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WO2024195609A1 - Poudre de nitrure de silicium et son procédé de production, et corps fritté de nitrure de silicium et son procédé de production - Google Patents

Poudre de nitrure de silicium et son procédé de production, et corps fritté de nitrure de silicium et son procédé de production Download PDF

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WO2024195609A1
WO2024195609A1 PCT/JP2024/009344 JP2024009344W WO2024195609A1 WO 2024195609 A1 WO2024195609 A1 WO 2024195609A1 JP 2024009344 W JP2024009344 W JP 2024009344W WO 2024195609 A1 WO2024195609 A1 WO 2024195609A1
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Prior art keywords
silicon nitride
powder
containing component
content
chromium
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Japanese (ja)
Inventor
厚樹 五十嵐
一輝 鎌田
賢史 平田
竜之介 長與
聖治 小橋
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Denka Co Ltd
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Denka Co Ltd
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Priority to CN202480020343.6A priority Critical patent/CN120916972A/zh
Priority to JP2025508329A priority patent/JPWO2024195609A1/ja
Publication of WO2024195609A1 publication Critical patent/WO2024195609A1/fr
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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
    • C01B21/068—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 silicon
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C04B35/587—Fine ceramics

Definitions

  • This disclosure relates to silicon nitride powder and its manufacturing method, as well as silicon nitride sintered body and its manufacturing method.
  • Silicon nitride sintered compacts are a material with excellent strength, hardness, toughness, heat resistance, corrosion resistance, and thermal shock resistance, and are therefore used in various industrial parts such as die-casting machines and melting furnaces, as well as insulating substrates for automotive parts.
  • silicon nitride powder with a high alpha conversion rate is used as the raw material for silicon nitride sintered compacts.
  • Patent Document 1 attempts to produce silicon nitride powder with a high alpha conversion rate using a continuous fluidized bed reactor in order to improve productivity.
  • Patent Document 1 proposes using metallic silicon powder as the raw material, with a total metal impurity content of 1.3 wt% or less and an Fe content of 0.3 wt% or less.
  • the present disclosure provides a silicon nitride sintered body with sufficiently reduced quality variation and a method for producing the same. It provides silicon nitride powder with excellent sinterability and sufficiently reduced quality variation. It provides a method for producing silicon nitride powder that can efficiently produce silicon nitride powder with excellent sinterability and sufficiently reduced quality variation.
  • One aspect of the present disclosure provides the following silicon nitride powder:
  • the silicon nitride powder of [1] above has a high alpha conversion rate and therefore has excellent sinterability.
  • the nitriding reaction during production proceeds with high uniformity, and quality variation is sufficiently reduced. If this silicon nitride powder is used, for example, as a sintering raw material, a silicon nitride sintered body with sufficiently reduced quality variation can be obtained.
  • the use of silicon nitride powder is not limited to the production of silicon nitride sintered bodies.
  • the silicon nitride powder of [1] above may be the following [2] or [3].
  • the silicon nitride powder of [2] above has sufficiently excellent sinterability and can sufficiently suppress abnormal grain growth.
  • the silicon nitride powder of [3] above undergoes a more uniform nitriding reaction during production. This further reduces the variation in quality.
  • the original performance of silicon nitride can be fully maintained. Therefore, when used as a sintering raw material, it is possible to obtain a silicon nitride sintered body with a further reduced variation in quality and excellent performance.
  • One aspect of the present disclosure provides the following method for producing silicon nitride powder.
  • the raw material powder contains at least one selected from the group consisting of a chromium-containing component and a nickel-containing component, and satisfies one or both of the following: the chromium-containing component has a Cr-equivalent content of 100 to 1000 ⁇ g/g; and the nickel-containing component has a Ni-equivalent content of 50 to 1000 ⁇ g/g;
  • the method for producing silicon nitride powder described above in [4] uses a raw material powder containing a predetermined amount of at least one selected from the group consisting of a chromium-containing component and a nickel-containing component, which promotes the nitriding reaction.
  • silicon nitride powder with excellent sinterability and sufficiently reduced quality variation can be efficiently produced using a continuous furnace.
  • the manufacturing method of the above [4] may be the following [5] or [6].
  • the manufacturing method [5] above makes it possible to obtain silicon nitride powder that is excellent in sinterability and has sufficiently reduced quality variation.
  • the manufacturing method [6] above makes it possible to more efficiently manufacture silicon nitride powder having the above characteristics.
  • One aspect of the present disclosure provides the following silicon nitride sintered body:
  • the silicon nitride sintered body of [7] above contains a specified amount of at least one selected from the group consisting of a chromium-containing component and a nickel-containing component, so the particles that make up the silicon nitride sintered body are highly uniform. This makes it possible to sufficiently reduce the variation in quality.
  • the silicon nitride sintered body of [7] above has a Weibull coefficient of 9 or more, so the variation in bending strength is also sufficiently small.
  • the silicon nitride sintered body of [7] above may be the following [8].
  • One aspect of the present disclosure provides the following method for producing a silicon nitride sintered body.
  • a method for producing a silicon nitride sintered body comprising sintering a sintering raw material containing the silicon nitride powder described in any one of [1] to [3] above, or the silicon nitride powder obtained by the production method described in any one of [4] to [6] above, to obtain a silicon nitride sintered body.
  • the silicon nitride sintered body of [9] above has a sintering raw material containing the silicon nitride powder described above or silicon nitride powder obtained by the manufacturing method described above, so the particles constituting the silicon nitride sintered body can have high uniformity. This makes it possible to sufficiently reduce quality variation.
  • silicon nitride sintered body with sufficiently reduced quality variation and a method for producing the same. It is possible to provide a silicon nitride powder with excellent sinterability and sufficiently reduced quality variation. It is possible to provide a method for producing silicon nitride powder that can efficiently produce silicon nitride powder with excellent sinterability and sufficiently reduced quality variation.
  • the numerical ranges exemplified in the format of "a-b" are numerical ranges inclusive of a and b, with a lower limit being a and an upper limit being b.
