JP5791541B2 - Zirconia sintered body and electronic component mounting base using the same - Google Patents

Description

  The present invention relates to a zirconia sintered body and an electronic component mounting base using the same.

  It is a part of a high-speed measuring device or automatic visual inspection device that performs high-speed or automatic dimensional measurement and visual inspection of electronic components, and is used as a mounting base for holding, aligning, and transporting target electronic components. A zirconia sintered body having high wear resistance is applied. In particular, since the dimension measurement and appearance inspection of electronic parts are performed using an optical device such as a CCD camera, parts for high-speed measuring devices and automatic appearance inspection apparatuses, for example, electronic parts are arranged and transported. As the zirconia sintered body used as the electronic component mounting base, a black one is used in order to suppress reflection of light and increase the accuracy of dimensional measurement and appearance inspection.

As such a black zirconia sintered body, for example, Patent Document 1 discloses an A component (FeO, Fe ₃ O ₄ or FeO _X which is a lower oxide of Fe, Co, Ni, Cr and Ti (X < 1.5), CoO _X (X <1), NiO _X (X <1), CrO or CrO _X (X
<1.5), TiO _X (at least one of X <2)) and B component (Al ₂ O ₃ : TiO
_X 2 (X <2): Y ₂ O ₃ having a weight ratio of 60:40:10) is 0.005 to 7.0% by weight, and the balance is 2 to 5% by mole of Y ₂ O _3. There has been proposed a zirconia sintered body characterized by comprising ZrO ₂ partially stabilized in the above.

Japanese Patent Publication No. 63-37060

  However, although the zirconia sintered body described in Patent Document 1 has high mechanical properties, there is a problem that it is poor in workability and easily causes chipping during processing.

  In addition, when the zirconia sintered body described in Patent Document 1 is used, chipping occurs at the time of grinding and it cannot be processed with high accuracy, so that electronic components are aligned or transported with high accuracy. Since it becomes difficult, it was difficult to use it as a pedestal for mounting electronic components.

  The present invention has been devised to solve the above problems, and an object of the present invention is to provide a zirconia sintered body excellent in workability while maintaining high mechanical properties.

  Another object of the present invention is to provide an electronic component mounting base that can accurately align and transport electronic components and can perform dimension measurement and appearance inspection of electronic components over a long period of time. And

The zirconia sintered body of the present invention has a zirconia containing a stabilizer in an amount of 85% by mass to 93% by mass, Al in an Al ₂ O ₃ conversion of 0.1% by mass to 0.5% by mass, and Ni in an NiO conversion. in 1 wt% to 0.1 wt% or less, more than 0.5 mass% in terms _{of Cr} 2 _{O 3} Cr 5 wt% or less, Fe and _Fe 2 _{O 3} 5% by mass to 0.5% by mass in terms of the following, Si is contained in an amount of 0.05 to 0.5 mass% in terms of SiO ₂ .

  The electronic component mounting base of the present invention is made of the zirconia sintered body, and has a holding portion for holding the electronic component.

  According to the zirconia sintered body of the present invention, it is possible to achieve excellent workability while maintaining high mechanical characteristics.

  Further, according to the electronic component mounting base of the present invention, since it is made of the above-mentioned zirconia sintered body, it is possible to prevent the occurrence of chipping during processing, so that the electronic components are accurately aligned or transported. In addition, it is possible to carry out dimension measurement and appearance inspection of electronic components over a long period of time.

It is a schematic diagram which extracts a part of an example of the base for electronic component mounting for hold | maintaining an electronic component, and shows it.

  Hereinafter, an example of the zirconia sintered body of the present embodiment will be described.

The zirconia sintered body according to the present embodiment has a zirconia sintered body containing 100% by mass of zirconia and a zirconia containing 85% by mass to 95% by mass, and Al is 0.1 mass in terms of Al ₂ O _3. % To 0.5% by mass, Ni from 0.1% by mass to 1% by mass in terms of NiO, Cr from 0.5% by mass to 5% by mass in terms of Cr ₂ O ₃ , and Fe from 0.5% by mass in terms of Fe ₂ O ₃ 5% by mass or less, and Si is contained in an amount of 0.05 to 0.5% by mass in terms of SiO ₂ .

