WO2021248813A1 - Céramique d'alumine et procédé de préparation s'y rapportant - Google Patents

Céramique d'alumine et procédé de préparation s'y rapportant Download PDF

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WO2021248813A1
WO2021248813A1 PCT/CN2020/128669 CN2020128669W WO2021248813A1 WO 2021248813 A1 WO2021248813 A1 WO 2021248813A1 CN 2020128669 W CN2020128669 W CN 2020128669W WO 2021248813 A1 WO2021248813 A1 WO 2021248813A1
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alumina
slurry
powder
sintering
dispersant
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Chinese (zh)
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甘志俭
程银兵
杨斌
庄志杰
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基迈克材料科技（苏州）有限公司
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Definitions

  • the invention relates to the technical field of ceramics, in particular to an alumina ceramic and a preparation method thereof.
  • the content of alumina in high-purity alumina powder is greater than 99wt%, and it has the characteristics of uniform particle size, easy dispersion, stable chemical properties, etc. It has incomparable optical, electrical, magnetic, and thermal properties that ordinary alumina powder (alumina content greater than 80wt%) cannot match. And mechanical properties, high-purity alumina ceramics have been widely used as anti-plasma erosion materials in semiconductor and liquid crystal display etching manufacturing equipment. Among semiconductor equipment, the value of precision ceramics accounts for about 20% of the equipment value, and the global market has an output value of approximately US$6 billion. The production of semiconductor alumina precision ceramic components is in its infancy in China. The current accelerated development of the domestic semiconductor industry will inevitably lead to an increase in the demand for semiconductor alumina precision ceramics.
  • alumina ceramics are different. Among them, a large number of methods used in industrial production are isostatic pressing, high temperature sintering, grinding processing, polishing and other processes. This method is mainly suitable for alumina ceramics with a purity of 95%. , But it is not suitable for other alumina ceramics such as alumina ceramics with a purity of 99%.
  • the alumina ceramics prepared by the above methods have problems such as low density and low mechanical strength of the ceramics, and cannot meet the requirements of semiconductor devices for alumina ceramics.
  • alumina ceramic and a preparation method thereof that can improve the density and mechanical properties.
  • a method for preparing alumina ceramics which includes the following steps:
  • the alumina powder is made into a slurry to obtain an alumina slurry with a particle size D90 less than or equal to 0.8 ⁇ m; the alumina slurry is dried to obtain alumina fine powder; the content of alumina in the alumina powder is ⁇ 99wt%;
  • the first dispersant and the lubricant are heated and melted, the alumina fine powder and the ultraviolet light absorber are added, mixed uniformly, and then vacuumed to obtain an alumina light-cured slurry;
  • the conditions of the normal pressure debinding and sintering are: heating up to 550°C to 650°C at a rate of (0.2 ⁇ 1)°C/min, holding for 6h to 10h, and then heating up to 1200°C at a rate of (1 ⁇ 5)°C/min ⁇ 1400°C, keep for 5h ⁇ 8h.
  • the above preparation method uses high-purity alumina powder as a raw material to obtain alumina slurry with D90 ⁇ 0.8 ⁇ m through ball milling, and then dry to prepare nano-scale, high-activity spherical alumina fine powder, which is then made into a light-curing slurry.
  • 3D printing is used to form a blank to meet the requirements of semiconductor equipment for ceramic shape and dimensional accuracy. It is often pressed and sintered at low temperature to make alumina ceramics. Due to the small particle size and high sintering activity of alumina fine powder, sintering can be completed within 1400 °C, and the sintered alumina grains at low temperature will not undergo abnormal mutations.
  • the grain size is uniform, and high-density, high-density, high-density, Alumina ceramics with high mechanical properties meet the demand for alumina ceramics in semiconductor equipment.
  • the alumina ceramic body of this method can be sintered under normal pressure and within 1400°C. Therefore, the sintering requirements can be met by using an ordinary normal pressure sintering furnace, which can reduce equipment cost input, and the sintering temperature is low, which can greatly reduce Energy costs.
  • the content of alumina in the alumina powder is ⁇ 99.99%
  • the D50 is 0.3 ⁇ m to 0.6 ⁇ m
  • the BET is 10 m 2 /g to 20 m 2 /g.
  • the conditions for the normal pressure debinding and sintering are: heating up to 600°C at a rate of (0.2 ⁇ 1)°C/min, holding for 6h ⁇ 10h, and then at a rate of (2 ⁇ 5)°C/min Raise the temperature to 1200°C ⁇ 1400°C and keep it for 6h ⁇ 8h.