  • the present disclosure also includes numerical ranges in which the upper or lower limit of each numerical range is replaced with the numerical value of any of the examples, and numerical ranges in which the upper or lower limit is replaced with the upper or lower limit of another numerical range.
  • the silicon nitride powder (Si 3 N 4 powder) according to one embodiment contains a silicon nitride component having an alpha conversion rate of 90.0% or more, and at least one selected from the group consisting of a chromium-containing component and a nickel-containing component.
  • the silicon nitride powder may contain only the silicon nitride component and the chromium-containing component or only the nickel-containing component, or may contain both the silicon nitride component and the chromium-containing component and the nickel-containing component.
  • the silicon nitride powder contains silicon nitride as a main component.
  • the content of the silicon nitride in the silicon nitride powder may be 90% by mass or more, 95% by mass or more, 98% by mass or more, or 99% by mass or more.
  • the content of the silicon nitride in the silicon nitride powder can be measured using a commercially available X-ray diffraction device.
  • the alpha-phase ratio of the silicon nitride component (phase ratio of alpha-Si 3 N 4 to the whole Si 3 N 4 ) is 90.0% or more. Since such silicon nitride powder has excellent sinterability, when used as a sintering raw material, a silicon nitride sintered body having excellent mechanical properties and sufficiently reduced quality variation can be obtained. From the viewpoint of improving the bending strength of the silicon nitride sintered body, the alpha-phase ratio of the silicon nitride component may be 91.0% or more, 92.0% or more, or 93.0% or more.
  • the alpha-phase ratio of the silicon nitride component may be 98.0% or less, 97.0% or less, or 96.5% or less.
  • An example of the alpha-phase ratio of the silicon nitride component is 90.0 to 98.0%.
  • the alpha-phase ratio of the silicon nitride component can be determined by the method described in the examples.
  • the chromium-containing component in the silicon nitride powder may be a chromium compound such as chromium oxide or chromium nitride, or may be elemental chromium (metallic chromium).
  • the nickel-containing component in the silicon nitride powder may be a nickel compound such as nickel oxide or nickel nitride, or may be elemental nickel (metallic nickel).
  • the chromium-containing component and nickel-containing component may be contained in the metallic silicon particles, may be intentionally added to the raw material powder before sintering, or may be mixed in during the manufacturing process.
  • the Cr content of the chromium-containing component in the silicon nitride powder may be 50 to 250 ⁇ g/g.
  • Such silicon nitride powder has a narrow composition distribution because of the sufficient nitridation. Therefore, it is possible to obtain a silicon nitride sintered body with sufficiently reduced quality variation.
  • the Cr content in the silicon nitride powder may be 240 ⁇ g/g or less, 200 ⁇ g/g or less, or 190 ⁇ g/g or less. This allows the original properties of silicon nitride to be more sufficiently maintained.
  • the Cr content in the silicon nitride powder may be 60 ⁇ g/g or more, 70 ⁇ g/g or more, or 80 ⁇ g/g or more.
  • Such silicon nitride powder has a further advanced nitridation, so it is possible to obtain a silicon nitride sintered body with further reduced quality variation.
  • Ni content of the nickel-containing component in the silicon nitride powder may be 5 to 60 ⁇ g/g.
  • Such silicon nitride powder has a narrow composition distribution because nitridation has progressed sufficiently. Therefore, a silicon nitride sintered body with sufficiently reduced quality variation can be obtained.
  • the Ni content in the silicon nitride powder may be 50 ⁇ g/g or less, 40 ⁇ g/g or less, or 30 ⁇ g/g or less. This allows the original properties of silicon nitride to be more fully maintained.
  • the Ni content in the silicon nitride powder may be 7 ⁇ g/g or more, 8 ⁇ g/g or more, or 10 ⁇ g/g or more.
  • Such silicon nitride powder has a further progressed nitridation, so a silicon nitride sintered body with further reduced quality variation can be obtained.
  • Silicon nitride powder containing both a chromium-containing component and a nickel-containing component does not need to satisfy the numerical ranges for both the Cr content and Ni content described above, but only needs to satisfy the numerical range for at least one of the Cr content and Ni content.
  • the sum of the Cr content and Ni content (Cr+Ni content) in the silicon nitride powder may be 35 ⁇ g/g or more, 40 ⁇ g/g or more, or 50 ⁇ g/g or more.
  • the Cr+Ni content may be 280 ⁇ g/g or less, 240 ⁇ g/g or less, or 200 ⁇ g/g or less.
  • One example of the range of the Cr+Ni content is 30 to 300 ⁇ g/g.
  • the Cr and Ni contents in silicon nitride powder can be quantified by ICP atomic emission spectrometry.
  • ICP atomic emission spectrometry For example, an ICPE-9000 (instrument name, manufactured by Shimadzu Corporation) can be used as a measuring device.
  • the silicon nitride powder of this embodiment contains a silicon nitride component with a high alpha conversion rate, and also contains a predetermined amount of at least one of a chromium-containing component and a nickel-containing component. Since nitridation has progressed sufficiently in such silicon nitride powder, the compositional variation is small. Therefore, when used as a sintering raw material, a silicon nitride sintered body with sufficiently reduced quality variation can be obtained.
  • the use of silicon nitride powder is not limited to the production of silicon nitride sintered bodies, and it may be mixed with other types of powders (e.g., ceramic powders such as boron nitride) to produce a composite, for example.
  • the silicon nitride powder may contain components other than silicon nitride, the chromium-containing component, and the nickel-containing component. Such components include calcium-containing components, halogens, iron-containing components, etc.
  • the calcium-containing component and halogens (fluorine) may be derived from the fluorite used in synthesizing silicon nitride.
  • the iron-containing component may be derived from metal silicon particles, the manufacturing process, etc.
  • Such silicon nitride powder and silicon nitride sintered body can be produced using relatively low-cost raw materials and manufacturing processes, thereby reducing manufacturing costs.
  • the average particle size of the silicon nitride powder may be 0.5 to 2.0 ⁇ m. Such silicon nitride powder has sufficiently excellent sinterability and can sufficiently suppress abnormal grain growth during sintering.