The zirconia sintered body of the present embodiment contains zirconia, Al, Ni, Cr, Fe and Si containing a stabilizer in the above range, thereby maintaining excellent mechanical properties while maintaining high mechanical properties. Can be obtained. Note that maintaining high mechanical properties means, for example, that the values of bending strength, hardness, and fracture toughness are 500 MPa or more, 10 GPa or more, and 3.5 MPa√m or more, respectively. Note that as the value of fracture toughness increases, it takes time for the grinding process, so that there is a tendency that chipping is likely to occur. Therefore, the fracture toughness is more preferably less than 5.6 Mpa√m. In addition, excellent workability means that when a zirconia sintered body is ground, crystal grains such as zirconia particles constituting the sintered body are not broken. Here, the occurrence of chipping means that when the surface of the zirconia sintered body is observed with a metal microscope after grinding, lumps of zirconia particles fall off, and an opening having a maximum diameter of 0.1 mm or more It means that the dent which has is generated.

  In addition, about the value of the mechanical characteristic of the zirconia sintered body of this embodiment, the bending strength can be measured by a three-point bending strength according to JIS R 1601-1995, and the hardness conforms to JIS R 1601-1995. The fracture toughness can be measured by the Vickers hardness (Hv), and the fracture toughness can be measured by the fracture toughness value based on the indenter press-in method (IF method) defined in JIS R 1607-1995.

  Here, when the content of zirconia including the stabilizer is 85% by mass or more and 95% by mass or less, the mechanical characteristics can be maintained high.

Further, Al is 0.1% by mass or more and 0.5% by mass or less in terms of Al ₂ O ₃ , and Ni is 0.1% in terms of NiO.
1% by mass or more and 1% by mass or less, Cr 0.5 to 5% by mass in terms of Cr ₂ O ₃ , Fe 5 to 5% by mass in terms of Fe ₂ O ₃ , Si 0.05 or more in terms of SiO ₂ It is considered that the inclusion of 0.5% by mass or less can reinforce the brittleness of the crystal grain boundaries of the zirconia sintered body, and the crystal grains such as zirconia particles are broken during grinding. Can be prevented.

Here, Al exists as an Al ₂ O ₃ phase between the crystal phases of zirconia, and can prevent cracks generated at the grain boundaries of zirconia crystals from propagating. It is thought that it can prevent that this occurs.

Further, since Ni, Cr, and Fe exist as a NiO phase, a Cr ₂ O ₃ phase, and an Fe ₂ O ₃ phase between the zirconia phases, respectively, and can improve thermal conductivity, the processing tool and the zirconia material can be improved during grinding. Propagation of frictional heat caused by friction with the sintered body can be promoted. By promoting the propagation of this frictional heat, it is considered that the thermal stress applied to the zirconia sintered body can be reduced and the generation of internal stress can be suppressed, and when the internal stress is released during grinding, the crystal particles such as zirconia It is thought that it has the effect of preventing the occurrence of burrs.

In addition, Si exists as a SiO ₂ phase between crystal phases of zirconia (grain boundaries) and acts as a binder for crystal particles such as zirconia, Al ₂ O ₃ , NiO, and Cr ₂ O _3, so that during grinding Occurrence of chipping of crystal particles such as zirconia can be prevented.

However, if the added amount of Al, Ni, Cr, Fe and Si described above is excessive, mechanical control, particularly fracture toughness becomes too high, and it takes too much time for grinding, and further processing during grinding Thermal expansion easily occurs due to frictional heat with the jig. That is, if the addition of the above-described components is excessive, it takes too much time for the grinding process, and high frictional heat is generated between the grinding part of the zirconia sintered body and the grinding jig, and the frictional heat causes the grinding part. The content ratio of each component was important because the periphery was thermally expanded and chipped crystal grains such as zirconia particles were generated. Therefore, as a result of earnest research on the optimum range of the content of Al, Ni, Cr, Fe and Si described above, the present inventor includes a stabilizer when the entire zirconia sintered body is taken as 100% by mass. Zirconia 85
% By mass to 95% by mass, Al from 0.1% to 0.5% by mass in terms of Al ₂ O ₃ , Ni from 0.1% to 1% by mass in terms of NiO, and Cr by 0.5% by mass in terms of Cr ₂ O ₃ 5% by mass or less, Fe containing 0.5 to 5% by mass in terms of Fe ₂ O ₃ and Si containing 0.05 to 0.5% by mass in terms of SiO ₂ are excellent while maintaining high mechanical properties. It was found that it is important for obtaining processability.

Moreover, it is preferable that the zirconia sintered body of this embodiment does not contain Ti. Since TiO ₂ , which is an oxide of Ti, has low thermal conductivity, if Ti is contained in the zirconia sintered body, the frictional heat generated by friction between the processing tool and the zirconia sintered body during grinding is external. May be difficult to be released, and as a result, chipping of crystal particles such as zirconia particles may occur during grinding. Therefore, in the zirconia sintered body of the present embodiment, it is preferable not to contain Ti in order to prevent generation of chipping of crystal particles such as zirconia particles.

