300 located on the downstream side of the microorganism detecting means 200. It is.

  FIG. 2 is a basic configuration diagram of the microorganism detecting means 200. The glass cell 203 has a pair of opposed thin film electrodes 201a and 201b, and a measurement cell 202 is installed so as to protect the thin film electrodes 201a and 201b. Then, the current detection resistor 204 and the low voltage power source 205 are connected in series from one terminal, and the abrasive dispersion liquid 2 that is the microorganism detection target liquid is supplied from the abrasive dispersion liquid supply line 7 from the inflow port 206. It becomes the structure discharged | emitted from the outflow port 207. FIG. Moreover, the computer 208, the controller 208a, and the alerting | reporting means 208b are provided.

  A detection line 209 branched from the abrasive dispersion supply line 7 is connected to the inflow port 206. Further, the detection line 209 includes an on-off valve 210 and a three-way switching valve 211, and a cleaning liquid supply line 212 is connected to the three-way switching valve 211.

  Here, the basic operation of the microorganism detecting means 200 in the example provided in the abrasive dispersion supply line 7 will be described. First, the on-off valve 210 is opened, and the abrasive dispersion liquid 2 is supplied from the detection line 209 through the inlet 206 via the three-way switching valve 211 to fill the measurement cell 202. When the inside of the measurement cell 202 is filled with the abrasive dispersion 2, the on-off valve 210 is closed.

  Next, when the low voltage power supply 205 is turned on and a voltage is applied between the thin film electrodes 201a and 201b, microorganisms in the abrasive dispersion 2 sequentially move to a high electric field portion between the gaps of the thin film electrodes 201a and 201b by dielectrophoresis. Then, it is concentrated in a high electric field portion between the gaps of the thin film electrodes 201a and 201b. At this time, the impedance Z between the thin film electrodes 201a and 201b can be calculated from the voltage V applied to the entire circuit, the voltage Vo applied to the current detection resistor, and the current detection resistor 204 having a known value. From this change in impedance Z, the number of microorganisms in the sample can be measured. In the calculation method, as a first step, data entered in the arithmetic unit 208 is calculated by the following equation. That is, the current I flowing through the entire circuit is calculated from the value obtained by dividing the voltage Vo applied to the current detection resistor 204 by the current detection resistor RL.

  I = Vo / RL The value obtained by dividing the voltage V applied to the entire circuit by the detected current value I is the impedance Z of the entire circuit expressed by the following equation.

  Z = V / I As the second step, since the impedance Z of the entire circuit is a parallel circuit of the impedance ZT of the microorganism and the impedance ZE of the electrode, the measured value or the microorganism when the blank solution not containing the microorganism is passed By calculating an initial value that is considered that the concentration of microorganisms by the dielectrophoresis hardly starts immediately after the energization of the sample to be included, and calculating the impedance of the electrode by the following equation, the impedance ZT of the microorganism can be calculated.

  1 / Z = 1 / ZT + 1 / ZE In addition, since the electric field in the vicinity of the thin film electrodes 201a and 201b becomes strongest by applying a voltage for dielectrophoresis, the thin film electrodes 201a and 201b become electric field concentration portions in the present invention, and microorganisms Is electrophoresed near the thin film electrodes 201a and 201b where the electric field is concentrated. The number of microorganisms is input from the arithmetic unit 208 to the controller 208a that controls the entire electrical signal.

  Further, an electric signal is sent from the arithmetic unit 208 to the sterilizing unit 300 and the notifying unit 208b through the controller 208a. The notifying means 208b is configured to notify the detected value of the number of microorganisms by a screen, sound, or the like, and to issue an alarm when the detected value increases from a predetermined number of microorganisms.

  The film thickness of the thin film electrodes 201a and 201b in the present invention is about 5 nm. Since the film thickness of 5 nm is very small compared to the distance of 100 μm between the thin film electrodes 201a and 201b and the microorganism to be detected, the thin film electrodes 201a and 201b are two-dimensional with virtually negligible thickness. It can be considered as an electrode having only a general spread. Therefore, as already described, the boundary between the portion of the measurement electrode where the electrode is in close contact on the glass substrate 203 and the portion where the glass substrate 203 is exposed is expressed as an end line.

  Since the film thickness of the thin film electrodes 201a and 201b in the present invention is as thin as about 5 nm, the electric field is most concentrated on the portion sandwiched between the end lines of the two thin film electrodes 201a and 201b as shown in FIG. Here, when a high-frequency AC voltage is applied to the thin-film electrodes 201a and 201b, the microorganisms in the measurement cell 202 have the most intense and non-uniform portion due to their dielectric properties due to the action of the AC electric field generated thereby. That is, it migrates to the electric field concentration part. Here, the AC voltage is not only a sine wave but also a voltage that changes the direction of the flow at a substantially constant period, and the average value of the currents in both directions is equal.

  After detecting the presence / absence of microorganisms and the number of microorganisms, the on-off valve 210 is temporarily closed, and pure water or chemical liquid cleaning liquid not containing microorganisms is passed through the cleaning liquid supply line 212, the three-way switching valve 211, the detection line 209, and the inlet 206. Supply for a predetermined time, fill the measurement cell 202 and discharge from the outlet 207. Thereby, the thin-film electrodes 201a and 201b, the measurement cell 202, the detection line 209, the inflow port 206, and the outflow port 207 are washed to reliably remove microorganisms. After this cleaning operation, the on-off valve 210 is opened again, the abrasive dispersion 2 is supplied from the inflow port 206 from the detection line 209 via the three-way switching valve 211, and fills the measurement cell 202 to detect microorganisms. It is. During the cleaning operation using the cleaning liquid, an operation of calculating (zero point correction) the initial value of the microorganism detecting means 200 in a state that does not contain any microorganisms (blank) may be performed.

The microorganism detection operation and the washing operation in the microorganism detection means 200 are repeated as one cycle (for example, 3 to 5 minutes). The on-off valve 210 and the three-way switching valve 211 are controlled by the controller 208 a.

  In the example provided in the abrasive dispersion supply line 7, the basic operation of the microorganism detection unit 200 has been described, but the basic operation of the microorganism detection unit 200 provided in each of the circulation lines 24 and 30 is the same. . The microorganism detection means 200 provided in the circulation line 24 is configured such that the slurry (mixed polishing liquid) 12 in the slurry mixed storage container 11 is supplied from the inlet 206 and discharged from the outlet 207. Further, the microorganism detection means 200 provided in the circulation line 30 is configured such that the slurry (mixed polishing liquid) 29 in the slurry mixed storage container 28 is supplied from the inlet 206 and discharged from the outlet 207.

  In addition, the site | part which provided the microorganisms detection means 200 is not limited to the said structure, For example, you may provide in each of the slurry supply lines 26, 32, and 35. FIG.

  Although not shown in the drawings, the microorganism detection means 200 removes abrasive grains from the particle dispersion 2 or the slurry 12, 29, which is a mixed polishing liquid, by a centrifugal separation means or the like, and then detects microorganisms from the inlet 206. It is preferable to supply as a target liquid.

  Further, the sterilizing unit 300 operates according to an instruction from the control unit when the presence of microorganisms is detected. Sterilization is performed by irradiating ultraviolet rays from an ultraviolet irradiation unit attached in the sterilization means 300, and microorganisms are killed. Although the sterilizing means 300 is used, in the present embodiment, it is used not only for bacteria but also for widely killing all microorganisms. When microorganisms are not detected, the sterilization means 300 is not given an instruction for ultraviolet irradiation from the microorganism detection means 200 and the controller 208a in order to avoid wasting power by irradiating unnecessary ultraviolet rays. The sterilizing means 300 has a function of suppressing the increase of microorganisms or killing the microorganisms, and irradiates the slurry, which is the particle dispersion 2 or the mixed polishing liquid, with ultraviolet rays while adjusting the intensity thereof. is there. The sterilizing means 300 is not limited to ultraviolet irradiation, and may be other means such as heating to a predetermined temperature.

  Next, the operation of creating the slurry and supplying it to the polishing apparatuses 34 and 37 will be described with reference to FIG. In a state where the slurry mixing storage container 11 is empty, a predetermined pressure of nitrogen gas is applied from the nitrogen gas supply line 3 by opening the on-off valve 4 on the upper surface of the abrasive dispersion 2 that is the polishing stock solution in the abrasive dispersion container 1. In addition, an amount of abrasive dispersion 2 corresponding to the mixing ratio in the slurry is added to the abrasive dispersion supply line 7 through the abrasive dispersion supply pipe 6, the open on-off valve 8, and the three-way switching valve 10. To the slurry mixed storage container 11.

