WO2022202621A1 - Poudre de nitrure de silicium et procédé de production associé, et corps fritté en nitrure de silicium et procédé de production associé - Google Patents

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

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WO2022202621A1
WO2022202621A1 PCT/JP2022/012341 JP2022012341W WO2022202621A1 WO 2022202621 A1 WO2022202621 A1 WO 2022202621A1 JP 2022012341 W JP2022012341 W JP 2022012341W WO 2022202621 A1 WO2022202621 A1 WO 2022202621A1
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silicon nitride
powder
mass
raw material
nitride powder
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PCT/JP2022/012341
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Japanese (ja)
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直嗣 野上
稔男 田中
豪 竹田
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デンカ株式会社
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Priority to JP2022545936A priority Critical patent/JP7239787B2/ja
Priority to CN202280021892.6A priority patent/CN117120397A/zh
Publication of WO2022202621A1 publication Critical patent/WO2022202621A1/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

  • the present disclosure relates to a silicon nitride powder and its manufacturing method, and a silicon nitride sintered body and its manufacturing method.
  • Silicon nitride is a material with excellent strength, hardness, toughness, heat resistance, corrosion resistance, thermal shock resistance, etc., so it is used for various industrial parts such as die casting machines and melting furnaces, and automobile parts. .
  • the use of silicon nitride substrates as insulating substrates for power modules of automobiles, machine tools, etc. is also under study. For such applications, high heat dissipation is required. Therefore, Patent Document 1 proposes the use of silicon nitride powder with reduced impurities in order to obtain a silicon nitride sintered body having high thermal conductivity.
  • the present disclosure provides a silicon nitride powder with sufficiently reduced impurities and capable of producing a sintered body having excellent mechanical properties, and a method for producing the same. Also provided are a silicon nitride sintered body in which impurities are sufficiently reduced and which has excellent mechanical properties, and a method for producing the same.
  • the present disclosure provides a silicon nitride powder having a fluorine content of 600 mass ppm or less, a carbon content of 0.1 mass% or less, and a ⁇ conversion rate of 80% or more.
  • This silicon nitride powder has sufficiently low fluorine and carbon contents and a high alpha conversion rate.
  • This silicon nitride powder has sufficiently reduced impurities and can be used for various purposes. For example, if this silicon nitride powder is used for a sintered body, a sintered body having excellent mechanical properties can be obtained.
  • the ⁇ conversion rate of the silicon nitride powder may be 90% or more. By using this silicon nitride powder as a raw material for sintering, a sintered body having high fracture toughness can be obtained.
  • the silicon nitride powder may have a ⁇ conversion rate of 98% or less. This can reduce the manufacturing cost of the silicon nitride powder.
  • the present disclosure includes a raw material powder containing a silicon powder and having a fluoride content of 1 part by mass or less with respect to 100 parts by mass of the silicon powder, having a bulk density of 0.7 g/cm 3 or more and a filling height of the raw material powder of A filling step of filling the container so as to have a thickness of 15 to 80 mm, a firing step of firing the raw material powder filled in the container in an atmosphere containing nitrogen gas to obtain a fired product containing silicon nitride, and a firing step of obtaining a fired product. and a pulverizing step of pulverizing.
  • raw material powder having a fluoride content of 1 part by mass or less is filled into a container to a predetermined bulk density and filling height, and fired in an atmosphere containing nitrogen gas. Therefore, the nitriding reaction proceeds appropriately, and a silicon nitride powder having a high alpha conversion rate and a reduced fluorine content can be obtained.
  • This silicon nitride powder has sufficiently reduced impurities and can be used for various purposes. For example, if it is used for a sintered body, a sintered body having excellent mechanical properties can be produced at low cost.
  • the firing process may be performed in an atmosphere containing nitrogen gas and hydrogen gas. This promotes the formation of silicon nitride, and a silicon nitride powder having high purity can be obtained in a short firing time. Therefore, the manufacturing cost of silicon nitride powder can be reduced.
  • the carbon content in the raw material powder may be 0.1% by mass or less. This makes it possible to obtain a silicon nitride powder having a low carbon content and a high alpha conversion rate. By using such a silicon nitride powder as a raw material for sintering, a sintered body having excellent mechanical properties can be obtained.
  • the silicon nitride powder may have a fluorine content of 600 mass ppm or less, a carbon content of 0.1 mass% or less, and an ⁇ conversion rate of 80% or more.