Further, the zirconia sintered body of the present embodiment contains Y ₂ O ₃ as a zirconia stabilizer, and the content thereof is 2 mol% or more and 3.5 mol% or less with respect to the content of the zirconia component. preferable. As stabilizers for zirconia, CaO, MgO, Y ₂ O ₃ , CeO _2, Dy ₂ O _{3 and the} like are applicable, but good mechanical properties can be obtained by partially stabilizing with a small amount of addition. Therefore, Y ₂ O ₃ is preferably used as a stabilizer. When Y ₂ O ₃ is contained within the above range, generation of monoclinic crystals (monocry phase) accompanied by volume change can be suppressed, and generation of internal stress due to volume change can be suppressed, so that higher mechanical characteristics can be obtained.

When Y ₂ O ₃ is used as a zirconia stabilizer as the zirconia sintered body of the present embodiment, for example, in addition to Zr, Y, Al, Ni, Cr, Fe and Si, for example, Hf, Ca Inevitable impurities such as Cu, Zn can be included. The content of inevitable impurities such as Hf, Ca, Cu and Zn is preferably 4% by mass or less in total when the entire zirconia sintered body is 100% by mass.

Moreover, it is preferable that the zirconia sintered compact of this embodiment contains 0.5 mass% or more and 2 mass% or less of Co in conversion of CoO.

  When Co is contained in the above range, the thermal conductivity of the zirconia sintered body tends to be further increased, the thermal stress applied to the zirconia sintered body can be reduced, and the generation of internal stress can be further suppressed. Therefore, it is possible to prevent occurrence of chipping of crystal particles such as zirconia particles due to release of internal stress during grinding. Further, when Co is contained within the above range, the thermal expansion of the zirconia sintered body can be suppressed, and therefore the zirconia sintered body tends to be difficult to deform during firing.

In addition, about each component amount in conversion of the oxide of Zr, Al, Ni, Cr, Fe, Co, Si, and a stabilizer component in the zirconia sintered body of this embodiment, it is one of the zirconia sintered body. The powder can be measured by quantitative analysis with a fluorescent X-ray analyzer (manufactured by Rigaku: ZSX100e). In addition, after the pulverized powder is dissolved in a solution such as hydrochloric acid, it is measured using an ICP (Inductively Coupled Plasma) emission spectroscopic analyzer (manufactured by Shimadzu Corporation: ICPS-8100, etc.), and the amount of each component metal obtained Can also be measured by converting to an oxide.

Whether the zirconia of the zirconia sintered body contains a stabilizer may be confirmed by checking whether the stabilizer is dissolved in zirconia. As a method for this confirmation, for example, an arbitrary surface of a zirconia sintered body is subjected to X-ray diffraction measurement with an X-ray diffraction measurement apparatus (X'Pert PRO manufactured by PANalytical), and then analysis of the lattice constant of ZrO ₂ is performed. The stabilizer is dissolved in zirconia by comparing the obtained lattice constant data with the general lattice constant data described in the JCPDS card of the ZrO ₂ crystal. You can check if it is.

  The zirconia sintered body of the present embodiment preferably has a pore area occupation ratio (hereinafter referred to as void ratio) of 0.5% or less (including 0%).

If the void ratio is within the above range, higher hardness can be obtained. Furthermore, the void rate is 0.5%
The following zirconia sintered body is good because it is suppressed from increasing the number of voids even if it is ground and part of the voids are connected to the external space to form open pores. Abrasion resistance can be maintained. That is, since the zirconia sintered body is less likely to generate open pores on its surface even if it is ground, it can maintain good wear resistance with less irregularities due to the open pores.

  As for the void ratio of the zirconia sintered body of the present embodiment, the porcelain surface of the zirconia sintered body is measured by a metal microscope or SEM adjusted to an arbitrary magnification so that a range of 100 μm × 100 μm can be observed, for example. It is possible to calculate several void ratios by taking several places on the internal cross section as photographs or images, and analyzing these photographs or images with an image analyzer, and calculating the average value of them. is there. As an image analysis apparatus, for example, LUZEX-FS manufactured by Nireco Corporation may be used.

  Moreover, it is preferable that the value of the brightness index L * in the CIE1976 L * a * b * color space is 45 or less in the zirconia sintered body of the present embodiment.

If the brightness index is within the above range, the appearance of the zirconia sintered body will be black, so when using the zirconia sintered body as a pedestal for mounting electronic components, a high-speed measuring device or automatic appearance inspection device It is preferable that scattering of light such as illumination and laser light irradiated during inspection and measurement of electronic components can be suppressed, and that dimensional measurement and appearance inspection of electronic components can be favorably performed.

