JP2006027984A - Sintering tool made of ceramic and its manufacturing method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a sintering tool made of ceramic which is high in strength and is improved in handling quality at the time of sintering moldings, such as electronic components and is repeatedly usable and a method for manufacturing the sintering tool made of the ceramic. <P>SOLUTION: The sintering tool made of the ceramic composed of a ceramic sintered compact of 0.005 to 0.03 mm in average particle size is obtained by a method including a process of formulating a slurry by mixing a ceramic powder and a granulating agent, a process of obtaining the molding by applying the slurry on a support or mounting the same thereon and drying the slurry, and a process of sintering the molding. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a ceramic sintering jig used for sintering electronic material parts and the like, and a method for manufacturing the same.

Ceramic capacitors such as multilayer capacitors, piezoelectric materials such as piezoelectric ceramics, microwave dielectrics, multilayer LC composite chips, high frequency components such as SAW filters, semiconductor capacitors, semiconductor ceramics such as PTC thermistors, NTC thermistors, ceramic varistors, and ceramic sensors Barium titanate (BaTiO ₂ ), lead zirconate titanate (PbZrTiO ₃ ), strontium titanate (SrTiO ₃ ), zinc oxide (ZnO), zirconium oxide (ZrO ₂ ), rare earth oxides, glass materials, etc. Or a composite of these.

  Such electronic parts are generally prepared by mixing these raw materials, forming them, placing them on a ceramic sintering jig, and sintering them at 800-1400 ° C. The element is made by forming the, and finally it becomes a part by assembling.

  However, when a ceramic body is obtained by sintering a molded body containing a low melting point, low boiling point element, for example, lead, with a ceramic sintering jig such as aluminum oxide, a part of the lead is partly sintered. When a ceramic body is obtained by evaporating or sintering a compact containing a large amount of glass component near the melting temperature of the glass, the glass component melts and adheres and reacts with the ceramic sintering jig. However, due to the contamination, the electrical characteristics of the ceramic body are degraded, and the ceramic sintering jig cannot withstand repeated use.

  In addition, the thickness of the sintering jig is desirably small in order to ensure the effective volume of the molded body during sintering, but when the thickness is small, the strength tends to decrease and cracks and chips are likely to occur. This has been a problem because it has a large effect on handling properties.

In order to solve such a problem, there is a method of shot blasting a contact surface with a formed body as a method for manufacturing a ceramic sintering jig (for example, see Patent Documents 1 and 2). However, with this method, in the case of high-strength zirconium oxide such as partially stabilized zirconium oxide, it is difficult to roughen the surface by blasting. Further, when the thickness of the sintering jig is small, handling is difficult due to insufficient strength, and as a result, there is a problem that the jig cannot withstand repeated use.
JP 2002-333282 A Japanese Patent Laid-Open No. 9-157038

  An object of the present invention is to provide a ceramic sintering jig that can be used repeatedly, and further to provide a sintered body suitable for manufacturing such a jig.

  In order to achieve the above object, the present invention provides a ceramic sintering jig comprising a ceramic sintered body having an average particle diameter of 0.005 to 0.03 mm and a method for producing the same. .

  According to the present invention, as will be described below, ceramic sintering that can be used repeatedly even when the thickness of the jig for sintering is small, with less adhesion to the object to be sintered, high strength and improved handling properties A working jig can be obtained.

  The ceramic sintering jig of the present invention is made of a ceramic sintered body having an average particle diameter of 0.005 to 0.03 mm. Here, the average particle diameter means an equivalent circle diameter, and is obtained by obtaining the diameter of an equivalent circle having the same area as the area A of the substance, as represented by the following equation.

Average particle diameter (equivalent circle diameter) = 2 × (A / π) ^1/2
When the average particle diameter is smaller than 0.005 mm, the number of contact points with the sintered body increases, and when sintered near the melting temperature, it adheres and reacts with the glass component in the molten sintered body, Contaminated. Moreover, since the intensity | strength of a sintered compact falls and handling will become difficult when it is larger than 0.03 mm, it cannot endure repeated use. A more preferable average particle diameter is 0.006 to 0.025 mm, and still more preferably 0.006 to 0.02 mm. In addition, in this invention, a to-be-sintered body means the molded object sintered using the ceramic sintering jig | tool in this invention, or the sintered compact after sintering.