  • the aluminum oxide particles are 80 to 85 parts
  • the photosensitive resin is 5 to 10 parts
  • the first dispersant is 1-10 parts
  • the lubricant is 2-10 parts
  • the ultraviolet light absorber is 1-5 parts.
  • the photosensitive resin is selected from at least one of epoxy acrylic resin, urethane acrylic resin, and polyester acrylic resin.
  • the first dispersant is selected from at least one of stearic acid, oleic acid, and polyethylene glycol.
  • the lubricant is selected from at least one of paraffin wax and glycerin.
  • the ultraviolet light absorber is selected from at least one of phenyl salicylate, 2,4-dihydroxybenzophenone, and resorcinol monobenzoate.
  • the step of preparing alumina powder into a slurry is: after mixing water, a second dispersant and the high-purity alumina powder, ball milling for 2h-6h, the high-purity alumina
  • the weight ratio of the powder to the water is (4-7):(3-6)
  • the weight of the second dispersant is 1% to 3% of the high-purity alumina powder
  • the second dispersant For organic solvents.
  • the second dispersant is selected from at least one of polyvinyl alcohol, polyethylene glycol, and polystyrene.
  • the drying adopts a spray drying method, and the inlet air temperature of the drying is 250° C. to 350° C., the outlet air temperature is 100° C. to 150° C., and the rotation speed is 9000 rpm to 12000 rpm.
  • the step of grinding and polishing the alumina ceramic is further included to control the surface roughness Ra of the alumina ceramic after grinding and polishing Ra ⁇ 0.1 ⁇ m.
  • an alumina ceramic is provided, which is prepared by the above-mentioned preparation method of alumina ceramic.
  • FIG. 1 is a schematic diagram of a method for preparing alumina ceramics according to an embodiment.
  • the molding methods of alumina ceramic products mainly adopt dry pressing, grouting, extrusion, cold isostatic pressing, injection, casting, hot pressing and hot isostatic pressing. These molding methods are not easy to prepare with complex shapes and sizes. The problem of high-precision green bodies.
  • the present invention uses high-purity alumina as a raw material, combined with a 3D printing molding method, and then performs low-temperature and atmospheric sintering at 1400°C and below to prepare alumina ceramics with high density, fine grains, and high mechanical properties. Meet the requirements of semiconductor equipment for alumina ceramics.
  • An embodiment of the present invention provides a method for preparing an alumina ceramic sintered body, as shown in FIG. 1, including the following steps S10 to S18.
  • the alumina powder is made into a slurry and dried to obtain alumina fine powder.
  • alumina powder with alumina content ⁇ 99wt% is made into slurry to obtain alumina slurry with particle size D90 ⁇ 0.8 ⁇ m, and then dried to obtain alumina fine powder.
  • the content of alumina in the alumina powder is ⁇ 99.99 wt%
  • the D50 is 0.3 ⁇ m to 0.6 ⁇ m
  • the BET (specific surface area) is 10 m 2 /g to 20 m 2 /g.
  • D90 represents the particle size whose cumulative distribution of particles is 90%, that is, the volume content of particles smaller than this size accounts for 90% of all particles.
  • D50 represents the particle size at which the cumulative distribution of particles is 50%, also called median particle.
  • a D50 of 0.3 ⁇ m to 0.6 ⁇ m means that the volume of particles with a particle size of 0.3 ⁇ m to 0.6 ⁇ m in the alumina powder accounts for 50%, and the volume of particles smaller than 0.3 ⁇ m and larger than 0.6 ⁇ m accounts for 50%.
  • the step of preparing the alumina powder into a slurry is: after mixing the ball milling medium, the second dispersant and the alumina powder, ball milling for 2h-6h, the weight ratio of the alumina powder to the ball milling medium is (4 ⁇ 7): (3 ⁇ 6), the weight of the second dispersant is 1% ⁇ 3% of the high purity alumina powder.
  • the ball milling medium is selected from water and volatile organic solvents; preferably, the ball milling medium is water.
  • the second dispersant is selected from at least one of polyvinyl alcohol, polyethylene glycol and polystyrene; preferably, the second dispersant is polyvinyl alcohol.
  • high-purity alumina powder is added, and after stirring to form a slurry, ball milling is performed in a high-speed nano-sand mill.
  • the high-purity alumina powder accounts for 40% to 70% of the total weight of the high-purity alumina powder and the ball milling medium, and the weight of the second dispersant is 1% to 3% of the weight of the high-purity alumina powder.