  • the upper limit of the average particle size of the silicon nitride powder may be 1.6 ⁇ m, 1.4 ⁇ m, 1.2 ⁇ m, or 1.0 ⁇ m. This can further suppress abnormal grain growth during sintering.
  • the lower limit of the average particle size of the silicon nitride powder may be 0.6 ⁇ m or 0.7 ⁇ m. This can further increase the sinterability.
  • the average particle size of each powder in this specification is determined based on the method described in JIS Z 8825:2013 "Particle size analysis - Laser diffraction and scattering method".
  • the particle size distribution (cumulative distribution) measured based on the above method, where the horizontal axis is the particle size [ ⁇ m] on a logarithmic scale and the vertical axis is the frequency [volume %]
  • the particle size when the cumulative value from the smallest particle size reaches 50% of the total is the average particle size (D50, median size).
  • the measuring device described in the examples can be used.
  • the average particle size of silicon nitride powder can be adjusted by changing the particle size of the raw material powder, the firing temperature and firing time when producing silicon nitride powder, and the conditions when crushing the calcined body.
  • the BET specific surface area of the silicon nitride powder may be 5 to 15 m 2 /g. Such silicon nitride powder has sufficiently excellent sinterability and can sufficiently suppress abnormal grain growth.
  • the upper limit of the BET specific surface area of the silicon nitride powder may be 14 m 2 /g or 13 m 2 /g. This can further increase the sinterability.
  • the lower limit of the BET specific surface area of the silicon nitride powder may be 6 m 2 /g or 7 m 2 /g. This can further suppress abnormal grain growth during sintering.
  • the BET specific surface area of each powder in this specification is a value measured by the BET single-point method using nitrogen gas in accordance with the method described in JIS Z 8830:2013 "Method for measuring specific surface area of powder (solid) by gas adsorption.”
  • the BET specific surface area of silicon nitride powder can be adjusted by changing the particle size of the raw material powder and the firing temperature and firing time when producing silicon nitride powder.
  • the method for producing silicon nitride powder includes a step of sintering a raw material powder containing metal silicon powder using a continuous furnace in an atmosphere containing nitrogen gas and hydrogen gas to obtain a calcined body containing silicon nitride components with an alpha conversion rate of 90.0% or more.
  • the silicon nitride powder described above may be produced by this production method. Therefore, the contents described in the embodiment of the silicon nitride powder also apply to this production method.
  • the metal silicon powder may be made by crushing metal silicon particles (or lumps). Examples of crushing devices include a hammer mill, a pin mill, a ball mill, a vibration mill, a bead mill, and a jet mill.
  • the average particle size (median size, D50) of the metal silicon powder may be 15 to 30 ⁇ m. From the viewpoint of smoothly progressing nitriding, the average particle size of the metal silicon powder may be 28 ⁇ m or less, 26 ⁇ m or less, or 24 ⁇ m or less. If the raw material is nitrided in a powdered state, excessive heat may be generated. From the viewpoint of suppressing such heat generation, the average particle size of the metal silicon powder may be 16 ⁇ m or more, or 18 ⁇ m or more. The average particle size of the metal silicon powder can be measured in the same manner as the average particle size of the silicon nitride powder.
  • the purity of the metal silicon powder may be 98% by mass or more, or 99% by mass or more.
  • the metal silicon powder may also contain impurities that are mixed in during pulverization using a pulverizer.
  • the metallic silicon powder may be used as the raw material powder as it is, or the raw material powder may be prepared by blending the metallic silicon powder with a powder containing at least one component selected from the group consisting of fluorite, metallic chromium, chromium compounds, metallic nickel, and nickel compounds. Examples of chromium compounds and nickel compounds include oxides and nitrides.
  • the raw material powder may also be prepared by blending the metallic silicon powder with an alloy powder (e.g., stainless steel) containing a chromium component and a nickel component.
  • the raw material powder contains a metallic silicon component as a main component, and at least one selected from the group consisting of a chromium-containing component and a nickel-containing component as a secondary component.
  • the raw material powder may contain a metallic silicon component and either a chromium-containing component or a nickel-containing component.
  • the raw material powder may contain a metallic silicon component and both a chromium-containing component and a nickel-containing component.
  • the content of the metallic silicon component in the raw material powder may be 95% by mass or more, 97% by mass or more, or 98% by mass or more.
  • the content of the metallic silicon component in the raw material powder can be measured using a commercially available X-ray fluorescence analyzer.
  • the Cr content of the chromium-containing component in the raw material powder may be 100 to 1000 ⁇ g/g. With such raw material powder, nitridation proceeds sufficiently smoothly. Therefore, silicon nitride powder with sufficiently reduced composition variation can be obtained in a short time. By using such silicon nitride powder as a sintering raw material, a silicon nitride sintered body with sufficiently reduced quality variation can be obtained.
  • the Cr content in the raw material powder may be 960 ⁇ g/g or less, 900 ⁇ g/g or less, or 850 ⁇ g/g or less. This allows the obtained silicon nitride powder to more fully maintain the original properties of silicon nitride.
  • the Cr content in the raw material powder may be 150 ⁇ g/g or more, or 190 ⁇ g/g or more. By using such raw material powder, nitridation can proceed more smoothly.
  • Ni content of the nickel-containing component in the raw powder may be 50 to 1000 ⁇ g/g.
  • nitridation proceeds sufficiently smoothly. Therefore, silicon nitride powder with sufficiently reduced composition variation can be obtained in a short time.
  • silicon nitride powder as a sintering raw material, a silicon nitride sintered body with sufficiently reduced quality variation can be obtained.
  • the Ni content in the raw powder may be 970 ⁇ g/g or less, 900 ⁇ g/g or less, 800 ⁇ g/g or less, 600 ⁇ g/g or less, or 500 ⁇ g/g or less.
  • the Ni content in the raw powder may be 60 ⁇ g/g or more, 80 ⁇ g/g or more, or 100 ⁇ g/g or more. By using such raw powder, nitridation can proceed more smoothly.