  After closing the on-off valve 4, the on-off valve 16 is opened on the upper surface of the hydrogen peroxide solution 14, which is a polishing stock solution in the hydrogen peroxide solution container 13, and a predetermined pressure of nitrogen gas is applied from the nitrogen gas supply line 15. Thus, an amount of the hydrogen peroxide solution 14 corresponding to the mixing ratio in the slurry is supplied from the hydrogen peroxide solution supply line 19 into the slurry mixture storage container 11 through the open on-off valve 20. Further, after closing the on-off valve 16, the on-off valve 23 is opened, and pure water which is a polishing stock solution for dilution corresponding to the mixing ratio in the slurry from the pure water supply line 21 and the pure water branch line 22 is mixed with slurry. Supply into the container 11. Each of the polishing stock solutions is supplied into the slurry mixed storage container 11, the pump 25 of the circulation line 24 is driven, and a predetermined amount is stored as the slurry 12 uniformly mixed by flow and agitation in the slurry mixed storage container 11. .

  The slurry 12 stored in a predetermined amount in the slurry mixed storage container 11 is supplied to the slurry mixed storage container 28 from the slurry supply line 26 by opening the on-off valve 27. The slurry 29 in the slurry mixing and storing container 28 circulates in the circulation line 30 by driving the pump 31, and is further supplied from the slurry supply lines 32 and 35 to the polishing apparatuses 34 and 37 by driving the pumps 33 and 36.

  The on-off valve 27 is controlled to be replenished by reducing the amount of the slurry 29 in the slurry mixing storage container 28.

  Furthermore, when the slurry 12 in the slurry mixed storage container 11 becomes empty, the above operation is repeated to store the slurry 12 in the slurry mixed storage container 11.

  During the operation of preparing the slurry and supplying it to the polishing apparatuses 34 and 37, as described above, the microorganism dispersion means 2 provided in each of the abrasive dispersion supply line 7 and the circulation lines 24 and 30 allows the abrasive dispersion 2 or Microorganisms in the slurry 12, 29 are detected. First, the on-off valve 210 is opened, and the abrasive dispersion 2 and the slurry 12 and 29 are supplied from the detection line 209 through the inlet 206 through the three-way switching valve 211 to fill the measurement cell 202. When the inside of the measurement cell 202 is filled with the abrasive dispersion 2 or the slurry 12, 29, the on-off valve 210 is closed for a predetermined time to detect microorganisms.

  When so-called microorganisms in which the impedance Z between the thin film electrodes 201a and 201b does not change are not detected, this is notified by the notification means 208b. Further, the sterilizing means 300 continues the operation of the normal slurry supply apparatus while the ultraviolet irradiation is stopped.

  In the process of continuing the operation of the slurry supply device, for example, when the microorganism detection means 200 provided in the abrasive dispersion supply line 7 detects a predetermined number of microorganisms, this is notified by the notification means 208b. Further, the sterilizing means 300 provided on the downstream side of the microorganism detecting means 200 irradiates the abrasive dispersion 2 passing therethrough with ultraviolet rays to kill the microorganisms. Thereby, the flow of microorganisms to the downstream area of the sterilization means 300 can be prevented.

  According to the detection level of the number of microorganisms in the predetermined range of the microorganism detection means 200, the irradiation intensity of ultraviolet rays necessary for killing the microorganisms in the sterilization means 300 is changed to kill the microorganisms even if the number of microorganisms varies. be able to. The effect of killing microorganisms by the sterilizing means 300 provided in the abrasive dispersion supply line 7 can be confirmed by detecting microorganisms by the microorganism detecting means 200 provided in each of the circulation lines 24 and 30.

  Further, when a predetermined number of microorganisms in the slurry 12, 29 are detected by the microorganism detection means 200 provided in each of the circulation lines 24, 30, this is notified by the notification means 208b. Further, the sterilization means 300 provided on the downstream side of the microorganism detection means 200 irradiates the slurry 12 and 29 passing therethrough with ultraviolet rays to kill the microorganisms.

  Although the sterilization means 300 is provided on the downstream side of the microorganism detection means 200, a plurality of microorganism detection means 200 may be provided on the downstream side and the upstream side in the vicinity of the sterilization means 300. In this case, microorganisms can be detected by the upstream microorganism detection means 200, and the sterilization effect of the sterilization means 300 can be confirmed by the downstream microorganism detection means 200 after passing through the sterilization means 300.

In Examples 1 two information, the microbial detection unit 200 has a plurality of supply lines of the polishing stock solution at the site leading to the feed line to the slurry of the polishing apparatus is a mixture of the plurality of polishing stock solution one It may be one. For example, the microorganism detecting means 200 may be provided here if it is possible to identify the most easily mixed or propagated microorganism. Further, the microorganism detecting means 200 may be provided in the circulation line 30 located upstream immediately before the polishing apparatuses 34 and 37.

  As described above, in the embodiment of the present invention, a microorganism that detects microorganisms in any part from the supply line of the polishing stock solution to the supply line of the slurry that is a mixed liquid of the plurality of polishing stock solutions to the polishing apparatus. It has a detecting means.

  Thereby, microorganisms in the slurry supply line that is a mixed liquid of the plurality of polishing stock solutions can always be continuously detected from the polishing stock solution supply line, and when the microorganisms are detected by the microorganism detection means 200, This makes it possible to quickly respond such as stopping the polishing apparatus, driving a sterilizing means for killing microorganisms, and cleaning for removing microorganisms. Therefore, it is possible to provide a slurry supply apparatus that can perform stable polishing.

  Further, the plurality of portions from the polishing stock solution supply line to the supply line to the polishing apparatus for the slurry, which is a mixed solution of the plurality of polishing stock solutions, are provided with microorganism detection means, so that the plurality of the polishing stock solution supply lines can be used. In the supply line of the slurry, which is a mixed liquid of the polishing stock solution, to the polishing apparatus, it is possible to identify a site where microorganisms are present or a breeding site.

  Furthermore, presence of microorganisms in the supply line from the supply line of the polishing stock solution to the polishing apparatus for slurry, which is a mixed liquid of the plurality of polishing stock solutions, is provided by providing notification means for reporting the detection value by the microorganism detection means. The level of the number of microorganisms can always be reliably grasped, and prompt treatment corresponding to this can be performed.

  In addition, a sterilization unit that sterilizes microorganisms is provided at least in a part from the supply line of the polishing stock solution to the supply line of the slurry, which is a mixed liquid of the plurality of polishing stock solutions, to the polishing apparatus. Based on the detection, the sterilizing means is driven.

  This stabilizes the polishing of the wafer by preventing the discharge of microorganisms to the polishing apparatus, and prevents the change in flow rate due to the increase in flow resistance in the polishing fluid supply path due to the growth of microorganisms, thus stabilizing the mixing ratio. Can be achieved. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.

  In the process of continuously operating the slurry supply device, there is a case where the microorganism detecting means 200 detects a continuous increasing tendency of microorganisms. This is because there is a possibility that microorganisms are attached and propagated in any part from the supply line of the polishing stock solution to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing apparatus.

When microorganisms adhere and propagate, there is a possibility that the fluctuation of the mixing ratio of a plurality of polishing stock solutions or the amount of slurry supplied to the polishing apparatus will change, which will adversely affect the polishing performance of the polishing apparatus.
For this reason, it is necessary to remove attached and propagated microorganisms.

  For this reason, when the number of microorganisms detected by the microorganism detection means 200 is a predetermined value or more, or when microorganisms are continuously detected for a long period of time, the microorganisms that have adhered and propagated when the increasing tendency of the number of microorganisms is confirmed for a certain period of time. Perform cleaning to remove. This cleaning means and each step during cleaning will be described in order with reference to FIGS. 3 to 8 by taking as an example the case of removing microorganisms in the abrasive dispersion supply line 7.

  The removal of microorganisms and the cleaning operation are performed within a time until the slurry 12 in the slurry mixed storage container 11 becomes empty after the slurry 12 is created in the slurry mixed storage container 11. Supply of the slurry 12 and 29 to 34 and 37 is in a continuous state.