  Moreover, it is preferable that the standard deviation which is a parameter | index of the dispersion | variation in an average particle diameter is 0.01 mm or less. That is, if the standard deviation is small, the quality is stable and management is easy, and if it exceeds 0.01 mm, the strength of the sintered body is not stable and the production efficiency may be reduced. More preferably, it is 0.008 mm or less.

  Furthermore, in the ceramic sintering jig of the present invention, the thickness of the ceramic sintered body constituting the ceramic jig is preferably 0.05 to 0.5 mm. In other words, the smaller the thickness of the jig, the more effective the sintering space can be used, and the more the thickness exceeds 0.5 mm, the more the jig occupies the sintering space, and the lower the production efficiency of electronic parts and the like. There is a case. On the other hand, when the thickness of the jig is less than 0.05 mm, the strength of the jig itself is lowered and handling becomes difficult, and it may not be able to withstand repeated use. A more preferred range is 0.1 to 0.4 mm, and even more preferred is 0.1 to 0.3 mm.

Furthermore, in the ceramic sintering jig of the present invention, the density of the ceramic sintered body constituting the ceramic jig is preferably 95% or more of the theoretical density. That is, when the density of the ceramic sintered body is less than 95% of the theoretical density, the strength of the jig is lowered and handling becomes difficult, and it may not be able to withstand repeated use. More preferably, it is 97% or more. The density can be obtained by an Archimedes method with about 20 g of a ceramic sintering jig placed in a container. As is well known, the theoretical density is calculated from a complete crystal lattice. For example, in the case of cubic zirconium oxide stabilized with yttrium oxide, 6.0 g / cm ³ , In the case of aluminum oxide, it is 4.0 g / cm ³ . For those containing different types of ceramics, calculation may be made according to the weight ratio of each ceramic. For example, when the ceramics of theoretical density D ₁ (g / cm ³ ) and D ₂ (g / cm ³ ) are 60% by weight and 40% by weight, respectively, D ₁ × (60/100) + D ₂ × ( 40/100).

  Furthermore, the ceramic sintering jig of the present invention preferably has a surface roughness (Ra) of the surface in contact with the sintered body of 0.7 to 5 μm. That is, when the surface roughness (Ra) of such a jig is less than 0.7 μm, the contact area with the object to be sintered increases, and it may be difficult to obtain the effect of preventing contact. On the other hand, if the surface roughness (Ra) of the jig exceeds 5 μm, the molded body may be deformed during sintering, and the surface of the jig is roughened using shot blasting. This may cause damage to the jig and reduce productivity. A more preferred range is 0.8 to 4 μm, and even more preferred is 1 to 3 μm. The surface roughness (Ra) in the present invention is based on a measurement method according to JIS B0601-1994 “Definition and display of arithmetic average roughness (Ra)”.

  Furthermore, the ceramic sintering jig of the present invention preferably has a warpage rate of the ceramic sintered body of 0.5% or less. That is, the smaller the warpage rate of such a jig, the more preferable it is because the deformation of the sintered body can be suppressed, and when it exceeds 0.5%, the deformation of the sintered body may occur. May decrease. More preferably, it is 0.4% or less, and still more preferably 0.3% or less. The warpage rate is greatly influenced by the distance between the powders constituting the ceramic sintered body. For example, by appropriately selecting the BET specific surface area of the powder constituting the ceramic sintered body and the addition amount of the granulating agent. It can be controlled. In addition, the warpage rate is rigid such as a brass plate, and on a flat plate, one side of the measurement sample in the longitudinal direction is rigid such as a brass plate and pressed by a flat plate. The vertical height Hmm from the upper surface of the brass plate on which the measurement sample is placed is measured, and is divided by the length Lmm in the longitudinal direction: the warpage rate = H / L × 100 (%).

  Furthermore, in the ceramic sintering jig of the present invention, from the viewpoint of strength and toughness, the ceramic sintered body suitable for manufacturing the jig is made of zirconium oxide, aluminum oxide, silicon oxide, silicon nitride, silicon carbide. It is preferable to include at least one selected, and a mixture thereof may be used, and it is preferable that the strength and toughness are excellent. Especially, the viewpoint of the manufacturing method mentioned later that the main component of a sintered compact is a zirconium oxide and contains 6-20 mol% of at least any 1 sort (s) of a yttrium oxide, a calcium oxide, magnesium oxide, and rare earth oxides. To preferred. Even more preferably, it is zirconium oxide stabilized in a cubic system containing yttrium oxide in a range of 7 to 9 mol%.