In addition, the value of the lightness index L * in the CIE1976 L * a * b * color space can be obtained by measuring in accordance with JIS Z 8722-2000. For example, using a color difference meter (former Minolta Co., Ltd. CR-221 or its successor model), the light source is CIE standard light source D65,
Measurement can be performed by setting the illumination light receiving method to condition a ((45-n) [45-0]) and the measurement diameter to 3 mm.

Here, in the zirconia sintered body, the value of the lightness index L * is 45 or less, and in order to maintain excellent mechanical properties and excellent workability, the entire zirconia sintered body is When 100% by mass, the stabilizer-containing zirconia is 88% by mass to 95% by mass, Al is Al
0.1 mass% or more and 0.3 mass% or less in terms of ₂ O ₃ , Ni is 0.2 mass% or more and 0.8 mass% or less in terms of NiO, Cr is 1 mass% or more and 4 mass% or less in terms of Cr ₂ O ₃ , and Fe is Fe ₂ O equivalent to ₃ 1% by mass or more and 4 wt% or less, Si and SiO ₂ 0.3 wt% 0.05 wt% in terms of the following, a Co C
What is necessary is just to contain 1 mass% or more and 2 mass% or less each in oO conversion.

  Next, an example of the manufacturing method of the zirconia sintered compact of this embodiment is shown.

First, a stabilizer Y ₂ O ₃ (for example, purity 99%) is added in an amount of 2 mol% to 3.5 mol%.
A commercially available zirconia having an average particle size of 0.5 to 3 μm manufactured by a coprecipitation method (for example,
Purity 99%) powder, aluminum oxide (for example, purity 99%) powder having an average particle size of 0.5 to 5 μm,
Prepare nickel oxide (eg purity 99%) powder, silicon oxide (eg purity 99%) powder, chromium oxide (eg purity 99%) powder and iron oxide (eg purity 99%) powder, each powder Are weighed to a predetermined ratio. Each powder after weighing is 100% by mass in total, the binder is 1 to 5% by mass, the solvent is 100% by mass, the dispersant is 0.1 to 1% by mass, weighed into the stirrer, and mixed and stirred. After making into a slurry, spray granulation is performed using a spray dryer to obtain a secondary material composed of spherical granules.

  Thereafter, the secondary material is formed into a predetermined shape by an isostatic press molding method (rubber press) or a powder press molding method, and is subjected to cutting as necessary to obtain a molded body. The zirconia sintered body of this embodiment can be obtained by firing at a temperature of 1350 to 1550 ° C. in an air atmosphere to obtain a sintered body and then grinding.

Here, when it is desired to improve the processability, a commercially available cobalt oxide (CoO) powder having a particle size of 0.5 to 5 μm is prepared, and this powder, and zirconia powder and aluminum oxide (Al ₂ O ₃ ) that have already been weighed are prepared. ) Powder, nickel oxide (NiO) powder, chromium oxide (Cr ₂ O ₃ ) powder, iron oxide (Fe ₂ O ₃ ) powder and silicon oxide (SiO ₂ ) powder in a total of 100 mass%, and the binder is 1 to 5 mass %, The solvent is 100% by mass and the dispersing agent is weighed within the range of 0.1% to 1%, and the powder, binder, solvent and dispersing agent are put into a stirrer, mixed and stirred to form a slurry. Then, after spray granulation using a spray dryer to obtain a secondary raw material consisting of spherical granules, the zirconia sintered body of this embodiment can be obtained through the same molding, firing, and grinding steps as described above. it can.

In order to make the void ratio of the zirconia sintered body 0.5% or less (including 0%), the water content of the secondary raw material powder obtained by spray granulation using a spray dryer is 0.3 to 3%. It should be a range. Within this range, the secondary raw material granules at the time of molding are well crushed so that they can be molded without gaps between the particles, and the void ratio of the zirconia sintered body should be 0.5% or less (including 0%). Can do. The water content of the secondary raw material powder can be controlled by adjusting the inlet temperature and the outlet temperature of the spray dryer.

  Next, an example of using the zirconia sintered body of the present embodiment as a pedestal for mounting electronic components for holding and transporting electronic components in a high-speed measuring device or automatic visual inspection device is shown in FIG. It explains using.

  FIG. 1 is a partial schematic diagram illustrating a part of an example of an electronic component placement base having a holding unit for holding an electronic component in a high-speed measuring device or an automatic visual inspection device.