  • the raw powder containing both the chromium-containing component and the nickel-containing component does not need to satisfy the numerical ranges of both the Cr content and the Ni content described above, but only needs to satisfy the numerical range of at least one of the Cr content and the Ni content.
  • the total value of the Cr content and the Ni content in the raw powder may be 160 ⁇ g/g or more, 170 ⁇ g/g or more, or 180 ⁇ g/g or more.
  • the Cr+Ni content may be 1800 ⁇ g/g or less, 1600 ⁇ g/g or less, 1400 ⁇ g/g or less, or 1100 ⁇ g/g or less.
  • An example of the range of the Cr+Ni content is 150 to 2000 ⁇ g/g.
  • the Cr and Ni contents in the raw material powder can be quantified by ICP atomic emission spectrometry.
  • ICP atomic emission spectrometry For example, an ICPE-9000 (instrument name, manufactured by Shimadzu Corporation) can be used as a measuring device.
  • the raw material powder may contain fluorite to promote nitridation of the metal silicon.
  • the content of fluorite per 100 parts by mass of the metal silicon powder may be 0.2 to 3 parts by mass. From the viewpoint of sufficiently promoting the nitridation of the metal silicon, the content of fluorite per 100 parts by mass of the metal silicon powder may be 0.5 parts by mass or more, or 0.8 parts by mass or more. From the viewpoint of reducing the Ca and F contents in the obtained silicon nitride powder, the content of fluorite per 100 parts by mass of the metal silicon powder may be 2 parts by mass or less, or 1.5 parts by mass or less.
  • the raw material powder may contain components other than the metallic silicon component, the chromium-containing component, the nickel-containing component, and the fluorite.
  • Such components include an iron-containing component.
  • the iron-containing component may be derived from metallic silicon particles, the manufacturing process, etc.
  • Such raw material powders can be prepared at low cost, thereby reducing the manufacturing costs of silicon nitride powder and sintered silicon nitride bodies.
  • the raw material powder is sintered in a continuous furnace to obtain a calcined body containing silicon nitride components.
  • the continuous furnace may be, for example, a tunnel-type pusher furnace with a container transport system, a roller hearth kiln, or the like. With such a continuous furnace, the container containing the raw material powder can be continuously heated inside the furnace. Since the raw material powder can be sintered without being molded, the nitriding reaction proceeds efficiently. This makes it possible to obtain a calcined body containing silicon nitride components in a short time.
  • the silicon nitride component contained in such a calcined body has a high alpha conversion rate. The specific numerical value of the alpha conversion rate is as explained in the embodiment of the silicon nitride powder.
  • the container to be filled with the raw material powder can be made of a material that does not change in quality even at temperatures of about 1500°C in an inert gas atmosphere.
  • the container can be made of, for example, carbon, alumina, or boron nitride.
  • There are no particular restrictions on the structure of the container and it can be one that has a storage section for storing the raw material powder.
  • the container can be one that has a container body with a recess and a lid that covers the recess in the main body. Also, multiple containers can be stacked, with the upper container used as the lid for the lower container.
  • the maximum temperature when sintering the raw material powder contained in a container is 1300-1500°C.
  • the temperature is increased to this temperature at a rate of 10-150°C/hour.
  • the temperature may be increased from 30°C to 1100°C at a rate of 50-150°C/hour, and then increased from 1100°C to the maximum temperature at a rate of 10-40°C/hour. This allows the exothermic reaction caused by the nitriding of the raw material powder to be appropriately controlled.
  • the atmosphere during firing may contain nitrogen gas and hydrogen gas. From the viewpoint of promoting nitridation of metal silicon, the ratio of nitrogen gas in the firing atmosphere may be 95.1 vol% or more, or may be 96.0 vol% or more. From the viewpoint of reducing oxides such as SiO 2 contained in the raw material powder and promoting nitridation, the ratio of hydrogen gas in the firing atmosphere may be 2.0 vol% or more, 3.0 vol% or more, or 4.0 vol% or more. An example of the ratio of nitrogen gas in the firing atmosphere is 95.1 to 98.0 vol%. An example of the ratio of hydrogen gas in the firing atmosphere is 2.0 to 4.9 vol%.
  • the atmosphere during firing may contain gases other than nitrogen gas and hydrogen gas. Examples of such gases include argon gas.
  • the ratio (vol%) of each gas in this specification is a value in standard state (0 ° C, 1 atm).
  • the time for heating the raw material powder to 1100°C or higher in the continuous furnace may be 24 hours or less, 22 hours or less, or 20 hours or less. Even if the heating time at high temperatures is shortened in this way, nitridation proceeds smoothly because the raw material powder contains chromium-containing components and/or nickel-containing components. Therefore, silicon nitride powder with sufficiently high purity can be obtained.
  • the time for heating to 1100°C or higher may be 10 hours or more, or 12 hours or more.
  • the temperature After reaching the maximum temperature in the continuous furnace, the temperature may be held for several hours, or cooling may begin immediately. There is no particular limit to the cooling rate, and the temperature may be reduced at a rate of, for example, 10 to 200°C/hour. When the temperature reaches approximately 300°C or less, it may be cooled in the air. Until then, the temperature may be reduced in the above atmosphere.
  • the calcined body obtained by the above-mentioned firing contains silicon nitride (silicon nitride component) as the main component.
  • silicon nitride silicon nitride component
  • the composition and particle size of the silicon nitride powder are as described above.
  • the pulverization may be carried out using, for example, a coarse pulverizer, a wet attritor, a ball mill, a vibrating mill, etc.
  • the silicon nitride component contained as the main component in the calcined body has a high alpha conversion rate, so the calcined body can be pulverized smoothly.
  • the crushed calcined body may be mixed with hydrofluoric acid having a hydrogen fluoride concentration of 10 to 40 mass % to reduce impurities.
  • the crushed calcined body may be dispersed in hydrofluoric acid for treatment.
  • the hydrogen fluoride concentration in the hydrofluoric acid may be 15 to 30 mass %.
  • the temperature of the hydrofluoric acid in the treatment step is, for example, 40 to 80°C.
  • the time for which the silicon nitride powder is immersed in hydrofluoric acid is, for example, 1 to 10 hours.
