WO2021131407A1 - 窒化アルミニウム粒子 - Google Patents

窒化アルミニウム粒子 Download PDF

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WO2021131407A1
WO2021131407A1 PCT/JP2020/042864 JP2020042864W WO2021131407A1 WO 2021131407 A1 WO2021131407 A1 WO 2021131407A1 JP 2020042864 W JP2020042864 W JP 2020042864W WO 2021131407 A1 WO2021131407 A1 WO 2021131407A1
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aluminum nitride
particles
nitride particles
plate
ppm
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French (fr)
Japanese (ja)
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博治 小林
達也 菱木
竹内　勝之
義政 小林
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NGK Insulators Ltd
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NGK Insulators Ltd
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Priority to US17/804,319 priority patent/US20220281745A1/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the present specification discloses techniques relating to aluminum nitride particles.
  • the present specification discloses techniques relating to aluminum nitride particles used as raw materials for aluminum nitride plates.
  • Patent Document 1 discloses a method for producing a group III nitride semiconductor, specifically, an aluminum nitride plate (single crystal plate). Since the aluminum nitride plate has a close lattice constant, it is used as a growth substrate for a group III nitride semiconductor such as gallium nitride.
  • the raw material space in which the raw material is arranged is heated to a high temperature to sublimate the raw material, and the base substrate space in which the base substrate is arranged is maintained at a lower temperature than the raw material space. To do.
  • Patent Document 1 by keeping the space of the base substrate lower than the space of the raw material, it is possible to suppress the re-sublimation of the aluminum nitride crystal-grown on the base substrate and improve the growth rate of the aluminum nitride plate.
  • Aluminum nitride plate may be required to have high light transmittance (for example, total transmittance).
  • high light transmittance for example, total transmittance
  • the manufacturing process of a semiconductor device when a step of irradiating light from the back surface of the aluminum nitride plate toward a functional layer (semiconductor layer) formed on the surface of the aluminum nitride plate is required, high light transmission is required. ..
  • the aluminum nitride plate is used as the light emitting portion of the light emitting element, high light transmission is required.
  • the growth rate of the aluminum nitride plate can be improved.
  • impurities such as carbon may be mixed in the aluminum nitride plate.
  • Impurities such as carbon are removed by heating (firing) the aluminum nitride plate in the manufacturing process (heat treatment process) of the semiconductor device.
  • heat treatment process heat treatment process
  • pores are formed in the aluminum nitride plate. The pores scatter light and become a factor that lowers the light transmittance (total transmittance).
  • the present inventors have conducted research on raw materials (aluminum nitride particles) used in the production of aluminum nitride plates, and have obtained the finding that the generation of pores can be suppressed by using a specific raw material.
  • the present specification is based on this knowledge and discloses novel aluminum nitride particles used as a raw material for an aluminum nitride plate.
  • the aluminum nitride particles disclosed in the present specification may contain 100 ppm or less of carbon in the particles. By using such aluminum nitride particles, the amount of carbon contained in the aluminum nitride plate (or the intermediate in manufacturing the aluminum nitride plate) is reduced, and carbon is lost during heat treatment such as firing to nitride the aluminum nitride.
  • the aluminum nitride Reducing the amount of carbon contained in the plate is a useful technique for improving the light transmission of the aluminum nitride plate.
  • the aluminum nitride particles disclosed in the present specification are usefully used as a raw material for an aluminum nitride plate (single crystal aluminum nitride plate or polycrystalline aluminum nitride plate). Specifically, the aluminum nitride particles can be used as a raw material for an aluminum nitride plate that requires good light transmission.
  • a flat plate-shaped molded body (intermediate body) is produced by a sublimation method or aluminum nitride powder, and then the molded body is subjected to a normal pressure sintering method, a hot press method, or a hot static method.
  • the aluminum nitride particles disclosed in the present specification can be more preferably used as a raw material for producing an aluminum nitride plate by utilizing a sintering method.
  • the aluminum nitride particles may have a particle size (median diameter) of 0.1 ⁇ m or more and 10 ⁇ m or less.
  • the particle size of the aluminum nitride particles can be measured with a particle size distribution measuring device.