Figure 3 shows the state of the first step at the time of cleaning with pure water supply is in a state to discharge the abrasive dispersion 2 of abrasive dispersion liquid in the supply line 7, in FIG. 3, the same portions as FIG. 1 Are given the same numbers and their explanation is omitted. The difference from FIG. 1 is that the abrasive dispersion container 1 is moved apart at the part of the detachable member 5 and the receiving container 58 for receiving the abrasive dispersion 2 discharged from the abrasive dispersion supply pipe 6 is positioned. It is a configuration. In addition, the solid line arrow in a figure shows the flow of pure water.

Pure water is supplied from the pure water supply line 21 into the abrasive dispersion supply line 7 through the branch line 56, the open on-off valve 57, and the three-way switching valves 43 and 10. Pure water flows through the on-off valve 8 with the abrasive dispersion supply line 7 open and the abrasive dispersion supply pipe 6, thereby receiving the abrasive dispersion 2 in the abrasive dispersion supply line 7 and discharging it to the container 58. At the same time, the inside of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 are once cleaned with pure water. When the inside of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 is replaced with pure water, and when a predetermined amount of pure water has flowed into the receiving container 58, the open / close valve 57 is closed to supply pure water. Stop. At this time, the open / close valve 42 of the related flow path is closed, and each of the three-way switching valves 43 and 10 controls the flow path in the direction indicated by the solid line arrow in the figure.

Figure 4 shows a state of the second step during cleaning supplies TMAH solution 39 into abrasive dispersion liquid supply line in the 7, 4, the same portions as FIG. 1, 3 are denoted by the same number Description Is omitted. The difference from FIGS. 1 and 3 is that a receiving container 59 for receiving the TMAH liquid discharged from the abrasive dispersion supply pipe 6 is located. In addition, the solid line arrow in a figure shows the flow of TMAH liquid, and the broken line arrow shows the flow of nitrogen gas.

  As described above, a predetermined amount of the TMAH liquid 39 is stored in the TMAH liquid container 38, and the TMAH liquid supply line 40 opened in the TMAH liquid container 38 includes the three-way switching valve 41, the on-off valve 42, the three-way switching valve 43, the cleaning liquid. It is connected to the three-way switching valve 10 via a supply line 44. At this time, the on-off valve 8 is opened, the on-off valves 48, 57 related to the flow path of the TMAH liquid 39 are closed, and each of the three-way switching valves 41, 43, 10 flows in the direction indicated by the solid line arrow in the figure. The road is controlled.

  The on-off valve 46 is opened from the nitrogen gas supply line 45 and the supply pressure of nitrogen gas is applied to the upper surface of the TMAH liquid 39 in the TMAH liquid container 38. The TMAH liquid 39 in the TMAH liquid container 38 is pushed out to the TMAH liquid supply line 40, and passes through the three-way switching valve 41, the open on-off valve 42, the three-way switching valve 43, the cleaning liquid supply line 44, and the three-way switching valve 10. It flows into the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6. As a result, the pure water in the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 is pushed out and replaced with the TMAH liquid 39. Pure water and TMAH liquid 39 flow out from the abrasive dispersion supply pipe 6 to the receiving container 59.

When the abrasive dispersion liquid supply line 7 and the abrasive dispersion liquid supply pipe 6 are replaced with the TMAH liquid 39, the on-off valves 46 and 42 are closed to stop the supply of the TMAH liquid 39 and the abrasive dispersion liquid. The TMAH liquid is retained and held in the supply line 7 and the abrasive dispersion supply pipe 6 for a predetermined time (for example, 5 to 10 minutes). At this time, in the process in which the TMAH liquid which is an organic strong alkaline substance is in contact with the microorganisms which have adhered and propagated to the inner walls of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6, the cells of the microorganisms are dissolved. Sterilize. As a result, the TMAH liquid 39, which is an organic strong alkali substance, sufficiently contacts and permeates the microorganisms that adhere to and propagate on the inner wall of the supply line having a bent portion, and that are partially agglomerated. Cells can be lysed and sterilized. In addition, the microorganisms are negatively charged due to the change in pH to the alkali side due to the supply of the TMAH solution, and the microorganisms are electrically repelled by the inner wall of the particle dispersion supply line 7 and the abrasive dispersion supply tube 6 made of a resin material. Physical delamination also occurs. The TMAH solution 39 is not particularly limited, but is used after being diluted with ultrapure water to a concentration of 25%. It is used as the mainstream of developer in semiconductor factories and can be shared as a whole semiconductor manufacturing facility.

  As described above, by discharging the abrasive dispersion 2 from the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 and cleaning with pure water, the abrasive dispersion supply line 7, the abrasive The components of the abrasive dispersion 2 are removed from the surface of the microorganisms that have adhered and propagated on the inner wall and the inner wall of the particle dispersion supply pipe 6, and the TMAH solution 39 directly contacts and penetrates the microorganisms. Can be dissolved and sterilized.

Incidentally, abrasive dispersion liquid supply line within 7, pure water abrasive dispersion liquid in the supply pipe 6, extruded by supplying the TMAH solution 39, but so as to replace the TMAH solution 39, Ri by the nitrogen gas supply abrasive dispersion liquid supply line within 7 after draining the purified water abrasive dispersion liquid in the supply pipe 6, may be supplied to TMAH solution.

Figure 5 shows a state of the third step during washing discharging the TMAH solution 39 of abrasive dispersion liquid in the supply line 7 by the nitrogen gas supply, 5, 1, 4 and the same place the same number The description is omitted. In addition, the broken line arrow in a figure shows the flow of nitrogen gas. After the TMAH liquid is retained and held in the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 for a predetermined time, the on-off valve 46 and the on-off valve 57 are closed, the on-off valve 42, the on-off valve 48, and the on-off valve 8 is opened. The three-way valve 41,43,10 are those that controls the flow path in the flow direction of the nitrogen gas as shown in FIG. The nitrogen gas is supplied from the nitrogen gas supply line 45 to the branch line 47, the opening / closing valve 48, the three-way switching valve 41, the opening / closing valve 42, the three-way switching valve 43, the three-way switching valve 10, and the cleaning liquid supply line 44. 7 and supplied into the abrasive dispersion supply pipe 6. As a result, the TMAH liquid 39 staying in the cleaning liquid supply line 44, the abrasive dispersion supply line 7, and the abrasive dispersion supply pipe 6 is discharged to the receiving container 59 through the opening / closing valve 8.

Figure 6 shows a state of the fourth step during cleaning supplies hydrogen peroxide to the abrasive dispersion liquid supply line within 7, 6, 1, 5 and the same portion is denoted by the same numbers Description is omitted. The difference from FIGS. 1 and 5 is that the receiving container 60 for receiving the hydrogen peroxide solution discharged from the abrasive dispersion supply pipe 6 is located. In the figure, solid arrows indicate the flow of hydrogen peroxide water, and broken arrows indicate the flow of nitrogen gas.

As described above, a predetermined amount of hydrogen peroxide solution (H ₂ O ₂ ) 50 is stored in the hydrogen peroxide solution container 49, and the hydrogen peroxide solution supply line 51 opened in the hydrogen peroxide solution container 49 has three sides. The three-way switching valve 10 is connected via a switching valve 41, an on-off valve 42, a three-way switching valve 43, and a cleaning liquid supply line 44. At this time, the on-off valve 8 is opened, the on-off valves 55 and 57 related to the flow path of the hydrogen peroxide solution 50 are closed, and each of the three-way switching valves 41, 43, and 10 is in the direction indicated by the solid arrow in the figure. The flow path is controlled.

  The on-off valve 53 is opened from the nitrogen gas supply line 52, and the supply pressure of nitrogen gas is applied to the upper surface of the hydrogen peroxide solution 50 in the hydrogen peroxide solution container 49. The hydrogen peroxide solution 50 in the hydrogen peroxide solution container 49 is pushed out to the hydrogen peroxide solution supply line 51, and the three-way switching valve 41, the open on-off valve 42, the three-way switching valve 43, the cleaning liquid supply line 44, and the three-way switching. It flows to the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 through the valve 10. Further, it flows out from the abrasive dispersion supply pipe 6 to the receiving container 60 through the on-off valve 2.

  At the stage where the abrasive dispersion liquid supply line 7 and the abrasive dispersion supply pipe 6 are filled with the hydrogen peroxide solution 50, the on-off valves 53 and 42 are closed to stop the supply of the hydrogen peroxide solution 50, The hydrogen peroxide solution 50 is retained and held in the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 for a predetermined time (for example, 5 to 10 minutes).