  • the silicon nitride sintered body according to one embodiment can be obtained by using the silicon nitride powder described above.
  • the silicon nitride sintered body may be obtained by firing a molded body of silicon nitride powder.
  • the silicon nitride sintered body contains a silicon nitride component as a main component and at least one selected from the group consisting of a chromium-containing component and a nickel-containing component as a secondary component.
  • the content of the silicon nitride component in the silicon nitride sintered body may be 90 mass% or more, 93 mass% or more, 95 mass% or more, or 97 mass% or more.
  • the content of the silicon nitride component in the silicon nitride sintered body can be measured using a commercially available X-ray diffraction device.
  • the chromium-containing component in the silicon nitride sintered body may be a chromium compound such as chromium oxide or chromium nitride, or may be simple chromium (metallic chromium).
  • the nickel-containing component in the silicon nitride sintered body may be a nickel compound such as nickel oxide or nickel nitride, or may be simple nickel (metallic nickel).
  • the Cr content of the chromium-containing component in the silicon nitride sintered body may be 10 to 220 ⁇ g/g. Since such a silicon nitride sintered body uses silicon nitride powder in which nitridation has progressed sufficiently, the particles constituting the silicon nitride sintered body are highly uniform. In other words, the composition distribution is sufficiently narrow. Therefore, the quality variation can be sufficiently reduced.
  • the Cr content in the silicon nitride sintered body may be 180 ⁇ g/g or less, 170 ⁇ g/g or less, 160 ⁇ g/g or less, or 100 ⁇ g/g or less.
  • the Cr content in the silicon nitride powder may be 20 ⁇ g/g or more, 30 ⁇ g/g or more, or 40 ⁇ g/g or more. Since such a silicon nitride sintered body is obtained using silicon nitride powder in which nitridation has progressed further, the quality variation can be further reduced.
  • Ni content of the nickel-containing component in the silicon nitride sintered body may be 1 to 60 ⁇ g/g. Since such a silicon nitride sintered body is obtained using silicon nitride powder in which nitridation has progressed sufficiently, the particles constituting the silicon nitride sintered body are highly uniform. In other words, the composition distribution is sufficiently narrow. Therefore, the quality variation can be sufficiently reduced.
  • the Ni content in the silicon nitride sintered body may be 55 ⁇ g/g or less, 50 ⁇ g/g or less, or 45 ⁇ g/g or less. This allows the original properties of silicon nitride to be more sufficiently maintained.
  • the Ni content in the silicon nitride sintered body may be 5 ⁇ g/g or more, 10 ⁇ g/g or more, or 15 ⁇ g/g or more. Since such a silicon nitride sintered body is obtained using silicon nitride powder in which nitridation has progressed further, the quality variation can be further reduced.
  • Silicon nitride sintered bodies containing both a chromium-containing component and a nickel-containing component do not need to satisfy the above-mentioned numerical ranges for both the Cr content and the Ni content, but only need to satisfy the numerical range for at least one of the Cr content and the Ni content.
  • the total value of the Cr content and the Ni content in the silicon nitride sintered body may be 30 ⁇ g/g or more, 40 ⁇ g/g or more, 50 ⁇ g/g or more, or 60 ⁇ g/g or more.
  • the Cr+Ni content may be 280 ⁇ g/g or less, 260 ⁇ g/g or less, 240 ⁇ g/g or less, or 220 ⁇ g/g or less.
  • An example of the range of the Cr+Ni content is 20 to 300 ⁇ g/g.
  • the chromium-containing component in the silicon nitride sintered body may be a chromium compound such as chromium oxide or chromium nitride, or may be simple chromium (metallic chromium).
  • the nickel-containing component in the silicon nitride sintered body may be a nickel compound such as nickel oxide or nickel nitride, or may be simple nickel (metallic nickel).
  • the chromium-containing component and nickel-containing component may be derived from the silicon nitride powder or may be derived from the manufacturing process.
  • the Cr and Ni contents in sintered silicon nitride can be quantified by ICP atomic emission spectroscopy.
  • ICP atomic emission spectroscopy For example, an ICPE-9000 (instrument name, manufactured by Shimadzu Corporation) can be used as a measuring device.
  • the silicon nitride sintered body may contain components other than silicon nitride, the chromium-containing component, and the nickel-containing component.
  • Such components include components derived from sintering aids, iron-containing components, etc.
  • sintering aids include oxide-based ones such as Y 2 O 3 , MgO, and Al 2 O 3.
  • the content of the components derived from the sintering aids in the silicon nitride sintered body may be, for example, 3 to 10 mass %.
  • the Weibull coefficient (m) of the silicon nitride sintered body may be 9 or more, 10 or more, or 11 or more. This allows the variation in quality to be sufficiently reduced.
  • the Weibull coefficient (m) in this specification is a shape parameter in JIS R 1625:2010, and can be obtained by statistically processing the bending strength ( ⁇ ).
  • the single-mode, two-parameter Weibull distribution function (F( ⁇ )) is expressed by the following formula (1).
  • ⁇ is the bending strength measured in accordance with JIS R 1601:2008
  • ⁇ is the scale parameter.
  • the Weibull coefficient m can be obtained as the slope of a straight line in a Weibull plot obtained by a graph with the vertical axis being ln(ln(1/(1-F( ⁇ )))) and the horizontal axis being ln ⁇ .
  • F( ⁇ ) 1-exp[-( ⁇ / ⁇ ) m ]...(1)
  • the bending strength of the silicon nitride sintered body measured in accordance with JIS R 1601:2008 may be 920 MPa or more, 1000 MPa or more, or 1050 MPa or more.
  • the relative density of the silicon nitride sintered body may be 97% or more, or 98% or more, from the viewpoint of improving bending strength.
  • the bulk density of the silicon nitride sintered body may be 3.1 g/ cm3 or more, from the viewpoint of improving bending strength.
  • the relative density and bulk density of the silicon nitride sintered body in this specification are measured by the Archimedes method.
  • the method for producing a silicon nitride sintered body includes a sintering step of molding and firing a sintering raw material containing the above-mentioned silicon nitride powder as a main component.