  • the present disclosure provides a method for producing a silicon nitride sintered body, which has a sintering step of molding and firing a sintering raw material containing the silicon nitride powder produced by any of the above production methods. According to this manufacturing method, a silicon nitride sintered body having excellent mechanical properties can be manufactured at low cost.
  • the present disclosure provides a silicon nitride sintered body having a fluorine content of 600 mass ppm or less and a carbon content of 0.1 mass% or less.
  • This silicon nitride sintered body has sufficiently reduced impurities and has excellent mechanical properties.
  • the silicon nitride powder (Si 3 N 4 powder) according to one embodiment has a fluorine content of 600 mass ppm or less and a carbon content of 0.1 mass ppm or less.
  • a sintered body obtained by using such a silicon nitride powder as a sintering raw material has sufficiently high bending strength at room temperature (20° C.) and high temperature (1300° C.). Moreover, since the contents of fluorine and carbon are sufficiently low, it can be suitably used for various applications without being limited to sintered bodies.
  • the fluorine content of the silicon nitride powder may be 300 mass ppm or less, 100 mass ppm or less, or even 60 mass ppm or less. good. From the viewpoint of ease of production, the fluorine content may be 5 mass ppm or more, 10 mass ppm or more, or 30 mass ppm or more. An example of the fluorine content of silicon nitride powder is 5 to 600 mass ppm.
  • the carbon content of the silicon nitride powder is 0.1% by mass or less.
  • a sintered body obtained by using such a silicon nitride powder as a sintering raw material has sufficiently high bending strength at room temperature (20° C.) and high temperature (1300° C.).
  • the carbon content of the silicon nitride powder may be 0.08% by mass or less, may be 0.07% by mass or less, and may be 0.06% by mass. % or less.
  • the carbon content of the silicon nitride powder may be 0.01% by mass or more, or may be 0.02% by mass or more.
  • An example of the carbon content of silicon nitride powder is 0.01 to 0.1% by mass.
  • the carbon contained in the silicon nitride powder is derived from the organic binder and the material of the container when molding the raw material powder. Normally, even if the raw material powder is fired as it is, the nitriding does not progress sufficiently, so it may be fired as a compact. At this time, a binder such as polyvinyl alcohol is used to ensure moldability. By changing the amount of the binder used, the carbon content of the silicon nitride powder can be adjusted. The carbon content of the silicon nitride powder can be determined by the "combustion (high-frequency heating) - infrared absorption method" in "11 carbon determination method" of JIS R 1603:2007. In addition, when manufacturing the silicon nitride powder of this embodiment, it is not necessary to use an organic binder.
  • the purity of the silicon nitride powder may be 99% by mass or higher, 99.5% by mass or higher, or 99.8% by mass or higher.
  • the ⁇ conversion rate of the silicon nitride powder (the phase ratio of ⁇ -Si 3 N 4 to the whole Si 3 N 4 ) is 80% or more.
  • a sintered body obtained by using such a silicon nitride powder as a sintering raw material has excellent mechanical properties. From the viewpoint of further improving the fracture toughness, the alpha conversion rate of the silicon nitride powder may be 85% or more, 88% or more, or 90% or more.
  • the ⁇ conversion rate of the silicon nitride powder may be 98% or less, 97% or less, or 96% or less.
  • An example of the ⁇ conversion rate of silicon nitride powder is 80 to 98%.
  • the ⁇ conversion rate of the silicon nitride powder (the phase ratio of ⁇ -Si 3 N 4 to the entire Si 3 N 4 ) may be 20% or less, preferably 15% or less, from the viewpoint of sufficiently increasing the alpha conversion rate. may be 12% or less, or may be 10% or less.
  • the ⁇ conversion rate of the silicon nitride powder may be 2% or more, or may be 4% or more, from the viewpoint of ease of production.
  • the alpha conversion rate of silicon nitride powder depends on the firing conditions. If the nitriding reaction of the raw material powder proceeds appropriately, it is possible to obtain a silicon nitride powder having a high degree of alpha conversion. On the other hand, if the nitriding reaction of the raw material powder progresses rapidly or the contact between the raw material powders is insufficient, the ⁇ conversion rate tends to decrease.
  • the ⁇ conversion rate of the silicon nitride powder can be obtained from the diffraction line intensity of X-ray diffraction.