In this case, the foamed by reaction abrasive dispersion liquid supply line 7, the inner wall of the abrasive dispersion liquid in the supply pipe 6, TMAH solution 39 and hydrogen peroxide 50 is a strong alkaline substance adhering residual microorganisms, which By this, it is possible to further promote the separation of the microorganisms dissolved by the TMAH solution from the inner walls of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 and the sterilization of the inner walls of the supply line.

  The hydrogen peroxide solution 50 is used in a semiconductor factory and can be shared as a whole semiconductor manufacturing facility.

Figure 7 shows a state of the fifth step during cleaning with pure water supply is in a state of discharging the hydrogen peroxide solution 50 in the abrasive dispersion liquid in the supply line 7, 7, and FIG. 1, 6 The same parts are denoted by the same reference numerals and the description thereof is omitted. In addition, the solid line arrow in a figure shows the flow of pure water.

  Pure water is supplied from the pure water supply line 21 into the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 through the branch line 56, the open on-off valve 57, and the three-way switching valves 43 and 10. The pure water flows through the on-off valve 8 and the abrasive dispersion supply pipe 6 that are opened in the abrasive dispersion supply line 7, and thereby the hydrogen peroxide solution 50 in the abrasive dispersion supply line 7 is received in the container 60. While discharging, the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 are cleaned with pure water. When a predetermined amount of pure water flows out from the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 into the receiving container 60, the on-off valve 57 is closed to stop the supply of pure water. At this time, the open / close valve 42 of the related flow path is closed, and each of the three-way switching valves 43 and 10 controls the flow path in the direction indicated by the solid line arrow in the figure. As a result, microorganisms adhering to the inner walls of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 are discharged together with the hydrogen peroxide solution 50 and pure water into the receiving container 60.

Figure 8 shows the state of the sixth step during washing for discharging the pure water abrasive dispersion liquid in the supply line 7 by the nitrogen gas supply, 8, 1, 7 and the same place the same number The description is omitted. In addition, the broken line arrow in a figure shows the flow of nitrogen gas.

After the hydrogen peroxide solution 50 in the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 is discharged and washed with pure water, the on-off valve 46 and the on-off valve 57 are closed, the on-off valve 42 and the on-off valve 48. The on-off valve 8 is opened. The three-way valve 41,43,10 are those that controls the flow path in the flow direction of the nitrogen gas as shown in FIG. The nitrogen gas is supplied from the nitrogen gas supply line 45 to the branch line 47, the opening / closing valve 48, the three-way switching valve 41, the opening / closing valve 42, the three-way switching valve 43, the three-way switching valve 10, and the cleaning liquid supply line 44. 7 and supplied into the abrasive dispersion supply pipe 6. As a result, pure water in the cleaning liquid supply line 44, the abrasive dispersion supply line 7, and the abrasive dispersion supply pipe 6 is discharged to the receiving container 60 through the on-off valve 8.

  The microorganism removal and cleaning operations are completed by the first to sixth steps. The abrasive dispersion container 1 for storing the abrasive dispersion 2 again is attached to the detachable member 5, and the slurry is produced as shown in FIG.

  In the embodiment, each on-off valve, three-way switching valve, and pump constituting the slurry supply device are individually controlled by a controller (not shown). Further, the abrasive dispersion liquid 2, the hydrogen peroxide solutions 14, 50, and the TMAH liquid 39 are supplied by means of pressurization with nitrogen gas, but supply means by a pump, a drop pressure, or the like may be used. Furthermore, the number of polishing stock solutions for slurry, the components, and the configuration of the slurry supply device are merely examples, and the present invention is not limited thereto. Further, in the cleaning step, the TMAH solution 39, the hydrogen peroxide solution 50, pure water, and nitrogen gas are supplied from the opposite direction (reverse direction) of the abrasive dispersion 2 to the abrasive dispersion supply pipe 6 and the abrasive dispersion supply line. Although it was made to supply and flow to 7, it may be the same direction. The abrasive dispersion container 1 is exchanged with the new abrasive dispersion container 1 containing the abrasive dispersion 2 via the detachable member 5 when the abrasive dispersion 2 becomes empty. Therefore, the containers 58, 59, and 60 that receive the abrasive dispersion 2, the TMAH 39, the hydrogen peroxide solution 50, and the pure water are also exchanged via the detachable member 5 in the same manner as the abrasive dispersion container 1 at the time of cleaning. Therefore, the TMAH solution 39, the hydrogen peroxide solution 50, pure water, and nitrogen gas can be supplied from the opposite direction (reverse direction) to the abrasive dispersion 62 flow. It is preferable to feed and flow to the tube 6 and the abrasive dispersion supply line 7.

  Further, in the embodiment, the example of removing and cleaning microorganisms adhering in the abrasive dispersion supply line 7 has been described, but polishing of a slurry which is a mixed liquid of the plurality of polishing stock solutions from the polishing stock solution supply line. The slurry supply lines 26, 32, 36, 35, and the circulation lines 24, 30, the slurry mixed storage container 11, and the slurry mixed storage container 28, respectively, which are at least a part of the supply line to the apparatus The basic microorganism removal and cleaning operations of the first to sixth steps can be similarly performed.

  As described above, the TMAH liquid 39 is supplied to and discharged from at least a part of the polishing stock solution from the supply line to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing apparatus. The present invention is a slurry supply apparatus cleaning method characterized in that hydrogen water 50 is supplied and discharged, and a slurry supply apparatus using this cleaning method.

  As a result, microorganisms adhered and propagated by the TMAH solution are dissolved, and further, the removal of the microorganisms by the reaction between the TMAH solution and the hydrogen peroxide solution is promoted, so that the microorganisms can be reliably removed and washed. Therefore, it is possible to prevent a change in flow rate due to an increase in flow resistance in the polishing fluid supply path due to the propagation of microorganisms, and to stabilize the mixing ratio. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.

  In addition, by supplying the TMAH liquid and retaining it in the supply line for a predetermined time, TMAH, which is an organic strong alkaline substance, is added to the microorganisms that adhere to and propagate on the inner wall even in the bent part of the supply line and partly become agglomerated. The liquid can be sufficiently contacted and penetrated to lyse and sterilize microbial cells more reliably.

Also, by supplying hydrogen peroxide water and retaining it in the supply line for a predetermined time, the tetramethylammonium hydroxide liquid, which is a strong alkaline substance that remains attached to the inner wall of the supply line and the microorganisms, reacts with the hydrogen peroxide water. and foamed, the microorganisms and dissolved by TMAH solution, it is possible to further promote the release and sterilization of the inner wall of the supply line from the inner wall.

  As described above, the microorganisms adhere to and propagate on the abrasive dispersion supply pipe 6 and the abrasive dispersion supply line 7 as time passes when the slurry 12 is created in the slurry mixing storage container 11. For this reason, removal and washing of microorganisms adhering to and growing on the abrasive dispersion supply line 7 may be performed at predetermined intervals within a permissible range in which the mixing ratio of the plurality of polishing stock solutions does not adversely affect the polishing performance of the polishing apparatus. Good.

  In addition, microorganism removal and cleaning operations are performed by detecting the pressure on the upstream and downstream sides of the abrasive dispersion supply pipe 6 and the abrasive dispersion supply line 7 (not shown), thereby causing the flow of microorganisms due to adhesion and propagation. When the road resistance has increased by a predetermined value or more, it is possible to determine when to perform the microorganism removal and cleaning operations. In this case, it is possible to more surely grasp the time required for removing and washing the microorganisms.

  Next, another configuration of the first embodiment will be described with reference to FIG. This is because a single microorganism detection means 200 is used to detect the polishing stock solution or slurry from a plurality of portions from a supply line of the polishing stock solution to a supply line of a slurry, which is a mixed liquid of the plurality of polishing stock solutions, to the polishing apparatus. 200 is used to detect microorganisms. The same reference numerals as those in FIG.

  A detection line 209 branched from the abrasive dispersion supply line 7 is connected to the switching valve 400, and the switching valve 400 and the microorganism detecting means 200 are further connected. The sterilizing means 300 is provided on the downstream side of the abrasive dispersion supply line 7 where the detection line 209 branches.

  Further, the detection line 209 branched from the circulation line 24 is connected to the switching valve 400, and the switching valve 400 and the microorganism detecting means 200 are further connected. The sterilizing means 300 is provided on the downstream side of the circulation line 24 where the detection line 209 branches.