  • Use water as the ball milling medium and alumina ball as the milling ball is 2h-6h, and the particle size of the slurry obtained after ball milling is D90 ⁇ 0.8 ⁇ m.
  • a centrifugal spray dryer is used for spray drying, and the centrifugal drying of spray drying has an inlet air temperature of 250°C to 350°C, an outlet temperature of 100°C to 150°C, and an atomization speed of 9000rpm to 12000rpm to prepare Nano-level, high bulk density spherical alumina fine powder.
  • the first dispersant and the lubricant are heated and melted, the alumina fine powder and the ultraviolet light absorber are added, mixed uniformly, and then vacuumed to obtain the alumina light-cured slurry.
  • the amount of alumina fine powder is 80 to 85 parts by weight, the photosensitive resin is 5 to 10 parts, and the first dispersant is 1 to 10 parts.
  • the amount of the agent is 2-10 parts, and the amount of the ultraviolet light absorber is 1-5 parts.
  • the photosensitive resin is selected from at least one of polyacrylic resin, epoxy acrylic resin, urethane acrylic resin, and polyester acrylic resin;
  • the first dispersant is selected from stearic acid, oleic acid, and polyethylene glycol
  • the lubricant is selected from paraffin wax and/or glycerin;
  • the ultraviolet light absorber is selected from at least one of phenyl salicylate, 2,4-dihydroxybenzophenone and resorcinol monobenzoate A sort of.
  • the photosensitive resin is a polyacrylic resin
  • the first dispersant is stearic acid
  • the lubricant is paraffin wax
  • the ultraviolet light absorber is phenyl salicylate.
  • the polyacrylic resin is melted at 190°C ⁇ 200°C, after cooling to 100°C ⁇ 120°C, stearic acid is added, after melting, the temperature is reduced to 80°C ⁇ 100°C, paraffin wax is added to melt, and after the organic fat is completely melted, Continue to add alumina fine powder under stirring. After the addition is complete, add ultraviolet light absorber and continue to stir for 2h ⁇ 4h until the slurry is uniformly mixed. Then vacuum treatment is carried out to eliminate bubbles in the slurry to obtain aluminum oxide light curing Slurry. In this way, defects such as holes in the aluminum oxide light-curing slurry can be avoided during molding.
  • the alumina light-cured slurry prepared in step S12 is printed and molded by a 3D printer according to the design drawings to obtain an alumina ceramic body.
  • 3D printing molding can meet the requirements of semiconductor equipment for shape complex and high dimensional accuracy, and high production efficiency.
  • the alumina ceramic body undergoes atmospheric pressure debinding and sintering to obtain alumina ceramics.
  • the conditions for normal pressure debinding and sintering are: heating up to 550°C to 650°C at a rate of (0.2 ⁇ 1)°C/min, holding for 6h to 10h, and then heating up to 1200°C at a rate of (1 ⁇ 5)°C/min °C ⁇ 1400°C, keep for 5h ⁇ 8h.
  • the present invention uses nano-grade high-purity alumina powder as the raw material, can complete debinding and sintering at 1400°C or less, and can avoid the excessively large sintering temperature (such as 1600°C ⁇ 1700°C) causing part of the crystal grain size in the ceramic to be too large.
  • the mechanical strength of the body is reduced and it is easy to crack.
  • the ceramic grain size obtained by sintering is uniform, high density, and high mechanical properties, which can meet the needs of alumina ceramics for semiconductor equipment.
  • the conditions for normal pressure debinding and sintering are: heating up to 600°C at a rate of (0.2 ⁇ 1)°C/min, holding for 6h-10h, and then heating up to 1200°C at a rate of (2 ⁇ 5)°C/min °C ⁇ 1400°C, keep for 6h ⁇ 8h.
  • an atmospheric pressure sintering furnace is used to perform debinding and sintering of the alumina ceramic body.
  • the debinding and sintering work can be completed at one time, avoiding the need to cool down and then increase the temperature to perform the sintering operation after the debinding furnace is used alone to complete the debinding.
  • it can save the installation of debinding equipment, shorten the sintering time and improve production efficiency.
  • a CNC grinder is used to perform fine processing operations such as surface grinding, drilling, and grooving on the sintered alumina ceramic.
  • the alumina ceramic is polished with a neutral polishing liquid, and the surface roughness Ra of the alumina ceramic is controlled by grinding and polishing to be less than or equal to 0.1 ⁇ m.