  • the sintering raw material may contain an oxide-based sintering aid in addition to the silicon nitride powder.
  • the oxide-based sintering aid include Y 2 O 3 , MgO, and Al 2 O 3.
  • the content of the oxide-based sintering aid in the sintering raw material may be, for example, 3 to 10 mass %.
  • the above-mentioned sintering raw materials are pressed at a molding pressure of, for example, 3.0 to 200 MPa to obtain a molded body.
  • the molded body may be produced by uniaxial pressing or by CIP. It may also be fired while being molded by hot pressing.
  • the molded body may be fired in an inert gas atmosphere such as nitrogen gas or argon gas.
  • the pressure during firing may be 0.7 to 1 MPa.
  • the firing temperature may be 1700 to 2100°C or 1800 to 2000°C.
  • the firing time at the firing temperature may be 2 to 20 hours or 4 to 16 hours.
  • the heating rate to the firing temperature may be, for example, 1.0 to 10.0°C/hour. In this manner, a silicon nitride sintered body can be obtained.
  • the above-mentioned manufacturing method uses a sintering raw material containing silicon nitride powder in which nitridation has progressed sufficiently uniformly, so the uniformity of the particles that make up the silicon nitride sintered body can be increased. In other words, the distribution of the composition can be made sufficiently narrow.
  • Such silicon nitride sintered bodies have sufficiently reduced quality variation and are highly reliable.
  • Example 1 Preparation and Evaluation of Metallic Silicon Powder> A metal silicon chunk having a particle size of 10 to 50 mm was prepared. The metal silicon chunk was coarsely crushed using a crushing device (device name: jaw crusher, manufactured by Makino Corporation) and a crushing device (device name: roll crusher, manufactured by Makino Corporation), and then finely crushed using a crushing device (device name: vibration mill, manufactured by Chuo Kakoki Co., Ltd.) to obtain a metal silicon powder. The crushing time by the vibration mill was 300 minutes. The particle size distribution of the metal silicon powder was measured. The particle size distribution was measured by a laser diffraction and scattering method.
  • a crushing device device name: jaw crusher, manufactured by Makino Corporation
  • a crushing device device name: roll crusher, manufactured by Makino Corporation
  • the crushing time by the vibration mill was 300 minutes.
  • the particle size distribution of the metal silicon powder was measured. The particle size distribution was measured by a laser diffraction and scattering method.
  • the measurement was performed in accordance with the method described in JIS Z 8825:2013 "Particle size analysis - laser diffraction and scattering method".
  • the measurement of the particle size distribution was performed by weighing 60 mg of metal silicon powder into a 500 mL container. A 20% aqueous solution of sodium hexametaphosphate (2 mL) and water (200 g) were mixed therewith as a dispersant. The container was set in an ultrasonic disperser manufactured by Sharp Corporation so that the entire portion containing the dispersion liquid was immersed, and ultrasonic dispersion was performed for 1 minute. The above-mentioned particle size distribution measurement was performed using the sample after ultrasonic dispersion. LS13 320 (device name, manufactured by Beckman Coulter, Inc.) was used to measure the particle size distribution. The average particle size (D50, median diameter) of the metal silicon powder was as shown in Table 1.
  • the above-mentioned metal silicon powder was mixed with fluorite and nickel oxide powder (NiO) to prepare a raw material powder.
  • the amount of fluorite based on the metal silicon powder was 1 mass %, and the amount of nickel oxide powder was 200 mass ppm.
  • the Cr-equivalent content (Cr content) of the chromium-containing component and the Ni-equivalent content (Ni content) of the nickel-containing component in the raw material powder thus prepared were measured by ICP emission spectrometry.
  • the measurement device used was ICPE-9000 (device name, manufactured by Shimadzu Corporation). The measurement results were as shown in Table 1. Table 1 also shows the total value of the Cr content and the Ni content.
  • a plurality of graphite containers having recesses were prepared.
  • the recesses of each of the plurality of containers were filled with raw material powder.
  • Each container was filled with 1.4 kg of raw material powder.
  • the filling height H of the raw material powder in the recesses was 30 mm.
  • the containers filled with the raw material powder were introduced into a container-transporting continuous furnace, and the metal silicon component contained in the raw material powder was nitrided.
  • the temperature was raised from room temperature to 1100°C in an atmosphere containing nitrogen gas and hydrogen gas over 11 hours, and then from 1100°C to 1400°C over 18 hours.
  • the ratio of nitrogen gas in the atmosphere was 96% by volume, and the ratio of hydrogen gas was 4% by volume.
  • After raising the temperature to 1400°C it was cooled to 200°C in the above atmosphere to obtain a calcined body containing silicon nitride as the main component.
  • the raw material powder was heated to 1100°C or higher for 18 hours. The calcined body was then allowed to cool to room temperature in the air.
  • the calcined body was coarsely crushed using a coarse crushing device (device name: jaw crusher, manufactured by Makino Co., Ltd.) and a crushing device (device name: roll crusher, manufactured by Makino Co., Ltd.), and then wet-pulverized in a ball mill to obtain a pulverized product.
  • a coarse crushing device device name: jaw crusher, manufactured by Makino Co., Ltd.
  • a crushing device device name: roll crusher, manufactured by Makino Co., Ltd.
  • the crushing time was 10 hours (wet-pulverization time).
  • the above-mentioned pulverized material obtained by wet pulverization was immersed in hydrofluoric acid (hydrofluoric acid concentration: 30% by mass) at a temperature of 70°C for 2 hours for acid treatment. The pulverized material was then removed from the hydrofluoric acid, washed with water, and dried under a nitrogen atmosphere. In this way, silicon nitride powder was obtained.
  • the alpha-phase ratio of the silicon nitride component contained in the silicon nitride powder was measured by the following procedure. X-ray diffraction of the silicon nitride powder was performed with CuK ⁇ radiation using an X-ray diffractometer (manufactured by Rigaku Corporation, device name: Ultima IV). The alpha phase was represented by the diffraction line intensity I a102 of the (102) plane and the diffraction line intensity I a210 of the (210) plane. The beta phase was represented by the diffraction line intensity I b101 of the (101) plane and the diffraction line intensity I b210 of the (210) plane.