  Further, the switching line 400 is connected to the detection line 209 branched from the circulation line 30, and the switching valve 400 and the microorganism detection means 200 are further connected. The sterilizing means 300 is provided on the downstream side of the circulation line 30 where the detection line 209 branches.

  In the configuration described above, the flow path is switched by the switching valve 400 to sequentially detect the abrasive dispersion 2 from the abrasive dispersion supply line 7, the slurry 12 from the circulation line 24, and the slurry 29 from the circulation line 30. 200. The operations of the microorganism detecting means 200 and the sterilizing means 300 are the same as in the above-described example, and the description thereof is omitted.

  Thereby, in the supply line from the supply line of the polishing stock solution to the polishing apparatus for the slurry, which is a mixed solution of the plurality of polishing stock solutions, the number of microorganism detecting means is reduced and the site where the microorganisms are present or the breeding site is specified. Can do.

(Example 2)
Hereinafter, the slurry supply apparatus of Example 2 of this invention is demonstrated, referring FIGS. 10-16.

  A fundamental difference from the first embodiment is that a plurality of polishing stock solutions are mixed as much as possible immediately before the polishing apparatus and supplied to the polishing apparatus without providing a container for storing a predetermined amount of slurry. FIG. 10 is a basic configuration diagram of the slurry supply device of the present invention, FIG. 11 is a configuration diagram of the slurry supply device showing the state of the first step during cleaning to discharge the abrasive dispersion by supplying pure water, and FIG. 12 is a TMAH solution. FIG. 13 is a configuration diagram of the slurry supply apparatus showing the state of the third step during cleaning to discharge the TMAH liquid supplied with nitrogen gas, and FIG. 14 is a configuration diagram of the slurry supply apparatus showing the state of the fourth step at the time of cleaning to supply the hydrogen peroxide solution, and FIG. 15 shows the state of the fifth step at the time of cleaning to discharge the hydrogen peroxide solution by supplying pure water. FIG. 16 is a configuration diagram of the slurry supply apparatus, FIG. 16 is a configuration diagram of the slurry supply apparatus showing the state of the sixth step during cleaning for discharging pure water by supplying nitrogen gas, and FIG. 17 is a diagram showing another configuration of the first embodiment. is there.

  In FIG. 10, the basic configuration will be described first. A predetermined amount of the abrasive dispersion 62 is stored in the abrasive dispersion container 61, and nitrogen gas is supplied from the nitrogen gas supply line 63 through the opening / closing valve 64 to the upper surface of the abrasive dispersion 62 in the abrasive dispersion container 61. Pressurize. A supply pipe 66 is provided in the abrasive dispersion container 61 and communicates with the abrasive dispersion supply line 67. The nitrogen gas supply line 63 and the abrasive dispersion liquid supply line 67 are fixed to the detachable member 65 and configured to be detachable from the abrasive dispersion container 61.

  The abrasive dispersion 62 is supplied to the mixer 70 via the on-off valve 69 and the flow meter 68 of the abrasive dispersion supply line 67. The abrasive dispersion supply line 67 is installed with a plurality of bent portions in the mounted state. An abrasive dispersion 62, a hydrogen peroxide solution to be described later, and pure water as needed are supplied into the mixer 70, and mixing thereof is promoted to create a slurry that is a mixed polishing liquid.

  The hydrogen peroxide solution 72 is stored in the hydrogen peroxide solution container 71, and the upper surface of the hydrogen peroxide solution 72 in the hydrogen peroxide solution container 71 is pressurized with nitrogen gas from the nitrogen gas supply line 73 through the on-off valve 74. . A supply pipe 76 is provided in the hydrogen peroxide solution container 71 and communicates with the hydrogen peroxide solution supply line 77. Further, the nitrogen gas supply line 73 and the hydrogen peroxide solution supply line 77 are fixed to the detachable member 75 and are configured to be detachable from the hydrogen peroxide solution container 71. A hydrogen peroxide solution 72 is supplied to the mixer 70 via the on-off valve 79 of the hydrogen peroxide solution supply line 77.

The mixed slurry is supplied from the mixer 70 via the slurry supply line 80 and the three-way switching valve 81 to the polishing unit 83 via the slurry discharge line 82.

  A TMAH liquid 85 is stored in a predetermined amount in the TMAH liquid container 84, and a TMAH liquid supply line 90 opened in the TMAH liquid container 84 is passed through a three-way switching valve 91, a three-way switching valve 92, and a cleaning liquid supply line 93. It is connected to the. Nitrogen gas is pressurized from the nitrogen gas supply line 86 through the on-off valve 87 to pressurize the upper surface of the TMAH liquid 85 in the TMAH liquid container 84. A branch line 88 branched from the nitrogen gas supply line 86 is connected to a TMAH liquid supply line 90 via an on-off valve 89.

A predetermined amount of hydrogen peroxide solution 95 is stored in the hydrogen peroxide solution container 94, and a hydrogen peroxide solution supply line 96 opened in the hydrogen peroxide solution container 94 is connected to the three-way switching valve 91. Nitrogen gas is pressurized from the nitrogen gas supply line 97 through the on-off valve 98 to pressurize the upper surface of the hydrogen peroxide solution 95 in the hydrogen peroxide solution container 94. Branch line 99 branching from the nitrogen gas supply line 97 is connected via an on-off valve 100 is connected to the hydrogen peroxide solution supply line 96, the three-way selector valve 91, via a three-way valve 92 to the cleaning liquid supply line 93 . A branch line 101 branched from the pure water supply line is connected to a three-way switching valve 92 via an on-off valve 102.

  Microorganism detection means 200 is provided in the slurry supply line 80 leading to the three-way switching valve 81 and the polishing device 83 of the slurry supply line 80, and the sterilization means 300 is provided downstream of the microorganism detection means 200. The microorganism detecting means 200 and the sterilizing means 300 are the same as those used in the first embodiment and will not be described.

Next, the preparation of the slurry and the supply operation to the polishing unit 83 will be described. An opening / closing valve 64 is opened on the upper surface of the abrasive dispersion 62 in the abrasive dispersion container 61 and a predetermined pressure of nitrogen gas is applied from the nitrogen gas supply line 63, whereby an amount of abrasive grains corresponding to the mixing ratio in the slurry is applied. the dispersion 62 is supplied to and through the opening and closing valve 69 is opened abrasive dispersion liquid mixer 70 from the supply line 67.

At the same time as the supply of the abrasive dispersion 62 is started, the open / close valve 74 is opened on the upper surface of the hydrogen peroxide solution 72 in the hydrogen peroxide solution container 71 to apply a predetermined pressure of nitrogen gas from the nitrogen gas supply line 73. Thus, an amount of hydrogen peroxide solution 72 corresponding to the mixing ratio in the slurry is supplied from the hydrogen peroxide solution supply line 77 into the mixer 70 via the open on-off valve 79 . The abrasive dispersion 62 and the hydrogen peroxide solution 72 are uniformly mixed in a mixer 70, and a slurry as a mixed polishing liquid is passed through a three-way switching valve 81 from a slurry supply line 80 and a slurry discharge line 82 to a polishing unit 83. To supply. The mixing ratio of the abrasive dispersion 62 and the hydrogen peroxide solution is measured and managed by the respective flow meters 68 and 78, and is controlled to a predetermined component ratio.

  During the preparation of the slurry and the supply operation to the polishing apparatus 83, the microorganisms in the slurry are detected by the microorganism detection means 200 provided in the slurry supply line 80 as described above. First, the on-off valve 210 is opened, and slurry is supplied from the inflow port 206 through the detection line 209 via the three-way switching valve 211 to fill the measurement cell 202. When the inside of the measurement cell 202 is filled with the abrasive dispersion 2 or the slurry 12, 29, the on-off valve 210 is closed for a predetermined time to detect microorganisms.

  When so-called microorganisms in which the impedance Z between the thin film electrodes 201a and 201b does not change are not detected, this is notified by the notification means 208b. Further, the sterilizing means 300 continues the operation of the normal slurry supply apparatus while the ultraviolet irradiation is stopped.

  In the process of continuing the operation of the slurry supply apparatus, for example, when the microorganism detection means 200 provided in the slurry supply line 80 detects a predetermined number of microorganisms, this is notified by the notification means 208b. Further, the sterilizing means 300 provided on the downstream side of the microorganism detecting means 200 irradiates the slurry passing therethrough with ultraviolet rays to kill the microorganisms. Thereby, the flow of microorganisms to the downstream area of the sterilization means 300 can be prevented.