  • the particle size of the aluminum nitride particles By setting the particle size of the aluminum nitride particles to 0.1 ⁇ m or more, the weight of the aluminum nitride particles themselves can be sufficiently secured, and the handleability of the aluminum nitride particles when manufacturing the aluminum nitride plate can be improved. That is, when the aluminum nitride plate is manufactured, it is possible to prevent the aluminum nitride particles from scattering (fluttering) in the air.
  • the density of the molded product can be sufficiently increased.
  • the particle size of the aluminum nitride particles may be 0.5 ⁇ m or more, 1 ⁇ m or more, 2 ⁇ m or more, 3 ⁇ m or more, or 4 ⁇ m or more. However, it may be 6 ⁇ m or more, or 8 ⁇ m or more.
  • the aluminum nitride particles can be sublimated (vaporized) in a relatively short time when the aluminum nitride plate is manufactured by the above sublimation method. Further, when the molded body (intermediate body) is sintered to produce an aluminum nitride plate, it is possible to suppress the formation of large pores (voids between aluminum nitride particles) in the molded body. As a result, it is possible to prevent pores from remaining in the aluminum nitride plate after the molded product is sintered.
  • the particle size of the aluminum nitride particles may be 8 ⁇ m or less, 6 ⁇ m or less, 5 ⁇ m or less, 4 ⁇ m or less, or 2 ⁇ m or less.
  • the aluminum nitride particles may have a distorted outer shape. That is, the aluminum nitride particles may not be spherical (for example, have a sphericity of 0.8 or less), but may have a crushed shape in which the surface of the sphere is crushed. Typically, as the sphericity of the aluminum nitride particles decreases (as the outer shape becomes distorted), the specific surface area of the aluminum nitride particles increases.
  • the heat receiving area of the aluminum nitride particles increases as the sphericity of the aluminum nitride particles decreases, and the aluminum nitride particles are sublimated (vaporized) in a relatively short time. Can be made to.
  • the contact area between the aluminum nitride particles increases as the sphericity of the aluminum nitride particles decreases, which is required for sintering. You can save time.
  • a method for reducing the sphericity of the aluminum nitride particles there is a method of pulverizing the aluminum nitride particles using a dry jet mill or the like.
  • the aluminum nitride particles may be in the form of non-aggregated particles, that is, in the form of primary particles.
  • the heat receiving area of the aluminum nitride particles can be increased, and the contact area between the aluminum nitride particles can be increased.
  • the agglomeration of the aluminum nitride particles (secondary particles) can be separated into the form of the primary particles.
  • the shape of the aluminum nitride particles is preferably an appropriately distorted shape. Specifically, when the aluminum nitride particles are viewed in a plane, the length of the outer edge with respect to the particle size appearing on the plane is preferably 3.5 times or more and 7 times or less.
  • the "particle size” that appears on the plane is the "particle size” that appears on the observation screen when the aluminum nitride particles are observed by SEM or the like, and the particles that appear on the observation screen are assumed to be circles.
  • Means diameter That is, it is a value obtained by dividing the area of the aluminum nitride particles appearing on the observation screen by the circumference ratio. Therefore, the "particle size” that appears on the plane when the aluminum nitride particles are viewed in a plane and the "particle size” (actual particle size) measured by the above-mentioned particle size distribution measuring device may be different.
  • the surface (outer surface) of the aluminum nitride particles may be observed, or the cross section (cut surface) of the aluminum nitride particles may be observed.
  • the outer edge ratio the length of the outer edge (hereinafter referred to as the outer edge ratio) with respect to the particle size appearing on the plane is 3.5 times or more, the contact area between the aluminum nitride particles is sufficiently secured, and the sintered aluminum nitride plate can be used. It is possible to suppress the remaining pores. Further, when the outer edge ratio is 7 times or less, the inter-particle distance (distance between the centers of the aluminum nitride particles) is suppressed from becoming too large, and the occurrence of a large gap between the aluminum nitride particles is suppressed.
  • the outer edge ratio may be 3.6 times or more, 3.8 times or more, 4 times or more, or 5 times or more. Further, the outer edge ratio may be 4.5 times or less, 4.2 times or less, 4 times or less, 3.8 times or less, or 3. It may be 6 times or less.