  • the average particle size (D50, median size) and BET specific surface area of the silicon nitride powder are shown in Table 1.
  • the average particle size of the silicon nitride powder was measured in the same manner as for the metal silicon powder.
  • the BET specific surface area of the silicon nitride powder was measured by the single-point BET method using nitrogen gas in accordance with JIS Z 8803:2013.
  • the Cr-equivalent content (Cr content) of chromium-containing components in the silicon nitride powder and the Ni-equivalent content (Ni content) of nickel-containing components were measured by ICP atomic emission spectrometry.
  • the measuring device used was an ICPE-9000 (device name, manufactured by Shimadzu Corporation). The measurement results are shown in Table 1. Table 1 also shows the total values of the Cr content and Ni content measured in this way.
  • the mixed powder obtained by drying was then molded in a mold at a pressure of 10 MPa, and then further molded by CIP at a pressure of 100 MPa.
  • the obtained molded body was set in a carbon crucible together with a packing powder consisting of a mixed powder of silicon nitride powder and BN powder, and sintered at a temperature of 1800 ° C for 4 hours in a nitrogen pressure atmosphere of 1 MPa to produce a silicon nitride sintered body.
  • Cr content Cr-equivalent content of chromium-containing components in the silicon nitride sintered body
  • Ni content Ni-equivalent content of nickel-containing components
  • Example 2 Metallic silicon powder was prepared in the same manner as in Example 1. Fluorite and chromium oxide powder (Cr 2 O 3 ) were blended and mixed with this metallic silicon powder. The blending amount of fluorite based on the metallic silicon powder was 1 mass %, and the blending amount of chromium oxide powder was 220 mass ppm. Aside from using the raw material powder prepared in this manner, silicon nitride powder and silicon nitride sintered body were prepared in the same manner as in Example 1, and each was evaluated. The results are shown in Table 1.
  • Example 3 A metal silicon powder was prepared in the same manner as in Example 1. This metal silicon powder was mixed with fluorite, chromium oxide powder (Cr 2 O 3 ), and nickel oxide powder (NiO). In Example 3, the amount of fluorite based on the metal silicon powder was 1 mass%, the amount of chromium oxide powder was 1300 mass ppm, and the amount of nickel oxide was 1200 mass ppm. In Example 4, the amount of fluorite based on the metal silicon powder was 1 mass%, the amount of chromium oxide powder was 90 mass ppm, and the amount of nickel oxide was 20 mass ppm. A silicon nitride powder and a silicon nitride sintered body were prepared and evaluated in the same manner as in Example 1, except that the raw material powders prepared in this manner were used. The results were as shown in Table 1.
  • Example 5 Metal silicon powder was prepared in the same manner as in Example 1. Fluorite, chromium oxide powder (Cr 2 O 3 ) and nickel oxide powder (NiO) were blended and mixed with this metal silicon powder. In Examples 5 and 6, the blending amount of fluorite based on the metal silicon powder was 1 mass%, the blending amount of chromium oxide powder was 220 mass ppm, and the blending amount of nickel oxide was 80 mass ppm.
  • Silicon nitride powder and silicon nitride sintered body were prepared in the same manner as in Example 1, except that the raw material powder prepared in this manner was used and the wet grinding time of the calcined body when preparing the silicon nitride powder was 6 hours in Example 5 and 14 hours in Example 6, and each was evaluated. The results were as shown in Table 1.
  • Example 7 Metallic silicon powder was prepared in the same manner as in Example 1. Fluorite, chromium oxide powder ( Cr2O3 ) , and nickel oxide powder (NiO) were blended and mixed with this metallic silicon powder. The blending amount of fluorite based on the metallic silicon powder was 1 mass%, the blending amount of chromium oxide powder was 220 mass ppm, and the blending amount of nickel oxide was 80 mass ppm.
  • Silicon nitride powder and sintered silicon nitride were prepared and evaluated using the same procedures as in Example 1, except that the raw material powder prepared in this manner was used and the ratio of hydrogen gas in the atmosphere of the continuous furnace during the preparation of the silicon nitride powder (the remainder being nitrogen gas) was set as shown in Table 2. The results are shown in Table 2.
  • Example 9 A metal silicon powder was prepared in the same manner as in Example 1. Fluorite and stainless steel powder (SUS304) were blended and mixed with this metal silicon powder. In Example 9, the amount of fluorite based on the metal silicon powder was 1 mass%, and the amount of stainless steel powder was 200 mass ppm. In Example 10, the amount of fluorite based on the metal silicon powder was 1 mass%, and the amount of stainless steel powder was 90 mass ppm. In Example 11, the amount of fluorite based on the metal silicon powder was 1 mass%, and the amount of stainless steel powder was 1300 mass ppm. A silicon nitride powder and a silicon nitride sintered body were prepared in the same manner as in Example 1, except that the raw material powders prepared in this manner were used, and each was evaluated. The results were as shown in Table 2.
  • Example 12 The grinding time by the grinding device (device name: vibration mill (manufactured by Chuo Kakoki Co., Ltd.) used to obtain metal silicon powder from the metal silicon chunks was changed from 300 minutes to 420 minutes. Fluorite and stainless steel powder (SUS304) were blended and mixed with the metal silicon powder thus obtained. The blending amount of fluorite based on the metal silicon powder was 1 mass %, and the blending amount of stainless steel powder was 80 mass ppm. A silicon nitride powder and a silicon nitride sintered body were prepared and evaluated in the same manner as in Example 1 except that the raw material powder prepared in this manner was used. The results are shown in Table 2.
  • Example 13 The grinding time by the grinding device (device name: vibration mill (manufactured by Chuo Kakoki Co., Ltd.) used to obtain metal silicon powder from the metal silicon chunks was changed from 300 minutes to 240 minutes. Fluorite and stainless steel powder (SUS304) were blended and mixed with the metal silicon powder thus obtained. The blending amount of fluorite based on the metal silicon powder was 1 mass %, and the blending amount of stainless steel powder was 1000 mass ppm. A silicon nitride powder and a silicon nitride sintered body were prepared and evaluated in the same manner as in Example 1 except that the raw material powder prepared in this manner was used. The results are shown in Table 3.