  • a method for producing a silicon nitride powder includes a raw material powder containing silicon powder and having a fluoride content of 1 part by mass or less with respect to 100 parts by mass of the silicon powder, and having a bulk density of 0.7 g/cm 3 or more. , and a filling step of filling the container so that the filling height of the raw material powder is 15 to 80 mm, and firing the raw material powder filled in the container in an atmosphere containing nitrogen gas, and firing containing silicon nitride It has a sintering step of obtaining a product and a pulverizing step of pulverizing the sintered product.
  • the raw material powder may contain a fluoride containing Li, Na, K, Mg, Ca, Sr or Ba as a constituent element in order to promote nitridation.
  • the content of fluoride with respect to 100 parts by mass of the silicon powder may be 0.5 parts by mass or less, or 0.3 parts by mass or less. good.
  • the raw material powder may not contain fluoride. If necessary, the silicon powder may be pretreated with an acid to reduce impurities in the silicon powder.
  • the silicon nitride powder can be produced without using an organic binder. Therefore, a silicon nitride powder with a sufficiently low carbon content can be produced.
  • the carbon content of the raw material powder may be 0.1% by mass or less.
  • the carbon content in the raw material powder can be determined by the "combustion (high-frequency heating) - infrared absorption method" in "11 carbon determination method" of JIS R 1603:2007.
  • the container filled with the raw material powder can be made of a material that does not change in quality up to a temperature of 1500°C under an inert atmosphere.
  • the container can be made of alumina, boron nitride, or carbon.
  • the structure of the container is not particularly limited, and for example, a container capable of forming an accommodation space for accommodating the raw material powder can be used.
  • the container body may include a container body having a recess and a lid covering the recess of the body.
  • a container is filled with the raw material powder so that the bulk density of the raw material powder is 0.7 g/cm 3 or more.
  • the nitridation of the silicon powder proceeds appropriately, and a silicon nitride powder having a high alpha conversion rate can be obtained.
  • the bulk density of the raw material powder in the container may be 0.8 g/cm 3 or more, or 0.9 g/cm 3 or more.
  • the bulk density of the raw material powder in the container may be 1.6 g/cm 3 or less, 1.2 g/cm 3 or less, or 1.0 g/cm 3 or less.
  • the calorific value tends to increase and the amount of ⁇ -Si 3 N 4 phase produced tends to increase. In addition, it may become difficult to fill the container.
  • An example of the bulk density of the raw material powder in the container is 0.7-1.6 g/cm 3 .
  • the filling height (thickness in the vertical direction) of the raw material powder in the container is 15 to 80 mm, and may be 20 to 60 mm. With such a filling height, the nitriding reaction proceeds smoothly.
  • the filling height of the raw material powder can be measured as the height along the vertical direction from the bottom of the container.
  • the raw material powder filled in the container is fired in an atmosphere containing nitrogen gas to nitride the silicon powder contained in the raw material powder.
  • concentration of nitrogen gas in the atmosphere during firing may be 90% by volume or more, 95% by volume or more, or 97% by volume or more.
  • the atmosphere during firing may contain nitrogen gas and other gases different from nitrogen gas.
  • gases include argon gas and hydrogen gas.
  • argon gas By adding argon gas, the reaction rate of the nitriding reaction can be adjusted.
  • hydrogen gas By adding hydrogen gas, oxides such as SiO 2 contained in the raw material powder can be reduced, and silicon nitride powder having high purity can be produced.
  • the content of hydrogen gas in the atmosphere during firing may be 1% by volume or more, or may be 2% by volume or more.
  • the content of hydrogen gas in the atmosphere during firing may be 5% by volume or less.
  • An example of the content of hydrogen gas in the atmosphere during firing is 1 to 5% by volume.
  • Gas content (% by volume) in this specification is a value under standard conditions (0° C., 1 atm).
  • the firing process may include multiple stages with different firing temperature ranges.
  • the multiple stages may include the following first stage and second stage.
  • the temperature is raised to the temperature range (1) of 1100 to 1200° C. and maintained. If the holding temperature in the first stage is too low, the nitriding reaction tends to be difficult to proceed. On the other hand, if the holding temperature in the first stage is too high, the nitriding reaction proceeds rapidly, increasing the amount of ⁇ -Si 3 N 4 ( ⁇ phase) produced.
  • the holding time in temperature range (1) may be from 2 to 12 hours. If the holding time is too short, the nitriding reaction may not proceed sufficiently. If the holding time is too long, the productivity of the silicon nitride powder will decrease.