  As shown in FIG. 1, an electronic component mounting base 1 made of a zirconia sintered body according to the present embodiment is, for example, entirely ring-shaped and can hold an electronic component 4 on the outer periphery thereof. The electronic component 4 is moved to a predetermined position in a high-speed measuring device or an automatic visual inspection device by moving in a form in which the electronic component 4 is held in the concave portion 2. At the bottom of the recess 2, for example, a groove 3 is provided for sandwiching and holding the electronic component 4. When the electronic component 4 is held, the groove 3 slightly expands, thereby sandwiching the electronic component 3. The electronic component mounting base 1 has a sufficient holding force to hold the electronic component 4. If the electronic component placing base 1 has such a structure, the electronic component 4 can be transported to the next step while performing dimension measurement and appearance inspection using an optical device such as a CCD camera.

  By the way, when the electronic component mounting base 1 is configured as described above, the concave portion 2 is worn by friction with the electronic component 4 when the electronic component 4 is held. Therefore, if the zirconia sintered body according to the present embodiment is used as the electronic component mounting base 1, chipping may occur even when a shape such as the recess 2 or the groove 3 at the bottom thereof is subjected to precise grinding. And a good electronic component mounting base 1 can be obtained. Further, by setting the value of the lightness index L * to 45 or less, it is possible to obtain a black electronic component mounting base 1 as a whole, thereby suppressing reflection of light. Measurement errors and inspection errors due to misrecognition of dimensional measurement using equipment and visual inspection are reduced, and it is possible to further improve measurement accuracy and inspection accuracy. Furthermore, the pedestal for mounting electronic parts using the zirconia sintered body of the present embodiment has high mechanical characteristics and can prevent the occurrence of chipping during processing. Therefore, the electronic parts can be accurately aligned or transported. In addition, it is possible to carry out dimension measurement and appearance inspection of electronic components over a long period of time.

  Note that the zirconia sintered body of the present embodiment can prevent generation of chipping by grinding a very delicate pattern and the like, and has good wear resistance. It can also be suitably used as a member for various decorative parts such as fishing line guide members, portable terminal parts, daily necessities, accessories, building material parts and sports equipment.

  Examples of the zirconia sintered body of the present embodiment are shown below.

  An electronic component mounting comprising the zirconia sintered body of the present embodiment in which the concave portion 2 and the groove 3 which are holding portions of the electronic component having the shape shown in FIG. 1 are provided by grinding on the outer peripheral portion of the ring-shaped sintered body. A mounting pedestal was prepared, and a test was conducted to confirm whether or not there was any chipping in the recesses 2 and grooves 3 after processing.

First, a commercially available zirconia (Y—ZrO ₂ ) powder having an average particle diameter of 1 μm and produced by a coprecipitation method with a content of Y ₂ O ₃ as a stabilizer of 3 mol% based on the zirconia component, Aluminum oxide (Al ₂ O ₃ ) powder having an average particle diameter of 1 μm, nickel oxide (NiO) powder having an average particle diameter of 1 μm, chromium oxide (Cr ₂ O ₃ ) powder having an average particle diameter of 1 μm, iron oxide having an average particle diameter of 1 μm ( Each powder of Fe ₂ O ₃ ) powder and silicon oxide (SiO ₂ ) powder having an average particle diameter of 1 μm are weighed so that each component contained in the zirconia sintered body has a mass ratio shown in Table 1. Then, after adding 3% by mass of a binder, 100% by mass of a solvent, and 0.5% by mass of a dispersing agent, which were weighed in advance, with the total amount of each powder after weighing being 100% by mass, the mixture was stirred into a slurry. The secondary raw material consisting of spherical granules is obtained by spray granulation using a spray dryer.

After that, the secondary raw material is filled in a mold of a powder press molding machine, and is molded into a predetermined shape by a powder press molding method to obtain a molded body, and then the molded body is heated to 1450 ° C. in an air atmosphere in a continuous firing furnace. Was sintered into a ring-shaped sintered body having an outer diameter of 50 mm, an inner diameter of 40 mm, and a thickness of 5 mm. After that, by using various grinding tools of count # 400 to # 1500 on a universal grinder, changing the various machining conditions at a feed rate of 50 to 300 mm / min and a cutting depth of 1 to 20 μm, the grinding ring 1 in the shape shown in FIG. 1 on the outer periphery of the sintered body, and a recess 2 having a width of 2 mm and a depth of 3 mm and a width of 0.5 m.
m, depth 1.5 mm, sample No. 2 provided with a groove 3 having a depth of 2 mm. 1-47 were obtained.

And sample no. About 1-47, the presence or absence of the generation | occurrence | production of the chip | tip at the time of a grinding process was confirmed with the metal microscope which made the naked eye and the magnification 10 time. In addition, the presence or absence of burrs, whether or not there is a trace that lumps such as zirconia particles have fallen off on the ground surface, and if the maximum diameter of the opening is 0.1 mm or more It was assumed that there was a chip, and there was no chip in the trace of degranulation where the maximum diameter of the opening was less than 0.1 mm.