  Next, the method for producing the ceramic sintering jig of the present invention will be described by way of example. First, a ceramic powder and a granulating agent are mixed to prepare a slurry. For mixing, a ball mill or an attritor mill can be used. As the ceramic powder, zirconium oxide powder, aluminum oxide powder, silicon oxide powder, silicon nitride powder, and silicon carbide powder excellent in strength and toughness can be used. A mixed powder of these ceramic powders may be used. Among them, it is preferable to contain 6 to 20 mol% of at least one of zirconium oxide powder excellent in strength and toughness, and yttrium oxide, calcium oxide, magnesium oxide and rare earth oxide. Here, if the content is too small or too large, the size of the particles of the sintered body of the ceramic sintering jig may not be stable. More preferably, it is a zirconium oxide powder containing yttrium oxide in a range of 7 to 9 mol%. If necessary, a slurry may be prepared by adding an additive such as a plasticizer. Examples of the plasticizer include di-n-butyl phthalate and di-n-octyl phthalate.

The BET specific surface area of the ceramic powder is preferably 3 to 15 m ² / g. The BET specific surface area in the present invention refers to a value measured by the BET 1-point method in accordance with the method for measuring the specific surface area according to JIS R1626 “Gas adsorption BET method of fine ceramic powder”. When the BET specific surface area is less than 3 m ² / g, the sinterability is lowered, and a dense and uniform sintered body may not be obtained. In addition, when the BET specific surface area exceeds 15 m ² / g, the particles are fine and the moldability tends to decrease. Furthermore, the crystal grains grow too early during the sintering, and aggregation may occur, resulting in a non-uniform sintered body. Moreover, when the powder in this range is used, it is possible to easily stabilize the average particle size particle size of the sintered body of the ceramic sintering jig within the range of 0.005 to 0.03 mm. . A more preferable BET specific surface area is 5 to 10 m ² / g.

  The average particle size of the ceramic powder (secondary particle size in the slurry) is preferably in the range of 0.1 to 3 μm because the strength of the ceramic sintered body obtained tends to decrease if it is too small or too large. Is within. Moreover, when the powder in this range is used, it is possible to easily stabilize the average particle diameter of the sintered body of the ceramic sintering jig within the range of 0.005 to 0.03 mm. Even more preferably, it is in the range of 0.2 to 1 μm. More preferably, it exists in the range of 0.3-0.8 micrometer. The average particle diameter can be measured using, for example, a scattering type particle size distribution measuring device.

  As a granulating agent, at least 1 sort (s) from water, an organic solvent, and a binder can be used. Here, examples of the organic solvent include alcohols such as methanol, ethanol, propanol and butanol, hydrocarbons such as toluene, xylene, cyclohexane and petroleum solvents, ketones such as acetone and 2-butanone, ethyl acetate and butyl acetate. May be selected from esters such as ethyl cellosolve, glycol ethers such as propylene glycol monomethyl ether, and the like. Examples of the binder include polyvinyl alcohol, polyethyl methacrylate, poly n-butyl methacrylate, polyisobutyl methacrylate, polymethyl methacrylate, and the like, and even in a mixture of these polymers, the monomers constituting these polymers A copolymer may also be used.

  Next, the slurry is applied or placed on a support and dried to obtain a molded body. The slurry is applied or placed on the support, particularly when a sintered body having a relatively small thickness of about 0.05 to 0.5 mm is obtained, generally formed by a press forming method used for forming. This is because it is difficult to do so, and cracks and chips may occur. Here, it is preferable to use, for example, a film-like polyethylene terephthalate (hereinafter referred to as PET film), polyphenylene sulfide (hereinafter referred to as PPS film), a glass plate, or the like as the support on which the slurry is applied.

  Moreover, the thickness of a support body should just be the thickness which is easy to handle with the thickness of the molded object obtained. For example, if a 0.2 mm molded body is to be obtained, a support of about 0.1 mm is used.

  In addition, as a method of applying or placing the slurry on the support, a doctor blade method, an extrusion method, or the like can be used.