  • the temperature is raised to the temperature range (2) of 1400-1500°C and maintained.
  • the temperature range (2) of 1400-1500°C and maintained.
  • unreacted Si can be sufficiently reduced. If the holding temperature in this second stage is too low, the residual amount of unreacted Si tends to increase. On the other hand, if the holding temperature in this second stage is too high, the resulting silicon nitride tends to undergo a transition from the ⁇ -phase to the ⁇ -phase.
  • the holding time in temperature range (2) may be from 1 to 8 hours. If the holding time is too short, unreacted Si tends to remain. If the holding time is too long, the productivity of the silicon nitride powder will decrease.
  • a pulverizing step of pulverizing the fired product obtained in the firing step is performed. Pulverization may be performed in multiple steps of coarse pulverization and fine pulverization. Grinding may be performed wet, for example using a ball mill. The fired product may be pulverized until the specific surface area reaches 8.0 to 15.0 m 2 /g.
  • a silicon nitride powder having a low fluorine content and a low carbon content and a high alpha conversion rate For example, a silicon nitride powder having a fluorine content of 600 mass ppm or less, a carbon content of 0.1 mass % or less, and a ⁇ conversion rate of 80% or more can be obtained. Since such silicon nitride powder has a low impurity concentration, it can be suitably used for various purposes. For example, by using it as a raw material for sintering, a sintered body having excellent mechanical properties can be obtained.
  • the ⁇ conversion rate may be 85% or more, 88% or more, or 90% or more.
  • the ⁇ conversion rate may be 98% or less, 97% or less, or 96% or less.
  • An example of the ⁇ conversion rate range is 80 to 98%.
  • a treatment process may be performed as necessary.
  • the pulverized fired product and hydrofluoric acid having a hydrogen fluoride concentration of 10 to 40% by mass may be blended to reduce impurities.
  • the pulverized fired product may be dispersed in hydrofluoric acid for treatment.
  • the concentration of hydrogen fluoride in hydrofluoric acid may be 15-30% by mass.
  • the temperature of hydrofluoric acid in the treatment step is, for example, 40-80.degree.
  • the time for immersing the silicon nitride powder in hydrofluoric acid is, for example, 1 to 10 hours.
  • the sintering raw material is pressed with a molding pressure of, for example, 3.0 to 30 MPa to obtain a compact.
  • the compact may be produced by uniaxial pressing or may be produced by CIP. Moreover, you may bake while shape
  • the firing temperature may be 1860-2100°C, or 1880-2000°C.
  • the firing time at the firing temperature may be 6 to 20 hours, or 8 to 16 hours.
  • the heating rate to the firing temperature may be, for example, 1.0 to 10.0° C./hour.
  • the silicon nitride sintered body produced in this way has a low production cost and excellent mechanical properties. In addition, since impurities are reduced, it can be used for various purposes.
  • the silicon nitride sintered body has a fluorine content of 600 mass ppm or less, a carbon content of 0.1 mass% or less, and a alpha conversion rate of 80% or more.
  • the fluorine content of the silicon nitride sintered body may be 300 mass ppm or less, 100 mass ppm or less, or 60 mass ppm or less. There may be. From the viewpoint of ease of manufacture, the fluorine content of the silicon nitride sintered body may be 5 mass ppm or more, 10 mass ppm or more, or 30 mass ppm or more. An example of the fluorine content of the silicon nitride sintered body is 5 to 600 mass ppm.
  • Such a silicon nitride sintered body can be produced using a sintering raw material having a fluorine content within the above range.
  • the carbon content of the silicon nitride sintered body is 0.1% by mass or less.
  • Such a silicon nitride sintered body has sufficiently high bending strength at room temperature (20° C.) and high temperature (1300° C.). From the viewpoint of obtaining a silicon nitride sintered body having higher bending strength, the carbon content of the silicon nitride sintered body may be 0.08% by mass or less, or 0.07% by mass or less, It may be 0.06% by mass or less. From the viewpoint of ease of manufacture, the carbon content of the silicon nitride sintered body may be 0.01% by mass or more, or may be 0.02% by mass or more.
  • Such a silicon nitride sintered body can be produced using a sintering raw material having a carbon content within the above range.