  According to the detection level of the number of microorganisms in the predetermined range of the microorganism detection means 200, the irradiation intensity of ultraviolet rays necessary for killing the microorganisms in the sterilization means 300 is changed to kill the microorganisms even if the number of microorganisms varies. be able to.

  Although the sterilization means 300 is provided on the downstream side of the microorganism detection means 200, a plurality of microorganism detection means 200 may be provided on the downstream side and the upstream side in the vicinity of the sterilization means 300. In this case, microorganisms can be detected by the upstream microorganism detection means 200, and the sterilization effect of the sterilization means 300 can be confirmed by the downstream microorganism detection means 200 after passing through the sterilization means 300.

In Examples 2 twofold information, the microbial detection unit 200, the is provided one in part extending in the supply line to a plurality of polishing apparatuses of the slurry is a mixture of abrasive stock, slurry supply line 80 and abrasive You may provide in the several places of the particle dispersion supply line 67. FIG.

  In the process of continuously operating the slurry supply device, there is a case where the microorganism detecting means 200 detects a continuous increasing tendency of microorganisms. This is because there is a possibility that microorganisms are attached and propagated in any part from the supply line of the polishing stock solution to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing apparatus.

When microorganisms adhere and propagate, there is a possibility that the fluctuation of the mixing ratio of a plurality of polishing stock solutions or the amount of slurry supplied to the polishing apparatus will change, which will adversely affect the polishing performance of the polishing apparatus.
For this reason, it is necessary to remove attached and propagated microorganisms.

  As described in Example 1, when the number of microorganisms detected by the microorganism detection unit 200 is equal to or greater than a predetermined value, or when microorganisms are continuously detected for a long period of time, an increasing tendency of the number of microorganisms was confirmed for a certain period. Occasionally, cleaning is performed to remove microorganisms that have adhered and propagated. The state of each step during cleaning for removing microorganisms in the abrasive dispersion supply line 67 and the slurry supply line 80 will be described in order with reference to FIGS.

  FIG. 11 shows the state of the first step during cleaning, which is a state in which the abrasive dispersion 2 in the abrasive dispersion supply line 7 by pure water supply is discharged. Are given the same numbers and their explanation is omitted. 10 differs from FIG. 10 in that the abrasive dispersion container 61 is moved apart at the detachable member 65 and the receiving container 103 for receiving the abrasive dispersion 62 discharged from the supply pipe 66 is positioned. It is. In addition, the solid line arrow in a figure shows the flow of pure water.

Pure water is supplied from the pure water supply line 101 into the slurry supply line 80 and the abrasive dispersion supply line 67 through the open on-off valve 102 and the three-way switching valves 92 and 81. The pure water flows to the slurry supply line 80, the mixer 70, the abrasive dispersion supply line 67, the open on-off valve 69, the flow meter 68, and the abrasive dispersion supply pipe 66 , whereby the abrasive dispersion 2 is supplied. It is discharged into the receiving container 103 and washed once with pure water. Further, when pure water is allowed to flow into the receiving container 103, the on-off valve 102 is closed to stop the supply of pure water. At this time, each of the three-way switching valves 92 and 81 of the related flow path controls the flow path in the direction indicated by the solid line arrow in the figure.

  FIG. 12 shows a state of the second step at the time of supplying the TMAH solution 85 into the slurry supply line 80 and the abrasive dispersion supply line 67. In FIG. 12, the same parts as those in FIGS. A number is attached and explanation is omitted. The difference from FIGS. 10 and 11 is that the receiving container 104 for receiving the TMAH liquid discharged from the supply pipe 66 is positioned. In addition, the solid line arrow in a figure shows the flow of TMAH liquid, and the broken line arrow shows the flow of nitrogen gas.

  As described above, a predetermined amount of TMAH liquid 85 is stored in the TMAH liquid container 84, and the TMAH liquid supply line 90 opened in the TMAH liquid container 84 is switched three-way through the three-way switching valves 91 and 92 and the cleaning liquid supply line 93. Connected to the valve 81. At this time, the on-off valve 69 is opened, the on-off valve 89 related to the flow path of the TMAH liquid 85 is closed, and each of the three-way switching valves 91, 92, 81 has a flow path in the direction indicated by the solid line arrow in the figure. It is what is being controlled.

The on-off valve 87 is opened from the nitrogen gas supply line 86 and the supply pressure of nitrogen gas is applied to the upper surface of the TMAH liquid 85 in the TMAH liquid container 84. The TMAH liquid 85 in the TMAH liquid container 84 is pushed out to the TMAH liquid supply line 90 and is supplied to the slurry supply line 80 and the abrasive dispersion liquid via the three-way switching valves 91 and 92, the cleaning liquid supply line 93, and the three-way switching valve 81. It flows to the line 67 and the supply pipe 66. As a result, the pure water in the slurry supply line 80, the abrasive dispersion supply line 67 and the abrasive dispersion supply pipe 66 is pushed out and replaced with the TMAH liquid 85. The pure water and the TMAH liquid 85 flow out from the supply pipe 66 to the receiving container 104.

At the stage where the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 are replaced with the TMAH liquid 85, the on-off valve 87 is closed to stop the supply of the TMAH liquid 85, and the slurry supply line 80, The TMAH liquid 85 is retained and held in the abrasive dispersion supply line 67 and the supply pipe 66 for a predetermined time (for example, 5 to 10 minutes). At this time, in the process in which the TMAH solution 85 which is an organic strong alkaline substance is in contact with the microorganisms attached and propagated on the inner wall of the slurry supply line 80, the abrasive dispersion supply line 67 and the supply pipe 66, the cells of the microorganisms are removed. Dissolve and sterilize. As a result, the TMAH solution 85, which is an organic strong alkali substance, sufficiently contacts and penetrates the microorganisms that adhere to and propagate on the inner wall of the supply line having the bent portion and are partially agglomerated. Cells can be lysed and sterilized. Further, the microorganisms are negatively charged due to the change of pH to the alkali side due to the supply of the TMAH liquid, and due to the electrical repulsion action between the slurry supply line 80 made of a resin material, the abrasive dispersion supply line 67, and the inner wall of the supply pipe 66. There is also physical detachment of microorganisms. The TMAH liquid 85 is not particularly limited, but is used after being diluted with ultrapure water to a concentration of 25%. It is used as the mainstream of developer in semiconductor factories and can be shared as a whole semiconductor manufacturing facility.

As described above, by discharging the abrasive dispersion 62 from the abrasive dispersion supply line 67 and the abrasive dispersion supply pipe 66 and cleaning with pure water, the abrasive dispersion supply line 67 , the abrasive The components of the abrasive dispersion liquid 62 are removed from the surface of the microorganisms adhered and propagated on the inner wall and the inner wall of the grain dispersion supply pipe 66 , and the TMAH solution 85 directly contacts and permeates the microorganisms. Can be dissolved and sterilized.

  The pure water in the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 is extruded by supplying the TMAH liquid 85 and replaced with the TMAH liquid 85. The pure water in the supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 may be discharged, and then the TMAH liquid 85 may be supplied.

FIG. 13 shows a state of the third step during washing discharging the TMAH solution 85 of the slurry feed line 80, abrasive dispersion liquid in the supply line 67 by the nitrogen gas supply, 13, 10, 12 and The same parts are denoted by the same reference numerals and the description thereof is omitted. In addition, the broken line arrow in a figure shows the flow of nitrogen gas. After retaining the TMAH solution 85 in the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 for a predetermined time, the on-off valve 87 is closed and the on-off valve 89 and the on-off valve 69 are opened. . The three-way valve 91,92,81 are those that controls the flow path in the flow direction of the nitrogen gas as shown in FIG. 13. Nitrogen gas is supplied from the nitrogen gas supply line 86 into the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 through the on-off valve 89, the three-way switching valves 91, 92, 81, and the cleaning liquid supply line 93. To do. As a result, the TMAH liquid 85 staying in the cleaning liquid supply line 93, the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 is discharged to the receiving container 104 through the opening / closing valve 69 and the flow meter 68.