  Next, the compact is sintered to obtain a ceramic sintering jig. Sintering conditions, that is, the sintering temperature and the sintering time, the density is 95% or more of the theoretical density so that the strength of the ceramic sintering jig to be obtained does not decrease and damage such as breakage does not occur during use. It is preferable to select as follows. Sintering conditions vary depending on the type of ceramic powder used. For example, when zirconium oxide powder or aluminum oxide powder is used, the temperature is preferably set to 1,450 to 1,800 ° C. for 1 to 5 hours. Under this temperature condition, it is possible to easily stabilize the average particle size of the sintered body of the ceramic sintering jig within the range of 0.005 to 0.03 mm. More preferably, it is 1,500-1,700 degreeC and 1 to 5 hours.

  Further, in order to roughen the sintered body, the surface with which the sintered body is in contact can be shot blasted. Shot blasting is performed by projecting shot material. As the shot material, a ceramic material, a hard metal material, or the like can be used. For example, silicon carbide, aluminum oxide, zirconium oxide, glass beads, etc. can be employed as the ceramic shot material. The size of the shot material is preferably 30 to 200 mesh.

  The ceramic sintering jig according to the present invention is, for example, for sintering when a molded body such as a ceramic capacitor or a high-frequency component composed of barium titanate, lead zirconate titanate or the like is used in the field of electronic materials. It can be suitably used as a jig.

Hereinafter, the present invention will be specifically described with reference to examples. In addition, the determination of the “strength” of the sintered body in the examples is made based on whether the handling property is good or not, and the obtained sintered body is repeatedly used 10 times. Although it was not impossible to use, it was judged as “difficult to use” when it was difficult to use due to adhesion, deformation, cracking, chipping, etc. in the middle when it was slightly inferior when it was slightly chipped.
Example 1:
Stabilized zirconium oxide powder containing 8 mol% of yttrium oxide having a BET specific surface area of 7.7 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of the mixture was mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed. After defoaming, the slurry was molded and dried to a thickness of 0.2 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

  Next, the obtained molded body was cut into a 30 × 30 mm shape, sintered in air at 1600 ° C. for 2 hours, and then subjected to shot blasting. The specifications of the sintered zirconium oxide were as follows.

Sintered body average particle diameter: 0.01 mm
Sintered body thickness: 0.18 mm
Density: 5.9 g / cm ³ (98% of theoretical density)
Surface roughness (Ra): 1.5 μm
Warpage rate: 0.1%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a molded body made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, the sintering jig and the sintered body were not bonded, and the sintered body was not deformed. Further, the strength was satisfactory and the handling property was good, and repeated use was possible.
Example 2:
Stabilized zirconium oxide powder containing 8 mol% of yttrium oxide having a BET specific surface area of 7.7 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight , Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of the mixture was mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed. After defoaming, the slurry was molded and dried to a thickness of 0.2 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

  Next, the obtained molded body was cut into a shape of 30 × 30 mm, sintered in air at 1700 ° C. for 2 hours, and then subjected to shot blasting. The specifications of the sintered zirconium oxide were as follows.

Sintered body average particle diameter: 0.02 mm
Sintered body thickness: 0.18 mm
Density: 5.9 g / cm ³ (98% of theoretical density)
Surface roughness (Ra): 2 μm
Warpage rate: 0.1%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a molded body made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, the sintering jig and the sintered body were not bonded, and the sintered body was not deformed. Further, the strength was satisfactory and the handling property was good, and repeated use was possible.
Example 3:
Stabilized zirconium oxide powder containing 8 mol% of yttrium oxide having a BET specific surface area of 7.7 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of the mixture was mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed. After defoaming, the slurry was molded and dried to a thickness of 0.06 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

  Next, the obtained molded body was cut into a 30 × 30 mm shape, sintered in air at 1600 ° C. for 2 hours, and then subjected to shot blasting. The specifications of the sintered zirconium oxide were as follows.

Sintered body average particle size: 0.01 m
Sintered body thickness: 0.045 mm
Density: 5.9 g / cm ³ (98% of theoretical density)
Surface roughness Ra: 0.7 μm
Warpage rate: 0.3%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a molded body made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, since the strength is lower than in Examples 1 and 2, the handling property is slightly inferior, but it can be used, and the sintering jig and the sintered body are not bonded, and the sintered body There was no deformation. Moreover, repeated use was possible.
Example 4:
Stabilized zirconium oxide powder containing 8 mol% of yttrium oxide having a BET specific surface area of 12 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight, Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of the mixture was mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed After defoaming, the slurry was molded and dried to a thickness of 0.2 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

  Next, the obtained molded body was cut into a shape of 30 × 30 mm, sintered in air at 1250 ° C. for 2 hours, and then shot blasted. The specifications of the sintered zirconium oxide were as follows.