  • the aluminum nitride particles may be single crystal or polycrystalline particles, and are more preferably single crystal particles from the viewpoint of improving the translucency of the aluminum nitride plate. Further, in order to reduce the carbon content of the aluminum nitride particles in the aluminum nitride plate (including the intermediate molded product), the carbon content contained in the particles is preferably 100 ppm or less. As a result, it is possible to prevent carbon from disappearing during the manufacturing process and the formation of pores in the aluminum nitride plate. Further, the carbon content contained in the aluminum nitride plate can be reduced even when a step of eliminating carbon (high temperature heat treatment step) is not performed in the manufacturing process.
  • the aluminum nitride plate has a large amount of carbon or pores, the light transmission of the aluminum nitride plate is impaired. Specifically, carbon or pores serve as a scattering source for light that passes (transmits) through the aluminum nitride plate.
  • the carbon content of the aluminum nitride plate or the amount of pores in the aluminum nitride plate can be reduced.
  • the carbon content contained in the particles may be 90 ppm or less, 70 ppm or less, 50 ppm or less, 20 ppm or less, 15 ppm or less, and 10 ppm or less. May be good.
  • the carbon content of the aluminum nitride particles can be measured using an ICP (inductively coupled plasma) emission spectrometer, an X-ray photoelectron spectroscopy measuring device, or the like.
  • the aluminum nitride particles When aluminum nitride particles are used as a raw material for producing an aluminum nitride plate by sintering a molded body (intermediate body), the aluminum nitride particles may contain an appropriate amount of oxygen. Specifically, the aluminum nitride particles may have an oxygen content (oxygen concentration of the entire particles) of 500 ppm or more and 8000 ppm or less. By setting the oxygen content in the particles to 500 ppm or more, a liquid phase is likely to occur during preliminary firing (primary firing before main firing), voids between particles are reduced, and a dense aluminum nitride plate is used. Can be formed. That is, the pores in the aluminum nitride plate can be reduced.
  • oxygen content oxygen concentration of the entire particles
  • the oxygen content contained in the particles may be 1000 ppm or more, 3000 ppm or more, 5000 ppm or more, 7000 ppm or more, or 7800 ppm or more. Further, the oxygen content contained in the particles may be 7800 ppm or less, 7000 ppm or less, 5000 ppm or less, 4000 ppm or less, or 3000 ppm or less. However, it may be 1000 ppm or less.
  • the oxygen content contained in the particles can be measured using an oxygen analyzer.
  • the oxygen content of the aluminum nitride particles may differ between the surface layer of the particles and the inside of the particles (the portion covered by the surface layer). Specifically, the oxygen content of the particle surface layer may be higher than the oxygen content inside the particles.
  • the aluminum nitride particles are provided with a first region having a high oxygen content on the particle surface layer, and a second region having a lower oxygen content than the first region is provided inside the first region (on the particle center side). It may have been done.
  • the first region may cover the second region.
  • the first region may be aluminum oxide (Al 2 O 3) obtained by oxidizing aluminum nitride.
  • the second region may be a solid solution (AlN—O 2 solid solution) in which oxygen is solid-dissolved in aluminum nitride.
  • AlN—O 2 solid solution a solid solution in which oxygen is solid-dissolved in aluminum nitride.
  • oxygen content contained in the particles corresponds to the oxygen content of the total of the first region and the second region (entire particles).
  • the oxygen content of the second region (inside the particles) may be 500 ppm or less.
  • the oxygen content of the second region may be 400 ppm or less, 300 ppm or less, 200 ppm or less, or 100 ppm or less.
  • the oxygen content contained in the particles can be measured using an oxygen analyzer.
  • the oxygen content of the particle surface layer is detected at a low temperature (less than 1900 ° C), and the oxygen content inside the particles is measured at a high temperature (1900 ° C). The above) can be detected.
  • the oxygen content from the particle surface to the center to a depth of 5 nm is defined as the oxygen content of the particle surface layer (first region).
  • the oxygen content in the deeper part (center side) than the depth of 5 nm may be regarded as the oxygen content inside the particles.
  • the aluminum nitride particles disclosed in the present specification can be obtained by heat-treating conventional aluminum nitride particles in the presence of aluminum oxide. Specifically, the aluminum nitride particles and aluminum oxide are calcined in a nitrogen atmosphere at 1700 to 2300 ° C. for 10 to 15 hours. As a result, the carbon contained in the aluminum nitride particles (conventional aluminum nitride particles) reacts with the oxygen constituting the aluminum oxide to remove the carbon contained in the aluminum nitride particles, which is disclosed herein. Aluminum nitride particles having a low carbon content (100 ppm or less) can be obtained. Typically, an oxide film (aluminum oxide) is formed on the surface of the aluminum nitride particles.