  For each sample, together with a ring-shaped sintered body, a test piece for measuring three-point bending strength according to JIS R 1601-1995, a test piece for measuring Vickers hardness according to JIS R 1601-1995, Test pieces for fracture toughness measurement conforming to the indenter press-in method (IF method) specified in JIS R 1607-1995 are formed using a powder press molding method, and fired under the same conditions as above. Each sample was obtained, and the bending strength, hardness and fracture toughness were measured.

The values in Table 1 are values obtained by pulverizing a part of the sintered body for each sample and performing quantitative analysis on the obtained powder with a fluorescent X-ray analyzer (manufactured by Rigaku: ZSX100e). It is. Moreover, the amount of components of zirconia, Al, Ni, Cr, Fe and Si containing a stabilizer was measured, and the amount as an oxide was shown, and zirconia, Al, Ni, Cr, Fe containing a stabilizer and Components other than Si components are not listed in Table 1 as inevitable impurities.

From Table 1, 85% by mass to 95% by mass of zirconia containing 3 mol% of Y ₂ O ₃ , Al of 0.1% by mass to 0.5% by mass in terms of Al ₂ O ₃ , and Ni of 0.1% by mass or more in terms of NiO 1 mass%
Hereinafter, Cr is 0.5 to 5% by mass in terms of Cr ₂ O ₃ and Fe is 0.5 to 5% by mass in terms of Fe ₂ O ₃ , and Si is 0.05 to 0.5% by mass in terms of SiO ₂ Sample No. containing 2-6,9,10,13,14,17,18,21-23 and 26-28 have a bending strength and hardness of 500 MPa or more and 10 GPa or more, and a fracture toughness of 3.5 MPa√m or more. However, even when grinding was performed, no chipping was observed and the workability was good.

In addition, only the content of zirconia including the stabilizer (the total content of ZrO ₂ and Y ₂ O ₃ ) out of the range among all the components is out of the range. 7 and sample no. Sample No. 47 having a large content of zirconia including a stabilizer (total content of ZrO ₂ and Y ₂ O ₃ ). No. 7 has high mechanical properties such as bending strength, hardness and fracture toughness of 500 MPa or more, 10 GPa or more and 3.5 MPa √m or more, respectively. The processability was bad.

In addition, sample No. 1 having a small content of zirconia including the stabilizer (the total content of ZrO ₂ and Y ₂ O ₃ ). In No. 47, no chipping was observed when grinding, but the bending strength, hardness and fracture toughness were 500 MPa or less, 10 GPa or less and less than 3.5 MPa√m, respectively, and the mechanical properties were low.

In addition, Sample No. in which only the Al content (in terms of Al ₂ O ₃ ) out of the total component is out of the range. For Samples 8, 11, and 46, Sample Nos. With low Al content (in terms of Al ₂ O ₃ ) were used. In Nos. 8 and 46, chipping was observed when grinding was performed, and Sample Nos. With a high Al content (in terms of Al ₂ O ₃ ) were observed. In No. 11, no chipping was observed when grinding, but the bending strength, hardness and fracture toughness were 500 MPa or less, 10 GPa or less and less than 3.5 MPa√m, respectively, and the mechanical properties were low.

In addition, the sample No. in which only the Ni content (NiO conversion) out of the range is out of the range. Samples Nos. 12 and 45 with low Ni content (NiO equivalent) for Nos. 12, 15 and 45 show chipping when grinding, and samples with high Ni content (NiO equivalent) No. In No. 15, no chipping was observed when grinding was performed, but the bending strength, hardness and fracture toughness were 500 MPa or less, 10 GPa or less and less than 3.5 MPa√m, respectively, and the mechanical properties were low.

Moreover, only the Cr content (Cr ₂ O ₃ conversion) of all the components is out of the range. For Samples Nos. 20, 24 and 43, Sample Nos. With low Cr content (Cr ₂ O ₃ equivalent) were used. In Nos. 20 and 43, chipping was observed when grinding was performed, and Sample Nos. With a high Cr content (Cr ₂ O ₃ equivalent) were observed. In No. 24, no chipping was observed when grinding, but the bending strength, hardness and fracture toughness were 500 MPa or less, 10 GPa or less and less than 3.5 MPa√m, respectively, and the mechanical properties were low.

In addition, only the Fe content (Fe ₂ O ₃ conversion) of all the components is out of the range. For samples Nos. 25, 29 and 42, sample Nos. With low Fe content (Fe ₂ O ₃ equivalent) were used. In Nos. 25 and 42, chipping was observed when grinding was performed, and Sample Nos. With a high Fe content (Fe ₂ O ₃ equivalent) were observed. In No. 29, no chipping was observed when grinding, but the bending strength, hardness and fracture toughness were 500 MPa or less, 10 GPa or less and less than 3.5 MPa√m, respectively, and the mechanical properties were low.