Sintered body average particle size: 0.01 m
Sintered body thickness: 0.19 mm
Density: 5.6 g / cm ³ (93% of theoretical density)
Surface roughness Ra: 1.5 μm
Warpage rate: 0.1%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a molded body made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, since the strength is lower than in Examples 1 and 2, the handling property is slightly inferior, but it can be used, and the sintering jig and the sintered body are not bonded, and the sintered body There was no deformation. Moreover, repeated use was possible.
Example 5:
Stabilized zirconium oxide powder containing 8 mol% of yttrium oxide having a BET specific surface area of 7.7 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight , Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of the mixture was mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed. After defoaming, the slurry was molded and dried to a thickness of 0.2 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

  Next, the obtained molded body was cut into a 30 × 30 mm shape and then sintered in air at 1600 ° C. for 2 hours. The specifications of the sintered zirconium oxide were as follows.

Sintered body average particle size: 0.01 m
Sintered body thickness: 0.18 mm
Density: 5.9 g / cm ³ (98% of theoretical density)
Surface roughness Ra: 0.1 μm
Warpage rate: 0.1%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a molded body made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, compared with Examples 1 and 2, there was slight adhesion between the sintering jig and the object to be sintered, but it was easily peeled off and the jig was not contaminated. Further, there was no deformation of the sintered body. Also, the strength was satisfactory and the handleability was good, and repeated use was possible.
Example 6:
Stabilized zirconium oxide powder containing 8 mol% of yttrium oxide having a BET specific surface area of 7.7 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of the mixture was mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed. After defoaming, the slurry was molded and dried to a thickness of 0.2 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

  Next, the obtained molded body was cut into a 30 × 30 mm shape, sintered in air at 1600 ° C. for 2 hours, and then subjected to shot blasting only on one side of the sintered body. The specifications of the sintered zirconium oxide were as follows.

Sintered body average particle size: 0.01 m
Sintered body thickness: 0.18 mm
Density: 5.9 g / cm ³
Surface roughness Ra: 1.5 μm
Warpage rate: 0.6%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a molded body made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, since the shape of the sintering jig was slightly inferior to that of Examples 1 and 2, the deformation of the sintered body was within the allowable range, but was slight. Further, there was no adhesion between the sintering jig and the object to be sintered. Moreover, there was no problem with the strength, the handling property was good, and repeated use was possible.
Example 7:
Zirconium oxide powder containing 5 mol% of yttrium oxide having a BET specific surface area of 7.7 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight, Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of the mixture was mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed After defoaming, the slurry was molded and dried to a thickness of 0.2 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

Next, the obtained molded body was cut into a 30 × 30 mm shape, sintered in air at 1600 ° C. for 2 hours, and then subjected to shot blasting. The specifications of the sintered zirconium oxide were as follows.
Sintered body average particle size: 0.005 mm
Sintered body thickness: 0.18 mm
Density: 5.9 g / cm ³ (98% of theoretical density)
Surface roughness Ra: 0.7 μm
Warpage rate: 0.1%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a compact made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, there was no deformation of the sintered body, but there was a slight adhesion between the sintering jig and the sintered body as compared with Examples 1 and 2, but it was easily peeled off and the jig was removed. There was no contamination. Moreover, there was no problem with the strength, the handling property was good, and repeated use was possible.
Example 8:
Stabilized zirconium oxide powder containing 8 mol% of yttrium oxide having a BET specific surface area of 2.5 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight , Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of the mixture was mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed. After defoaming, the slurry was molded and dried to a thickness of 0.2 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

Next, the obtained molded body was cut into a 30 × 30 mm shape, sintered in air at 1800 ° C. for 2 hours, and then subjected to shot blasting. The specifications of the sintered zirconium oxide were as follows.
Sintered body average particle diameter: 0.02 mm
Sintered body thickness: 0.18 mm
Density: 5.7 g / cm ³ (95% of theoretical density)
Surface roughness Ra: 2 μm
Warpage rate: 0.1%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a molded body made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, since the strength is lower than in Examples 1 and 2, the handling property is slightly inferior, but it can be used, and the sintering jig and the sintered body are not bonded, and the sintered body There was no deformation. Moreover, repeated use was possible.
Comparative Example 1:
Zirconium oxide powder containing 3 mol% of yttrium oxide having a BET specific surface area of 7.7 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight, Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of a mixture were mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed After defoaming, the slurry was molded and dried to a thickness of 0.2 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

  Next, the obtained molded body was cut into a 30 × 30 mm shape, sintered in air at 1450 ° C. for 2 hours, and then subjected to shot blasting. The specifications of the sintered zirconium oxide were as follows.