  • an oxide film aluminum oxide
  • the aluminum oxide that is heat-treated together with the aluminum nitride particles may be an oxide film (aluminum oxide) formed on the surface of the aluminum nitride particles.
  • oxide film aluminum oxide
  • the carbon content contained in the aluminum nitride particles is relatively low (200 ppm to 1000 ppm)
  • the aluminum nitride particles are formed into aluminum nitride particles by firing the aluminum nitride particles in a nitrogen atmosphere at 1700 to 2000 ° C. The contained carbon can be removed.
  • the carbon content contained in the aluminum nitride particles is relatively high (more than 1000 ppm)
  • a mixture of the aluminum nitride particles and the aluminum oxide particles may be fired under the above conditions.
  • the amount of the aluminum oxide particles added is adjusted according to the carbon content contained in the aluminum nitride particles so that the aluminum oxide particles do not remain after firing (after carbon removal). Is adjusted as appropriate. Further, the above-mentioned firing temperature and firing time are appropriately adjusted according to the state of the aluminum nitride particles before firing (carbon content, particle size and shape) and the state of the target aluminum nitride particles.
  • aluminum nitride so that when an aluminum nitride plate is produced using aluminum nitride particles, an aluminum nitride plate having a light transmittance (total transmittance) of 68% can be obtained. Adjust the state of the particles.
  • the conventional aluminum nitride particles are produced by reducing the aluminum oxide particles in a nitrogen atmosphere. Carbon is used as the reducing agent at that time. That is, the conventional aluminum nitride particles are produced by utilizing the reaction "Al 2 O 3 + 3C + N 2 ⁇ 2AlN + 3CO". Therefore, carbon used as a reducing agent may remain in the aluminum nitride particles.
  • the aluminum nitride particles disclosed in the present specification are evaluated as those obtained by firing aluminum nitride particles obtained by a conventional production method together with aluminum oxide to remove residual carbon used in the process of producing the aluminum nitride particles. Can be done.
  • An example of a method for manufacturing an aluminum nitride plate using the aluminum nitride particles disclosed in the present specification as a raw material will be described.
  • a flat plate-shaped molded product is produced using a raw material containing aluminum nitride particles, and the molded product is fired to produce a primary sintered body (intermediate body), and further, the primary sintered body is 2
  • main firing A method of manufacturing an aluminum nitride plate by next firing (main firing) will be described.
  • a pre-baked molded product of a predetermined size is molded using aluminum nitride particles.
  • the pre-baked molded product is formed by, for example, applying and drying a slurry containing aluminum nitride particles on the film, laminating the molded product peeled off from the film so as to have a predetermined thickness, and performing a hydrostatic pressure press.
  • the molding aid added when molding the pre-firing molded product is degreased, and the pre-firing molded product is fired at a predetermined temperature while being pressurized to sinter and grow particles of aluminum nitride, resulting in high-density nitride.
  • An aluminum primary sintered body is formed.
  • the voids between the aluminum nitride particles disappear.
  • the aluminum nitride primary sintered body is secondarily fired in a non-pressurized state to promote the sintering of the aluminum nitride particles and to bake. The aid is removed to give an aluminum nitride plate.
  • the secondary firing promotes sintering and removes carbon.
  • the carbon concentration was 230 ppm and the oxygen concentration was 7800 ppm.
  • the outer edge ratio was 3.1 to 3.5. Details of the method for measuring the carbon content, oxygen content and outer edge ratio will be described later.
  • the aluminum nitride particles after firing were subjected to a dry jet mill (Nanojetmizer MJ-50, manufactured by Aisin Technologies Co., Ltd.) with an air volume of 1.0 m 3 / min. Crushed with.
  • a dry jet mill Nemizer MJ-50, manufactured by Aisin Technologies Co., Ltd.
  • the air volume used was changed to change the particle size.
  • the carbon content, oxygen content, outer edge ratio and particle size of the crushed samples 1 to 13 and the uncalcined samples 14 and 15 were measured.