FIG. 14 shows the state of the fourth step at the time of cleaning in which the hydrogen peroxide solution is supplied into the slurry supply line 80 and the abrasive dispersion supply line 67. In FIG. 14, the same parts as those in FIGS. The same number is attached and explanation is omitted. A difference from FIGS. 10 and 13 is that the receiving container 105 for receiving the hydrogen peroxide solution discharged from the supply pipe 66 is located. In the figure, solid arrows indicate the flow of hydrogen peroxide water, and broken arrows indicate the flow of nitrogen gas.

As described above, a predetermined amount of hydrogen peroxide solution (H ₂ O ₂ ) 95 is stored in the hydrogen peroxide solution container 94, and the hydrogen peroxide solution supply line 96 opened in the hydrogen peroxide solution container 94 has three sides. It is connected to a three-way switching valve 81 through switching valves 91 and 92 and a cleaning liquid supply line 93. At this time, the opening / closing valve 69 is opened, the opening / closing valve 100 related to the flow path of the hydrogen peroxide solution 95 is closed, and each of the three-way switching valves 91, 92, 81 flows in the direction indicated by the solid line arrow in the figure. The road is controlled.

  The on-off valve 98 is opened from the nitrogen gas supply line 97, and the supply pressure of nitrogen gas is applied to the upper surface of the hydrogen peroxide solution 95 in the hydrogen peroxide solution container 94. The hydrogen peroxide solution 95 in the hydrogen peroxide solution container 94 is pushed out to the hydrogen peroxide solution supply line 96, and the slurry supply line 80 is passed through the three-way switching valves 91 and 92, the cleaning liquid supply line 93, and the three-way switching valve 81. , Flows into the abrasive dispersion supply line 67 and the supply pipe 66. Further, it flows out from the supply pipe 66 to the receiving container 105 through the on-off valve 69 and the flow meter 68.

When the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 are filled with the hydrogen peroxide solution 95, the on-off valve 98 is closed to stop the supply of the hydrogen peroxide solution 95 and the slurry. The hydrogen peroxide solution 95 is retained and held in the supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 for a predetermined time (for example, 5 to 10 minutes). At this time, the slurry feed line 80, abrasive dispersion liquid supply line 67, the inner wall of the supply tube 66, and foamed TMAH solution 85 and hydrogen peroxide 95 is a strong alkaline substance adhering residual microorganisms are reacted, it Thus, it is possible to further promote separation of the microorganisms dissolved by the TMAH solution 85 from the inner wall of the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 and sterilization of the inner wall of the supply line.

  FIG. 15 shows a state of the fifth step at the time of cleaning, which is a state in which the hydrogen peroxide solution 95 in the slurry supply line 80 and the abrasive dispersion supply line 67 by pure water supply is discharged. The same parts as those of FIGS. In addition, the solid line arrow in a figure shows the flow of pure water.

Pure water is supplied from the pure water supply line 101 into the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 through the open / close valve 102, the three-way switching valve 92, and the cleaning liquid supply line 93. Pure water flows through an on-off valve 69, a flow meter 68, and a supply pipe 66 with the slurry supply line 80 and the abrasive dispersion supply line 67 open, and is discharged to the receiving container 105 and supplied with the abrasive dispersion. The line 67 and the inside of the abrasive dispersion supply pipe 66 are cleaned with pure water. When pure water is allowed to flow out from the supply pipe 66 into the receiving container 105, the on-off valve 102 is closed to stop the supply of pure water. At this time, each of the related three-way switching valves 92 and 81 controls the flow path in the direction indicated by the solid line arrow in the figure. Thereby, the microorganisms adhering to the inner walls of the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 are discharged together with the hydrogen peroxide solution 95 and the pure water into the receiving container 105.

  FIG. 16 shows the state of the sixth step at the time of cleaning for discharging pure water in the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 by supplying nitrogen gas. , 15 are denoted by the same reference numerals and description thereof is omitted. In addition, the broken line arrow in a figure shows the flow of nitrogen gas.

  After the hydrogen peroxide solution 95 in the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 is discharged and washed with pure water, the open / close valve 87 is closed and the open / close valve 69 is opened. The three-way switching valves 91, 92, 81 control the flow path in the nitrogen gas flow direction shown in FIG. The nitrogen gas is supplied from the nitrogen gas supply line 86 to the branch line 88, the on-off valve 89, the three-way switching valves 91, 92, 81, and the cleaning liquid supply line 93, and then to the slurry supply line 80, abrasive dispersion supply line 67, and supply pipe 66. Supply in. As a result, pure water is discharged into the receiving container 105.

  The microorganism removal and cleaning operations are completed by the first to sixth steps. The abrasive dispersion container 61 for storing the abrasive dispersion 62 again is attached to the detachable member 65, and the slurry is produced and supplied to the polishing apparatus 83 as shown in FIG.

  In the embodiment, each on-off valve, three-way switching valve, and pump constituting the slurry supply device are individually controlled by a controller (not shown). Further, the abrasive dispersion liquid 62, the hydrogen peroxide solutions 72 and 95, and the TMAH liquid 85 are supplied by means of pressurizing with nitrogen gas, but supply means using a pump, a drop pressure, or the like may be used. Furthermore, the number of polishing stock solutions for slurry, the components, and the configuration of the slurry supply device are merely examples, and the present invention is not limited thereto. In addition to the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66, the mixer 70 and the flow meter 68 can be cleaned simultaneously.

  In the second embodiment, the slurry supply line 80, the abrasive dispersion supply line 67, and the microorganisms attached to the supply pipe 66 are removed and cleaned. Also in each part and path of each of the slurry supply line 80, the abrasive dispersion supply line 67, and the mixer 70, which are at least part of the slurry that is a mixed liquid of the polishing stock solution to the supply line to the polishing apparatus. The basic microorganism removal and cleaning operations in the first to sixth steps may be performed individually.

  Further, the TMAH liquid 39, the hydrogen peroxide solution 50, the pure water, and the nitrogen gas are supplied from the three-way switching valve 81 provided in the slurry supply line 80, but the slurry is discharged to the polishing device 83 of the slurry supply line 80. You may make it supply from an exit. Further, in the cleaning step, the TMAH solution 85, the hydrogen peroxide solution 95, pure water, and nitrogen gas are supplied from the slurry supply line 80 and the abrasive dispersion supply line 7 in the opposite direction (reverse direction) to the flow of the slurry and the abrasive dispersion liquid 62. The supply pipe 66 is supplied and flowed, but it may be in the same direction. The abrasive dispersion container 61 is replaced with a new abrasive dispersion container 61 containing the abrasive dispersion 62 via the detachable member 65 when the abrasive dispersion 62 becomes empty. Therefore, at the time of cleaning, the containers 103, 104, and 105 that receive the abrasive dispersion liquid 62, the TMAH liquid 85, the hydrogen peroxide solution 95, and the pure water are also replaced through the detachable member 65 in the same manner as the abrasive dispersion container 61. Therefore, the TMAH solution 85, the hydrogen peroxide solution 95, the pure water, and the nitrogen gas are supplied from the abrasive dispersion 62 and the slurry supply line in the opposite direction (reverse direction) to the slurry flow. 80, and preferably supplied to the abrasive dispersion supply line 67 and the abrasive dispersion supply pipe 6.

  In the second embodiment, the polishing apparatus 83 is stopped during cleaning, but the cleaning may be performed during regular maintenance of the slurry supply apparatus or the polishing apparatus 83. In addition, by providing two slurry supply devices for one polishing layer device 83, cleaning can be performed without stopping the polishing layer device 83.

  Next, another configuration of the second embodiment will be described with reference to FIG. This is because a single microorganism detection means 200 is used to detect the polishing stock solution or slurry from a plurality of portions from a supply line of the polishing stock solution to a supply line of a slurry, which is a mixed liquid of the plurality of polishing stock solutions, to the polishing apparatus. A configuration and an operation for detecting the microorganisms by deriving them to 200 will be described with reference to FIG. The same reference numerals as those in FIG.

  A detection line 209 branched from the abrasive dispersion supply line 67 is connected to the switching valve 400, and the switching valve 400 and the microorganism detection means 200 are further connected. The sterilizing means 300 is provided on the downstream side of the abrasive dispersion supply line 67 from which the detection line 209 is branched.

  A detection line 209 branched from the slurry discharge line 82 is connected to the switching valve 400, and the switching valve 400 and the microorganism detection means 200 are further connected. The sterilizing means 300 is provided on the downstream side of the circulation line 24 where the detection line 209 branches.