  • Another embodiment of the present invention provides an alumina ceramic prepared by the above preparation method.
  • the alumina ceramic has high density and good mechanical properties, and can meet the requirements of semiconductor equipment for ceramic materials.
  • the surface roughness Ra of the alumina ceramic is less than or equal to 0.1 ⁇ m.
  • the alumina ceramic prepared by the above method of the present invention has a density of 3.9g/cm 3 and above, a compressive strength>2600Mpa, a volume resistivity>10 14 ⁇ cm, a hardness (HRA) of 88, and a flexural strength of 350MPa ⁇ 360MPa, the thermal expansion coefficient is 7.5 ⁇ 10 -6 /°C ⁇ 8.5 ⁇ 10 -6 /°C, which meets the requirements for the use of alumina precision ceramics in semiconductor equipment.
  • Raw material high-purity alumina powder: alumina purity 99.99% or more, particle size D50: 0.4 ⁇ m, BET: 13m 2 /g.
  • alumina ceramic body Place the formed alumina ceramic body in the atmospheric pressure debinding and sintering furnace.
  • the furnace temperature is increased to 600°C at a heating rate of 0.5°C/min, and kept at this temperature for 6 hours to complete the debinding operation of the alumina ceramics, and completely remove Organic grease; alumina ceramics continue to heat up to 1400°C at a heating rate of 2.5°C/min, and keep it at 1400°C for 6 hours.
  • the alumina can be discharged from the sintering furnace when the temperature is naturally lowered to below 200°C, and the firing is completed to obtain an alumina ceramic sintered body.
  • the alumina ceramic sintered body is polished by a neutral polishing liquid after CNC grinding and finishing, and its surface roughness Ra ⁇ 0.1 ⁇ m.
  • Raw material high-purity alumina powder: alumina purity 99.99% or more, particle size D50: 0.3 ⁇ m, BET: 15m 2 /g.
  • alumina ceramic body Place the formed alumina ceramic body in the atmospheric pressure debinding and sintering furnace.
  • the furnace temperature is increased to 600°C at a heating rate of 0.5°C/min, and kept at this temperature for 6 hours to complete the debinding operation of the alumina ceramics, and completely remove Organic grease; alumina ceramics continue to heat up to 1350°C at a heating rate of 2.0°C/min, and keep it at 1350°C for 8 hours.
  • the alumina can be discharged from the sintering furnace when the temperature is naturally lowered to below 200°C, and the firing is completed to obtain an alumina ceramic sintered body.
  • the alumina ceramic sintered body is polished by a neutral polishing liquid after CNC grinding and finishing, and its surface roughness Ra ⁇ 0.1 ⁇ m.
  • Raw material high-purity alumina powder: alumina purity 99.99% or more, particle size D50: 0.3 ⁇ m, BET: 18m 2 /g.
  • alumina ceramic body Place the formed alumina ceramic body in an atmospheric degreasing and sintering furnace.
  • the temperature of the furnace is increased to 600°C at a heating rate of 0.5°C/min, and the alumina ceramics degreasing operation is completed by keeping it at this temperature for 6 hours. Removal of organic grease; the alumina ceramic continues to be heated to 1300°C at a heating rate of 2.0°C/min, and kept at 1300°C for 7 hours.
  • the alumina can be discharged from the sintering furnace when the temperature is naturally lowered to below 200°C, and the firing is completed to obtain an alumina ceramic sintered body.
  • Raw material high-purity alumina powder: alumina purity 99.99% or more, particle size D50: 2.5 ⁇ m, BET: 8m 2 /g.
  • alumina ceramic body Place the formed alumina ceramic body in an atmospheric degreasing and sintering furnace.
  • the temperature of the furnace is increased to 600°C at a heating rate of 0.5°C/min, and the alumina ceramics degreasing operation is completed by keeping it at this temperature for 6 hours.
  • Remove organic grease; alumina ceramics continue to heat up to 1400°C at a heating rate of 2.5°C/min, and keep it at 1400°C for 6 hours.
  • the alumina can be discharged after the sintering furnace is naturally cooled to below 200°C, and the firing is completed.
  • Raw material high-purity alumina powder: alumina purity 99.99% or more, particle size D50: 2.5 ⁇ m, BET: 8m 2 /g.
  • the alumina slurry is dried in a spray dryer at a drying temperature of 280°C and an atomizing plate rotating speed of 10,000 rpm to prepare spherical alumina powder.
  • Raw material alumina purity 95%, particle size D50: 0.3 ⁇ m, BET: 15 m 2 /g.