  • the carbon content was measured by the pressurized sulfuric acid decomposition method described in JIS R1649 using an ICP (inductively coupled plasma) emission spectrometer (PS3520UV-DD, manufactured by Hitachi High-Tech Science Co., Ltd.).
  • the oxygen content was measured by the inert gas melting-infrared absorption method described in JIS R1675 using an oxygen analyzer (EMGA-6500, manufactured by HORIBA, Ltd.).
  • the oxygen content detected below 1900 ° C is defined as the oxygen content of the particle surface layer, and the oxygen detected above 1900 ° C.
  • the oxygen content inside the particle was defined as the oxygen content inside the particle, and the total oxygen content between the surface layer of the particle and the inside of the particle was defined as the oxygen content of the entire particle (inside the particle).
  • the obtained sample was photographed using SEM (JSM-6390 manufactured by JEOL Ltd.) at a magnification of 1000 to 2000, and 10 particles were randomly selected from the photographed images and selected.
  • the particle size and the length of the outer edge of the particles were measured, and the outer edge length was divided by the particle size (“outer edge length” / “particle size on the image”) to calculate.
  • the actual particle size (median diameter) of the sample was measured using a laser diffraction type particle size distribution measuring device (LA-920, manufactured by HORIBA, Ltd.). The measurement results of each sample are shown in FIG.
  • An aluminum nitride plate was produced using the aluminum nitride particles of Samples 1 to 15. First, a method for synthesizing an auxiliary agent (Ca—Al—O-based firing auxiliary agent) used when sintering an aluminum nitride plate will be described.
  • the auxiliary agent is mixed with the aluminum nitride particles and fired together with the aluminum nitride particles.
  • the crucible filled with the mixture was placed in a heating furnace, the temperature was raised to 1250 ° C. at a heating rate of 200 ° C./hr in the air, and the temperature was maintained at 1250 ° C. for 3 hours. After the heating was completed, the mixture was naturally cooled and the mixture (auxiliary agent) was taken out from the crucible.
  • the amount of the dispersion medium added was adjusted so that the slurry viscosity was 20000 cP.
  • the obtained raw material slurry was molded on a PET film by the doctor blade method.
  • the thickness of the slurry was adjusted so that the thickness after drying was 30 ⁇ m.
  • a sheet-shaped tape molded product was obtained.
  • the obtained tape molded product was cut into a circle having a diameter of 20 mm, and then 120 circular tape molded products were laminated to obtain a pre-baked molded product.
  • the obtained pre-baked molded product was placed on an aluminum plate having a thickness of 10 mm, and then placed in a vacuum package to evacuate the inside. Then, the vacuum package was hydrostatically pressed at 100 kgf / cm 2 in warm water at 85 ° C. to obtain a disk-shaped pre-calcined molded product (laminated product for firing).
  • the pre-baked molded product was placed in a degreasing furnace and degreased at 600 ° C. for 10 hours. Then, it was fired at 1900 ° C. for 10 hours under the condition of a surface pressure of 200 kgf / cm 2 , and then cooled to room temperature to obtain an aluminum nitride primary sintered body.
  • the pressurizing direction at the time of hot pressing was the laminating direction of the molded product before firing (the direction substantially orthogonal to the surface of the tape molded product). The pressurization was maintained until the temperature dropped to room temperature.
  • the aluminum nitride particles constituting the pre-calcined molded product grow into grains, and the pores in the molded product disappear, so that the aluminum nitride primary sintered body having a high density (relative density) can be obtained. Then, the surface of the aluminum nitride primary sintered body was ground to obtain a diameter of 20 mm and a thickness of 1.5 mm.
  • the aluminum nitride plate is cut into a size of 10 mm ⁇ 10 mm, and the four aluminum nitride plates are placed at equal intervals on the outer peripheral portion of the alumina surface plate ( ⁇ 68 mm) (the angle formed by the aluminum nitride sintered body adjacent to the center of the surface plate). Polished with a copper lapping machine on which a slurry containing diamond abrasive grains having a particle size of 9 ⁇ m and 3 ⁇ m was dropped, and further polished on a buffing machine on which a slurry containing colloidal silica was dropped for 300 minutes. did.