  In the configuration described above, the flow path is switched by the switching valve 400 so that the abrasive dispersion 62 from the abrasive dispersion supply line 67 and the slurry from the slurry discharge line 82 are sequentially led to the microorganism detecting means 200. The operations of the microorganism detecting means 200 and the sterilizing means 300 are the same as in the above-described example, and the description thereof is omitted.

  Thereby, in the supply line from the supply line of the polishing stock solution to the polishing apparatus for the slurry, which is a mixed solution of the plurality of polishing stock solutions, the number of microorganism detecting means is reduced and the site where the microorganisms are present or the breeding site is specified. Can do.

  As described above, also in the second embodiment, the same effects as in the first embodiment can be obtained.

  The present invention can also be applied to a wide range of apparatuses that require supply of polishing liquid.

Basic configuration diagram of slurry supply apparatus of embodiment 1 of the present invention Basic configuration diagram of microorganism detection means The block diagram of the slurry supply apparatus which shows the state of the 1st step at the time of the washing | cleaning which discharges the abrasive grain dispersion liquid by a pure water supply The block diagram of the slurry supply apparatus which shows the state of the 2nd step at the time of the washing | cleaning which supplies a TMAH liquid The block diagram of the slurry supply apparatus which shows the state of the 3rd step at the time of the washing | cleaning which discharges the TMAH liquid by nitrogen gas supply The block diagram of the slurry supply apparatus which shows the state of the 4th step at the time of the washing | cleaning which supplies hydrogen peroxide water The block diagram of the slurry supply apparatus which shows the state of the 5th step at the time of the washing | cleaning which discharges the hydrogen peroxide solution by a pure water supply The block diagram of the slurry supply apparatus which shows the state of the 6th step at the time of the washing | cleaning which discharges the pure water by nitrogen gas supply The figure which shows the other structure of Example 1. Basic configuration diagram of slurry supply apparatus of embodiment 2 of the present invention The block diagram of the slurry supply apparatus which shows the state of the 1st step at the time of the washing | cleaning which discharges the abrasive grain dispersion liquid by a pure water supply The block diagram of the slurry supply apparatus which shows the state of the 2nd step at the time of the washing | cleaning which supplies a TMAH liquid The block diagram of the slurry supply apparatus which shows the state of the 3rd step at the time of the washing | cleaning which discharges the TMAH liquid by nitrogen gas supply The block diagram of the slurry supply apparatus which shows the state of the 4th step at the time of the washing | cleaning which supplies hydrogen peroxide water The block diagram of the slurry supply apparatus which shows the state of the 5th step at the time of the washing | cleaning which discharges the hydrogen peroxide solution by a pure water supply The block diagram of the slurry supply apparatus which shows the state of the 6th step at the time of the washing | cleaning which discharges the pure water by nitrogen gas supply The figure which shows the other structure of Example 2.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Abrasive dispersion container 2 Abrasive dispersion 3 Nitrogen gas supply line 4 On-off valve 5 Detachable member 6 Abrasive dispersion supply pipe 7 Abrasive dispersion supply line 8 On-off valve 9 Bending part 10 Three-way switching valve 11 Slurry mixed storage Container 12 Slurry (mixed polishing liquid)
13 Hydrogen peroxide solution container 14 Hydrogen peroxide solution 15 Nitrogen gas supply line 16 Open / close valve 17 Detachable member 18 Supply pipe 19 Hydrogen peroxide solution supply line 20 Open / close valve 21 Pure water supply line 22 Pure water branch line 23 Open / close valve 24 Circulation Line 25 Pump 26 Slurry supply line 27 On-off valve 28 Slurry storage container 29 Slurry 30 Circulation line 31 Pump 32 Slurry supply line 33 Pump 34 Polishing device 35 Slurry supply line 36 Pump 37 Polishing device 38 TMAH liquid container 39 TMAH liquid 40 TMAH liquid supply Line 41 Three-way selector valve 42 On-off valve 43 Three-way selector valve 44 Cleaning liquid supply line 45 Nitrogen gas supply line 46 On-off valve 47 Branch line 48 On-off valve 49 Hydrogen peroxide solution container 50 Hydrogen peroxide solution 51 Hydrogen peroxide solution supply line 52 Nitrogen Ga Gas supply line 53 On-off valve 54 Branch line 55 On-off valve 56 Branch line 57 On-off valve 58 Receiving container 59 Receiving container 60 Receiving container 61 Abrasive dispersion liquid container 62 Abrasive dispersion liquid 63 Nitrogen gas supply line 64 On-off valve 65 Removable member 66 Supply pipe (Abrasive dispersion supply line)
67 Abrasive dispersion supply line 68 Flow meter 69 On-off valve 70 Mixer 71 Hydrogen peroxide solution container 72 Hydrogen peroxide solution 73 Nitrogen gas supply line 74 On-off valve 75 Detachable member 76 Supply pipe 77 Hydrogen peroxide solution supply line 78 Flow rate Total 79 Open / close valve 80 Slurry supply line 81 Three-way switching valve 82 Slurry discharge line 83 Polishing device 84 TMAH liquid container 85 TMAH liquid 86 Nitrogen gas supply line 87 Open / close valve 88 Branch line 89 Open / close valve 90 TMAH liquid supply line 91 Three-way switch valve 92 Three-way selector valve 93 Cleaning liquid supply line 94 Hydrogen peroxide solution container 95 Hydrogen peroxide solution 96 Hydrogen peroxide solution supply line 97 Nitrogen gas supply line 98 On-off valve 99 Branch line 100 On-off valve 101 Pure water supply line 102 On-off valve 103 Receiving container 104 receiving container 105 receiving container 00 Microorganism detection means 201a Thin film electrode 201b Thin film electrode 202 Measurement cell 203 Glass substrate 204 Current detection resistance 205 Low voltage power supply 206 Inlet 207 Outlet 208 Arithmetic device 208a Controller 208b Notification means 209 Detection line 210 Open / close valve 211 Three-way switching valve 212 Cleaning liquid supply line 300 Sterilization means 400 Switching valve

Claims (6)

Comprising a microorganism detecting means for detecting microorganisms in any part from a supply line of a polishing stock solution to a supply line of a slurry that is a mixed liquid of the plurality of polishing stock solutions to a polishing apparatus ;
A cleaning means for cleaning at least a part of the polishing stock solution from the supply line to the supply line to the polishing apparatus for the slurry, which is a mixed solution of the plurality of polishing stock solutions, includes a detection value of microorganisms by the microorganism detection means. Based on the above, the at least a part of the polishing stock solution from the supply line to the supply line to the polishing apparatus of the slurry that is a mixed solution of the plurality of polishing stock solution is washed with pure water, after washing with pure water,
A tetramethylammonium hydroxide (TMAH) liquid is supplied to at least a part of a supply line from the supply line of the polishing stock solution to a polishing apparatus for slurry, which is a mixed polishing stock solution of the plurality of polishing stock solutions, and is supplied to the supply line. After being discharged for a period of time, hydrogen peroxide water is supplied and discharged for a predetermined time in the supply line.
Wherein the plurality of liquid mixture and abrasive dispersion liquid supply line der Ru slurry dispenser which at least part of the part extending in the supply line to the polishing apparatus slurry made of a resin material is polishing stock solution from the supply line of the polishing stock solution. 2. The slurry supply according to claim 1, further comprising a microorganism detecting unit at a plurality of portions from a supply line of the polishing stock solution to a supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing apparatus. apparatus. The microorganism stock detecting means is configured to cause the polishing stock solution or slurry to be led out from a plurality of portions from a supply line of the polishing stock solution to a supply line of a slurry that is a mixed liquid of the plurality of polishing stock solutions to a polishing apparatus. 2. The slurry supply apparatus according to 1. The slurry supply apparatus according to any one of claims 1 to 3, further comprising an informing means for informing a detection value by the microorganism detecting means. A sterilization means for sterilizing microorganisms is provided at least in a part from the polishing stock supply line to the slurry supply apparatus for the slurry, which is a mixed liquid of the plurality of polishing stock solutions, to detect microorganisms by the microorganism detection means. The slurry supply apparatus according to any one of claims 1 to 4, wherein the sterilizing means is driven based on the slurry. The TMAH liquid, the hydrogen peroxide solution, and the pure water are supplied to the abrasive dispersion supply line from the opposite direction (reverse direction) to the flow of the abrasive dispersion and flowed. Slurry feeder.

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