  • Example 14 Metal silicon powder was prepared in the same manner as in Example 1. This metal silicon powder was mixed with fluorite and one or both of metal chromium powder (Cr) and metal nickel powder (Ni). In Example 14, the amount of fluorite based on the metal silicon powder was 1 mass%, and the amount of metal nickel powder was 150 mass ppm. In Example 15, the amount of fluorite based on the metal silicon powder was 1 mass%, and the amount of metal chromium powder was 150 mass ppm. In Example 16, the amount of fluorite based on the metal silicon powder was 1 mass%, the amount of metal chromium powder was 150 mass ppm, and the amount of metal nickel was 50 mass ppm. Except for using the raw material powder prepared in this manner, silicon nitride powder and silicon nitride sintered body were prepared and evaluated in the same manner as in Example 1. The results were as shown in Table 3.
  • Example 1 Metallic silicon powder was prepared in the same manner as in Example 1. This metallic silicon powder was mixed with only fluorite to prepare a raw material powder. A silicon nitride powder and a silicon nitride sintered body were prepared in the same manner as in Example 1, except that the raw material powder prepared in this manner was used, and each was evaluated. The results are shown in Table 3.
  • Example 2 The grinding time by the grinding device (device name: vibration mill, manufactured by Chuo Kakoki Co., Ltd.) when obtaining metal silicon powder from metal silicon chunks was changed from 300 minutes to 210 minutes.
  • the metal silicon powder thus obtained was mixed with fluorite, chromium oxide powder (Cr 2 O 3 ) and nickel oxide powder (NiO).
  • the amount of fluorite based on the metal silicon powder was 1 mass%
  • the amount of chromium oxide powder was 220 mass ppm
  • the amount of nickel oxide was 80 mass ppm.
  • a silicon nitride powder and a silicon nitride sintered body were prepared and evaluated in the same procedure as in Example 1, except that the raw material powder thus prepared was used. The results were as shown in Table 3.
  • the Weibull coefficients of the silicon nitride sintered bodies of Examples 1 to 16 were 9 or more, which was greater than those of Comparative Examples 1 and 2. This confirmed that the silicon nitride sintered bodies of Examples 1 to 16 had less variation in bending strength than the silicon nitride sintered bodies of Comparative Examples 1 and 2, and that the variation in quality had been sufficiently reduced.
  • silicon nitride sintered body with sufficiently reduced variation in quality. It is possible to provide a silicon nitride powder with excellent sinterability and sufficiently reduced variation in quality. It is possible to provide a method for producing silicon nitride powder that can efficiently produce the above-mentioned silicon nitride powder.

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Abstract

L'invention concerne une poudre de nitrure de silicium contenant : un composant de nitrure de silicium ayant un rapport de transformation alpha égal ou supérieur à 90,0 % ; et au moins un élément choisi dans le groupe constitué par un composant contenant du chrome et un composant contenant du nickel. La poudre de nitrure de silicium satisfait l'un ou les deux des éléments suivants : la teneur en composant contenant du chrome en termes d'équivalent Cr est de 50 à 250 μg/g, et la teneur en composant contenant du nickel en termes d'équivalent Ni est de 5 à 60 μg/g.
PCT/JP2024/009344 2023-03-22 2024-03-11 Poudre de nitrure de silicium et son procédé de production, et corps fritté de nitrure de silicium et son procédé de production Pending WO2024195609A1 (fr)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5930767A (ja) * 1982-08-12 1984-02-18 工業技術院長 窒化珪素反応焼結体の製造方法
JPS6437469A (en) * 1987-08-04 1989-02-08 Kazuaki Shimizu Production of ceramic of silicon nitride
JPH03193611A (ja) * 1989-12-21 1991-08-23 Denki Kagaku Kogyo Kk 複合窒化ケイ素粉末の製造方法
JPH10265269A (ja) * 1997-03-21 1998-10-06 Natl Inst For Res In Inorg Mater 窒化ケイ素焼結体の熱処理法
JP2014148429A (ja) * 2013-01-31 2014-08-21 Kyocera Corp 窒化珪素質多孔体およびフィルタ
JP2020023406A (ja) * 2016-12-12 2020-02-13 宇部興産株式会社 高純度窒化ケイ素粉末の製造方法
WO2021117829A1 (fr) * 2019-12-11 2021-06-17 宇部興産株式会社 Corps fritté à base de nitrure de silicium de type plaque et son procédé de fabrication
CN113493191A (zh) * 2020-04-08 2021-10-12 新疆晶硕新材料有限公司 制备高纯度α-氮化硅粉的方法及高纯度α-氮化硅粉

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5930767A (ja) * 1982-08-12 1984-02-18 工業技術院長 窒化珪素反応焼結体の製造方法
JPS6437469A (en) * 1987-08-04 1989-02-08 Kazuaki Shimizu Production of ceramic of silicon nitride
JPH03193611A (ja) * 1989-12-21 1991-08-23 Denki Kagaku Kogyo Kk 複合窒化ケイ素粉末の製造方法
JPH10265269A (ja) * 1997-03-21 1998-10-06 Natl Inst For Res In Inorg Mater 窒化ケイ素焼結体の熱処理法
JP2014148429A (ja) * 2013-01-31 2014-08-21 Kyocera Corp 窒化珪素質多孔体およびフィルタ
JP2020023406A (ja) * 2016-12-12 2020-02-13 宇部興産株式会社 高純度窒化ケイ素粉末の製造方法
WO2021117829A1 (fr) * 2019-12-11 2021-06-17 宇部興産株式会社 Corps fritté à base de nitrure de silicium de type plaque et son procédé de fabrication
CN113493191A (zh) * 2020-04-08 2021-10-12 新疆晶硕新材料有限公司 制备高纯度α-氮化硅粉的方法及高纯度α-氮化硅粉

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