  • the polished 10 mm ⁇ 10 mm ⁇ 0.4 mm thick sample was washed in the order of ion-exchanged water, acetone, and ethanol for 3 minutes each, and then the entire line at a wavelength of 450 nm was used using a spectrophotometer (Perkin Elmer, Lambda900). The transmittance was measured.
  • the cross section of the central portion of the aluminum nitride plate in the thickness direction was observed using an SEM (manufactured by JEOL Ltd., JSM-6390) at a magnification of 3000, and the number of pores in the visual field was counted. The number of pores was randomly observed in 50 or more visual fields, and the number of pores around 1 mm 2 was calculated.
  • the carbon content (C concentration) of the spherical aluminum nitride particles was 230 ppm.
  • the samples (Samples 1 to 13) in which the spherical aluminum nitride particles were calcined in a nitrided atmosphere had a carbon content (C concentration) of 100 ppm or less in the aluminum nitride particles. This result indicates that the residual carbon contained in the commercially available aluminum nitride particles (spherical aluminum nitride particles) has been removed.
  • the aluminum nitride plates (samples 1 to 13) prepared using aluminum nitride particles having a carbon content of 100 ppm or less are compared with the aluminum nitride plates (samples 14 and 15) prepared using spherical aluminum nitride particles. It was confirmed that the number of pores in the plate was small and the total transmittance was high. Specifically, it was confirmed that the aluminum nitride plates produced using Samples 1 to 13 all had a total transmittance of 68% or more and had good light transmittance. It was confirmed that the total transmittance increased as the carbon content in the aluminum nitride particles decreased (Samples 1 to 3, Samples 4 and 5). It was also confirmed that the number of pores in the aluminum nitride plate decreased as the carbon content in the aluminum nitride particles decreased.
  • the total transmittance of the aluminum nitride plate tends to increase as the number of pores in the aluminum nitride plate decreases. That is, it was confirmed that by reducing the number of pores in the aluminum nitride plate, scattering of light (450 nm ultraviolet light) in the aluminum nitride plate can be suppressed and the total transmittance of the aluminum nitride plate can be increased.
  • samples 1 to 13 showed good total transmittance (68% or more), but the sample (sample 11) having an oxygen content (O concentration of the whole sample) of less than 500 ppm and the oxygen content of more than 8000 ppm.
  • the sample (Sample 12) has a larger number of pores in the aluminum nitride plate and a slightly lower total transmittance than the oxygen content of 500 ppm or more and 8000 ppm or less (to be exact, 1000 ppm or more and 7800 ppm or less). The results were (Samples 3, 5, 6, 11 and 12).
  • the oxygen content in the aluminum nitride particles to an appropriate range (500 ppm or more and 8000 ppm or less)
  • the liquid phase generated in the manufacturing process (primary firing) of the aluminum nitride plate becomes an appropriate range, and the nitriding is performed. It shows that pores are less likely to occur in the aluminum plate.
  • the oxygen content did not significantly affect the result of the total transmittance in the range of the oxygen content of 500 to 8000 ppm (Samples 2 and 4, Samples 3, 5 and 6). Further, it was confirmed that the O concentration inside the particles of each of the samples 1 to 13 was 500 ppm or less (more accurately, 400 ppm or less).
  • the aluminum nitride particles of Samples 1 to 10 have an outer edge ratio of 3,5 or more and 4 or less, and good total transmittance is obtained, but it is confirmed that the total transmittance tends to improve as the outer edge ratio increases. (Samples 5, 7 and 8). In addition, from the results of Samples 14 and 15, it was confirmed that the total transmittance tends to improve as the outer edge ratio increases.

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JP2017088459A (ja) * 2015-11-13 2017-05-25 株式会社トクヤマ 耐水性窒化アルミニウム粉末
JP2019137595A (ja) * 2018-02-14 2019-08-22 株式会社トクヤマ 金属含有窒化アルミニウム粉末の製造方法
JP2019147709A (ja) * 2018-02-27 2019-09-05 株式会社トクヤマ 窒化アルミニウム粉末の製造方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2025012551A (ja) * 2023-07-13 2025-01-24 株式会社Maruwa 窒化アルミニウム粉末及びその改質方法並びに高分子成形体
JP7626801B2 (ja) 2023-07-13 2025-02-04 株式会社Maruwa 窒化アルミニウム粉末及びその改質方法並びに高分子成形体

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