In addition, sample No. 1 in which only the Si content (in terms of SiO ₂ ) out of the total component is out of the range. For Samples 16, 19, and 44, Sample Nos. With low Si content (in terms of SiO ₂ ). In Samples 16 and 44, chipping was observed when grinding was performed, and Sample Nos. With a large Si content (in terms of SiO ₂ ) were observed. In No. 19, no chipping was observed when grinding was performed, but the bending strength, hardness and fracture toughness were 500 MPa or less, 10 GPa or less and less than 3.5 MPa√m, respectively, and the mechanical properties were low.

  In addition, among all the components, the sample No. About 30-33 and 39-41, generation | occurrence | production of the chip was seen when performing the grinding process.

  In addition, among all the components, Sample No. 1 and no. For 34 to 38, although no chipping was observed when grinding was performed, the bending strength, hardness, and fracture toughness were 500 MPa or less, 10 GPa or less and less than 3.5 MPa√m, respectively, and the mechanical properties were low. .

  In addition, sample No. which does not contain any one or more components among all the components. For 39 to 46, chipping was observed when grinding was performed, and the bending strength, hardness and fracture toughness were 500 MPa or less, 10 GPa or less and less than 3.5 MPa√m, respectively, and the mechanical properties were low.

  Next, sample No. No. in which no chipping was observed when grinding was applied to an automatic visual inspection apparatus previously improved so that a ring-shaped sintered body could be attached. 1 to 6, 9 to 11, 13 to 15, 17 to 19, 21 to 24, 26 to 29, and 34 to 38 are attached, the electronic parts are actually held and operated for one week, and then the wear state of the recess 2 Was subjected to an abrasion resistance test to confirm using a metal microscope.

As a result, sample No. which is within the scope of the present embodiment. 2-6, 9, 10, 13, 14, 17, 18, 21-23 and 26-28 have a bending strength, hardness and fracture toughness of 500 MPa or more, 10 GPa, respectively.
Above and 3.5 MPa√m or more, the mechanical properties are high, and the samples that did not show any chipping when ground were not worn and have good wear resistance. I understood. Therefore, sample no. It was confirmed that 2 to 6, 9, 10, 13, 14, 17, 18, 21 to 23 and 26 to 28 can be suitably used as electronic component placement bases. Sample Nos. With bending strength, hardness and fracture toughness of 500 MPa or less, 10 GPa or less and less than 3.5 MPa√m, respectively. For 1, 11, 15, 19, 24, 29, and 34 to 38, it was confirmed that there were wear marks due to contact with the electronic components inside the recess 2.

Sample No. of Example 1 was changed except that the amount of Y ₂ O ₃ added as a stabilizer added to zirconia was changed so that the content value relative to the zirconia component would be the value shown in Table 2. In the same manner as in No. 5, sample no. 48-53 were produced. Each sample thus prepared was checked for the presence or absence of chipping during grinding as in Example 1. Moreover, bending strength, hardness, and fracture toughness were measured. The results are shown in Table 2.

From Table 2, sample No. 2 containing ₂ to 3.5 mol% of Y ₂ O ₃ as a stabilizer with respect to the zirconia component was obtained. It was found that Nos. 49 to 52 tended to have higher bending strength, hardness, and fracture toughness values. Furthermore, no chipping was observed when grinding was performed, and it was found that the processability was excellent.

Next, the content ratios of zirconia, Al ₂ O ₃ , NiO, Cr ₂ O ₃ , Fe ₂ O ₃ and SiO ₂ containing the stabilizer were determined as sample No. 1 of Example 1. Same as 21, zirconia sintered body 100
Sample No. in which Co was added so as to contain the amount shown in Table 3 in terms of CoO with respect to mass%. 54-59 were produced.

For the manufacturing method of each sample zirconia containing _Y 2 _{O 3} is a stabilizer (Y-ZrO
₂ ) 1 of powder, aluminum oxide (Al ₂ O ₃ ) powder, nickel oxide (NiO) powder, chromium oxide (Cr ₂ O ₃ ) powder, iron oxide (Fe ₂ O ₃ ) powder and silicon oxide (SiO ₂ ) powder During weighing of the secondary raw material powder, a predetermined amount of cobalt oxide (CoO) powder is weighed, and the primary raw powder after weighing is put into a stirrer together with a binder, a solvent and a dispersing agent, mixed and stirred, and during grinding processing. In order to confirm the effect of the addition of Co, the processing speed (grinding tool feed speed) was set to the same shape as in Example 1 except that the same speed as that in Example 1 was doubled. Sample Nos. 54 to 59 made of a ring-shaped sintered body having the recesses 2 and the grooves 3 shown in FIG.