  • the slurry is dried in a spray dryer at a drying temperature of 280° C. and an atomizing plate rotating speed of 10000 rpm to prepare spherical alumina ultrafine powder.
  • the alumina ceramic body is placed in the atmospheric pressure debinding and sintering furnace.
  • the furnace temperature is increased to 600°C at a heating rate of 0.5°C/min, and the alumina ceramic body is debinding at this temperature for 6 hours to completely remove organic Grease;
  • Alumina ceramics continue to heat up to 1350°C at a heating rate of 2.0°C/min, and keep it at 1350°C for 8 hours.
  • the alumina can be discharged after the sintering furnace is naturally cooled to below 200°C, and the firing is completed.
  • test standards for each performance test item are as follows:
  • Examples 1 to 3 of the present invention use high-purity alumina powder as the raw material, after ball milling, spray drying, 3D printing, and low-temperature and atmospheric sintering, which can produce high density, fine grains, and high strength.
  • Precision alumina ceramics with high toughness, high hardness, high temperature resistance, low thermal expansion coefficient, and insulation.
  • the density of comparative example 1 alumina ceramics is too small, not completely sintered and compact, and does not meet the requirements of the use of alumina precision ceramics for semiconductor equipment, indicating that the performance indicators of alumina raw material powder have a significant effect on reducing the sintering temperature.
  • the particle size of the alumina raw material powder When the size of the slurry is too large or the size of the slurry after grinding is too large, the powder sintering activity will be reduced, and compact sintering cannot be completed at a lower temperature, resulting in low density of the sintered ceramics, and other performance indicators of the corresponding ceramics also decreasing.
  • Comparative Example 2 and Comparative Example 1 using the same alumina powder and treatment process, the density of alumina ceramics is increased when the sintering temperature is changed to 1700°C. However, the process requires high sintering temperature, energy consumption and equipment costs.
  • the performance parameters of the fired alumina ceramics still have a gap with the performance of the embodiment of the present invention, especially the compressive strength and flexural strength are obviously inferior to the embodiment of the present invention.
  • Comparative Example 3 and Example 2 used alumina raw material powder with the same particle size, but the purity of the alumina was 95%, and the other treatment processes were the same.
  • the alumina raw material powder Purity has a great influence on the preparation of alumina ceramics for semiconductor equipment.
  • the impurities contained in alumina are immiscible with alumina during the high temperature liquid phase reaction process, which prevents the fusion of alumina crystals, increases the energy required for the reaction, and causes The density of sintered products is not high, and the corresponding mechanical properties such as hardness, compressive strength and flexural strength are poor.

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Abstract

L'invention concerne une céramique d'alumine et un procédé de préparation s'y rapportant. Le procédé comprend les étapes suivantes : la préparation de poudre d'alumine sous forme d'une bouillie pour obtenir une bouillie d'alumine ayant une taille des particules D90 inférieure ou égale à 0,8 µm ; le séchage de la bouillie d'alumine pour obtenir de la fine poudre d'alumine, la teneur en alumine de la poudre d'alumine étant ≥ 99 % en poids ; le chauffage et la fusion d'une résine photosensible, d'un premier agent dispersant et d'un lubrifiant, puis l'addition de la fine poudre d'alumine et d'un absorbeur d'ultraviolets et la réalisation d'un traitement de mise sous vide après mélange homogène de ceux-ci pour obtenir une bouillie d'alumine photodurcissante ; la réalisation d'une impression 3D et d'un formage sur la bouillie d'alumine photodurcissante pour obtenir un corps cru en céramique d'alumine ; et la réalisation d'un dégraissage et d'un frittage atmosphériques sur le corps cru en céramique d'alumine pour obtenir une céramique d'alumine ; les conditions pour le dégraissage et le frittage atmosphériques étant les suivantes : l'augmentation de la température jusqu'à 550 °C à 650 °C à une vitesse de (0,2 à 1) °C/min, le maintien de la température pendant 6 h à 10 h, puis l'augmentation de la température jusqu'à 1200 °C à 1400 °C à une vitesse de (1 à 5) °C/min et le maintien de la température pendant 5 h à 8 h. La céramique d'alumine préparée à l'aide du procédé a une densité élevée et de bonnes propriétés mécaniques et peut satisfaire aux exigences d'un dispositif à semi-conducteur pour un matériau céramique.
PCT/CN2020/128669 2020-06-09 2020-11-13 Céramique d'alumine et procédé de préparation s'y rapportant WO2021248813A1 (fr)

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