  • the fluorine and carbon contents of the silicon nitride sintered body can be measured in the same manner as the silicon nitride powder using a sample obtained by pulverizing the silicon nitride sintered body into powder.
  • silicon nitride powder may be used as a raw material for sintering composite sintered bodies of silicon nitride and other substances. Moreover, you may use for uses other than a sintering raw material.
  • a raw material powder was prepared by blending 1 part by mass of fluorite with 100 parts by mass of silicon powder. That is, the raw material powder contained 1 part by mass of fluoride (fluorite) with respect to 100 parts by mass of silicon powder.
  • the carbon content in the raw material powder was 0.1% by mass or less.
  • An alumina container having a main body with a recess and a lid was prepared. The recess was filled with raw material powder.
  • the bulk density of the raw material powder after filling was 1 g/cm 3 .
  • the filling shape of the raw material powder was a rectangular parallelepiped, and the filling height was 45 mm.
  • the concave portion of the main body was covered with a lid, and the raw material powder was placed in an alumina container.
  • the raw material powder accommodated in the container was sintered in the following procedure.
  • Example 1 The obtained ingot was coarsely pulverized and then wet-pulverized with a ball mill. After that, it was dried under a nitrogen atmosphere. Thus, the silicon nitride powder of Example 1 was prepared.
  • the fluorine content of the silicon nitride powder was measured in the following manner.
  • the silicon nitride powder was heated using an automatic sample combustion apparatus (manufactured by Mitsubishi Chemical Corporation, device name: AQF-2100H type), and the generated gas was dissolved in water. Fluorine dissolved in water was measured using an ion chromatograph (manufactured by Thermo Fisher Scientific, device name: ICS-2100). Based on this measured value, the fluorine content of the silicon nitride powder was calculated.
  • the carbon content of the silicon nitride powder was measured by the "combustion (high-frequency heating) - infrared absorption method" in "11 carbon determination method” of JIS R 1603:2007.
  • CS-444LS trade name manufactured by LECO was used for the measurement.
  • the sample (silicon nitride powder) was combusted together with the combustion aid by high-frequency heating.
  • the carbon content in the sample was measured by quantifying the generated carbon dioxide by an infrared absorption method.
  • the bending strength is a three-point bending bending strength, and was measured using a commercially available bending strength meter (manufactured by Shimadzu Corporation, device name: AG-2000) in accordance with JIS R 1601:2008. Measurements were taken at room temperature (20°C) and 1300°C. The results (relative values) were as shown in Table 1.
  • the fracture toughness (K IC ) is a value measured by the SEPB method, and was measured using a commercially available measuring device (manufactured by Instron, device name: universal testing machine 5582) in accordance with JIS R1607:2015. The results (relative values) were as shown in Table 1.
  • Example 3 Example 1 except that fluoride (fluorite) was not blended during the preparation of the raw material powder, and the atmosphere during firing was the same mixed gas of nitrogen gas and hydrogen gas as in Example 2.
  • a silicon nitride powder was prepared in the same manner. The silicon nitride powder thus prepared was evaluated in the same manner as in Example 1. The results were as shown in Table 1. Using the silicon nitride powder thus prepared, a silicon nitride sintered body was produced and evaluated in the same manner as in Example 1. The results were as shown in Table 1.
  • Example 5 The temperature conditions for firing the raw material powder were as follows. The temperature was raised to 1150°C at a temperature elevation rate of 5°C/min. After holding the temperature at 1150° C. for 12 hours, the temperature was raised to 1450° C. at a rate of 0.018° C./min. After being held at a temperature of 1450° C. for 4 hours, it was naturally cooled to room temperature. A silicon nitride powder was prepared in the same manner as in Example 1, except that the temperature conditions during firing were set as described above. The silicon nitride powder thus prepared was evaluated in the same manner as in Example 1. The results were as shown in Table 1. Using the silicon nitride powder thus prepared, a silicon nitride sintered body was produced and evaluated in the same manner as in Example 1. The results were as shown in Table 1.
  • Example 1 A silicon nitride powder was prepared in the same manner as in Example 1, except that the amount of fluoride (fluorite) mixed with 100 parts by mass of the silicon powder was 2 parts by mass during the preparation of the raw material powder.
  • the silicon nitride powder thus prepared was evaluated in the same manner as in Example 1. The results were as shown in Table 2.
  • a silicon nitride sintered body was produced and evaluated in the same manner as in Example 1. The results were as shown in Table 2.