  Then, each sample after production was checked in the same manner as in Example 1 for the presence or absence of chipping during grinding.

  Place the sintered ring-shaped sintered body on a surface plate, measure the gap between the two end surfaces of the surface plate and the ring-shaped sintered body using a clearance gauge, and set the maximum clearance to the ring shape. The amount of deformation of the sintered body was determined to be good when the value was 0.5 mm or less. The results are shown in Table 3.

From Table 3, sample No. 1 containing Co in an amount less than the range of 0.5% by mass or more and 2% by mass or less in terms of CoO. For 54, no chipping was observed at the same processing speed as in Example 1. However, when grinding was performed at twice the processing speed, chipping was observed on the surface of the recess 2 and the groove 5 to improve workability. The effect was low.

Further, Sample No. containing Co in an amount larger than the range of 0.5% by mass or more and 2% by mass or less in terms of CoO. As for 58, the deformation amount of the ring-shaped sintered body after firing tended to increase beyond 0.5 mm.

  Sample No. containing no Co For 59, no chipping was observed at the same processing speed as in Example 1, but chipping was observed on the surface of the concave portion 2 or the groove portion 5 when grinding was performed at twice the processing speed.

Compared to these samples, Sample No. containing Co in a range of 0.5 mass% to 2 mass% in terms of CoO. For 54 to 56, the amount of deformation is 0.5 mm or less and the recess 2 or groove 5 after grinding
There was no occurrence of cracks.

  Next, sample no. Sample No. 5 having a composition similar to that of Sample No. 5, in which the water content of the secondary raw material spray granulated with a spray dryer in the production process was variously changed to the values shown in Table 4. 60-66 were produced.

  The sample was ring-shaped using the same method as in Example 1 except that the difference between the inlet temperature and outlet temperature of the spray dryer was variously changed to the values shown in Table 2 and the water content was controlled to the values shown in Table 4. The sintered body was manufactured.

As for the water content of the secondary raw material, after cooling the secondary raw material after spray granulation to room temperature in a room with a humidity of 30% or less, a predetermined amount of the raw material is taken out and the weight before drying is measured. 100 ingredients
After drying in a dryer at ℃ or higher for 10 hours or more, measure the weight after drying again in a room with a humidity of 30% or less, calculate the weight difference before and after drying, and divide this weight difference by the weight before drying. The value after division was multiplied by 100.

  Thereafter, five SEM photographs that allow observation of a 100 μm × 100 μm range on the surface of an arbitrary sintered body are taken arbitrarily, and the photographed images are analyzed by an image analyzer (LUZEX-FS manufactured by Nireco) to obtain five places. The void ratio was calculated and the average value was obtained, and the void ratio of each sample was calculated. The results are shown in Table 4.

From Table 4, the sample No. in which the water content of the secondary raw material is in the range of 0.3 to 3%. For 61 to 65, the void ratio was 0.5% or less, which was a good value as compared with other samples.

Thereafter, sample No. with a void ratio of 0.5% or less. Sample Nos. 61-65 and over 0.5%. When a wear resistance test using an automatic visual inspection apparatus was performed for the ring-shaped sintered body with No. 60 in the same manner as in Example 1, a sample No. with a void ratio of 0.5% or less was obtained. Nos. 61 to 65 were hardly worn. Compared to 60, it was confirmed that it was less likely to wear.

1: Electronic component mounting base 2: Concave portion 3: Groove 4: Electronic component

Claims (5)

9 3 wt% zirconia 85 wt% or more containing a stabilizer or less, Al to _Al 2 _{O 3} 0.5 wt% 0.1 wt% in terms of the following, 1 mass 0.1 mass% of Ni in terms of NiO % Or less, Cr is 0.5 to 5% by mass in terms of Cr ₂ O ₃ , Fe is 0.5 to 5% by mass in terms of Fe ₂ O ₃ , and Si is 0.05 in terms of SiO ₂ A zirconia sintered body characterized by containing not less than 0.5% by mass and not more than 0.5% by mass. The zirconia sintered body according to claim 1, wherein the zirconia contains 2 mol% or more and 3.5 mol% or less of Y ₂ O ₃ as a stabilizer.   The zirconia sintered body according to claim 1 or 2, wherein Co is contained in an amount of 0.5 mass% to 2 mass% in terms of CoO.   The zirconia sintered body according to any one of claims 1 to 3, wherein a pore occupation area ratio is 0.5% or less.   An electronic component mounting base comprising the zirconia sintered body according to any one of claims 1 to 4 and having a holding portion for holding the electronic component.

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