Sintered body average particle size: 0.001 μm
Sintered body thickness: 0.18 mm
Density: 6 g / cm ³ (98% of theoretical density)
Surface roughness Ra: 0.1 μm
Warpage rate: 0.1%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a molded body made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, the sintering jig and the object to be sintered were bonded and could not be used repeatedly.
Comparative Example 2:
Stabilized zirconium oxide powder containing 8 mol% of yttrium oxide having a BET specific surface area of 7.7 m ² / g and an average particle diameter of 0.5 μm: 100 parts by weight, toluene: 30 parts by weight, 2-propanol: 30 parts by weight Kyoeisha Chemical Oricox KC-800 (trade name): 10 parts by weight, di-n-butyl phthalate: 5 parts by weight of the mixture was mixed in a ball mill using zirconium oxide balls for 24 hours, and the resulting slurry was vacuumed. After defoaming, the slurry was molded and dried to a thickness of 0.2 mm on a polyethylene terephthalate film with a release agent using a doctor blade coater to obtain a molded body.

Next, the obtained molded body was cut into a 30 × 30 mm shape, sintered in air at 1800 ° C. for 2 hours, and then subjected to shot blasting. The specifications of the sintered zirconium oxide were as follows.
Sintered body average particle diameter: 0.04 mm
Sintered body thickness: 0.18 mm
Density: 5.9 g / cm ³ (98% of theoretical density)
Surface roughness Ra: 2.5 μm
Warpage rate: 0.1%
Here, using this zirconium oxide sintered body as a ceramic sintering jig, a molded body made of barium titanate was placed and sintered in air at 1300 ° C. for 2 hours. As a result, there was no adhesion between the sintering jig and the object to be sintered, and there was no deformation of the object to be sintered.

Claims (13)

  A ceramic sintering jig comprising a ceramic sintered body, wherein the ceramic sintered body has an average particle diameter of 0.005 to 0.03 mm.   The ceramic sintering jig according to claim 1, wherein the thickness of the ceramic sintered body is 0.05 to 0.5 mm.   The ceramic sintering jig according to claim 1 or 2, comprising a ceramic sintered body having a density of 95% or more of a theoretical density.   The ceramic sintering jig according to any one of claims 1 to 3, wherein the surface roughness Ra of the surface in contact with the sintered body is 0.7 to 5 µm.   The ceramic sintering jig according to any one of claims 1 to 4, wherein a warpage rate of the ceramic sintered body is 0.5% or less.   The ceramic sintering jig according to claim 1, wherein the ceramic sintered body includes at least one selected from zirconium oxide, aluminum oxide, silicon oxide, silicon nitride, and silicon carbide. .   The main component of the ceramic sintered body is zirconium oxide, and contains 6 to 20 mol% of at least one of yttrium oxide, calcium oxide, magnesium oxide, and rare earth oxide. The ceramic sintering jig described in 1.   A step of mixing a ceramic powder and a granulating agent to prepare a slurry, a step of applying or placing the slurry on a support and drying to obtain a formed body, and a step of sintering the formed body A method for manufacturing a ceramic sintering jig comprising:   The method for manufacturing a ceramic sintering jig according to claim 8, wherein the ceramic powder includes at least one selected from zirconium oxide powder, aluminum oxide powder, silicon oxide powder, silicon nitride powder, and silicon carbide powder.   10. The ceramic product according to claim 8, wherein the main component of the ceramic powder is zirconium oxide and contains 6 to 20 mol% of at least one of yttrium oxide, calcium oxide, magnesium oxide, and rare earth oxide. A method for manufacturing a sintering jig. The ceramic sintering jig according to claim 8, wherein the ceramic powder has a BET specific surface area of 3 to 15 m ² / g and an average particle diameter in the slurry of 0.1 to 3 μm. Manufacturing method.   The method for manufacturing a ceramic sintering jig according to any one of claims 8 to 11, wherein a sintering temperature in the step of sintering the compact is 1450 to 1800 ° C.   The method for manufacturing a ceramic sintering jig according to any one of claims 8 to 12, comprising a step of shot blasting a surface in contact with a sintered body.