  • Example 2 A raw material powder was prepared in the same manner as in Example 1, except that the amount of fluoride (fluorite) mixed with 100 parts by mass of the silicon powder was 0.2 parts by mass. 5 parts by mass of polyvinyl alcohol was blended with 100 parts by mass of this raw material powder to obtain a kneaded material. This kneaded material was molded using a high-temperature press to obtain a molded body. Firing was carried out in the same manner as in Example 2, except that a compact was used instead of the container, and that the rate of temperature increase from 1150°C to 1450°C was changed to 0.035°C/min. to prepare silicon nitride powder. The silicon nitride powder thus prepared was evaluated in the same manner as in Example 1. The results were as shown in Table 2. Using the silicon nitride powder thus prepared, a silicon nitride sintered body was produced and evaluated in the same manner as in Example 1. The results were as shown in Table 2.
  • Example 3 A raw material powder was prepared in the same manner as in Example 1, except that the amount of fluoride (fluorite) mixed with 100 parts by mass of silicon powder was 1 part by mass. 5 parts by mass of polyvinyl alcohol was blended with 100 parts by mass of this raw material powder to obtain a kneaded material. This kneaded material was molded using a high-temperature press to obtain a molded body. Silicon nitride powder was prepared in the same manner as in Comparative Example 2, except that this compact was used and the atmosphere during firing was changed to nitrogen gas only.
  • fluoride fluorite
  • the silicon nitride powder thus prepared was evaluated in the same manner as in Example 1. The results were as shown in Table 2. Using the silicon nitride powder thus prepared, a silicon nitride sintered body was produced and evaluated in the same manner as in Example 1. The results were as shown in Table 2.
  • Silicon nitride powder was prepared in the same manner as in Example 1, except that the filling height and filling density of the raw material powder in the container were changed as shown in Table 2.
  • the silicon nitride powder thus prepared was evaluated in the same manner as in Example 1. The results were as shown in Table 2.
  • a silicon nitride sintered body was produced and evaluated in the same manner as in Example 1. The results were as shown in Table 2.
  • the bending strength and fracture toughness in Tables 1 and 2 are relative values based on Comparative Example 3. It was confirmed that the silicon nitride sintered bodies of Examples 1-5 had better mechanical properties than the silicon nitride sintered bodies of Comparative Examples 1-4. It is considered that the carbon contained in the silicon nitride powder of each example was unavoidably mixed from raw materials and manufacturing equipment.
  • a silicon nitride powder and a method for producing the same which have sufficiently reduced impurities and are capable of producing a sintered body having excellent mechanical properties. It is possible to provide a method for producing a silicon nitride sintered body that can produce a silicon nitride sintered body having excellent mechanical properties.

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Abstract

L'invention concerne une poudre de nitrure de silicium qui contient du fluor en une quantité qui n'est pas supérieure à 600 ppm en masse et du carbone en une quantité qui n'est pas supérieure à 0,1 % en masse et qui a un taux de conversion α supérieur ou égal à 80 %. L'invention concerne également un procédé de production d'une poudre de nitrure de silicium, ledit procédé comprenant : une étape de remplissage pour remplir un récipient avec une poudre de matière première de telle sorte que la densité apparente n'est pas inférieure à 0,7 g/cm3 et la hauteur de remplissage de la poudre de matière première est de 15 à 80 mm, la poudre de matière première contenant une poudre de silicium et contenant du fluorure en une quantité inférieure ou égale à 1 partie en masse par rapport à 100 parties en masse de la poudre de silicium ; une étape de cuisson pour cuire la poudre de matière première avec laquelle le récipient est rempli dans une atmosphère contenant de l'azote gazeux pour obtenir un produit cuit contenant du nitrure de silicium ; et une étape de broyage pour broyer le produit cuit.
PCT/JP2022/012341 2021-03-25 2022-03-17 Poudre de nitrure de silicium et procédé de production associé, et corps fritté en nitrure de silicium et procédé de production associé WO2022202621A1 (fr)

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JP2022545936A JP7239787B2 (ja) 2021-03-25 2022-03-17 窒化ケイ素粉末及びその製造方法、並びに、窒化ケイ素焼結体の製造方法
CN202280021892.6A CN117120397A (zh) 2021-03-25 2022-03-17 氮化硅粉末及其制造方法、以及氮化硅烧结体及其制造方法

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JP2021051259 2021-03-25

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