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WO2024247755A1 - Procédé de production d'un corps fritté de nitrure de silicium - Google Patents

Procédé de production d'un corps fritté de nitrure de silicium Download PDF

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Publication number
WO2024247755A1
WO2024247755A1 PCT/JP2024/018194 JP2024018194W WO2024247755A1 WO 2024247755 A1 WO2024247755 A1 WO 2024247755A1 JP 2024018194 W JP2024018194 W JP 2024018194W WO 2024247755 A1 WO2024247755 A1 WO 2024247755A1
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WIPO (PCT)
Prior art keywords
sintered body
silicon nitride
sintering
sintered
density
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Application number
PCT/JP2024/018194
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English (en)
Japanese (ja)
Inventor
誠 長屋
昌克 前田
賢司 山田
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Tokuyama Corp
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Tokuyama Corp
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Publication of WO2024247755A1 publication Critical patent/WO2024247755A1/fr
Anticipated expiration legal-status Critical
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Classifications

    • 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
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes

Definitions

  • the present invention relates to a new method for producing sintered silicon nitride. More specifically, it provides a method for producing sintered silicon nitride that reduces the labor required for processing into the desired shape and makes it possible to obtain a sintered body with high dimensional accuracy.
  • silicon nitride sintered bodies which have high strength, hardness, high thermal conductivity and high toughness, are used as components for various industrial equipment such as circuit boards for power semiconductors, jigs for semiconductor manufacturing equipment and bearing balls, due to their characteristics such as resistance to cracking.
  • silicon nitride sintered bodies are produced by forming a raw material containing a mixture of silicon nitride powder, sintering aids, and binder into a green body, decomposing and removing the binder from the green body (degreasing), and then firing the green body.
  • the conventional manufacturing methods described above process the green body or degreased body before sintering to easily obtain the desired shape, but the strength of the green body and degreased body is low, so they are easily damaged during processing, and there is a concern that the product yield will decrease.
  • the application of external force for processing may cause dents and uneven density.
  • the object of the present invention is therefore to provide a manufacturing method capable of producing silicon nitride sintered bodies that have a high yield of molded bodies obtained by sintering and that have remarkably excellent surface precision, dimensional precision, etc., without sacrificing the processability of the conventional methods.
  • a pre-sintered body which is produced by stopping the firing process to obtain a silicon nitride sintered body so that the density falls within a specific range, is easy to process and remove by polishing, etc., and has sufficient strength during processing, so there is no risk of breakage. Furthermore, when the pre-sintered body is further fired after processing to produce a sintered body, changes due to subsequent sintering are suppressed, and a silicon nitride sintered body with significantly excellent surface precision and dimensional accuracy can be obtained, which led to the completion of the present invention.
  • a method for producing a silicon nitride sintered body which comprises sintering a green body containing silicon nitride powder and a sintering aid so that the density is 2.5 to 2.9 g/ cm3 (hereinafter also referred to as "pre-sintering") to obtain a pre-sintered body, subjecting the pre-sintered body to removal processing, and then sintering it so that the density is 3.0 g/ cm3 or more (hereinafter also referred to as "main sintering").
  • ⁇ -type silicon nitride powder in an amount of 60% by mass or more of the silicon nitride powder, as this reduces the occurrence of voids due to phase transition.
  • the material has workability comparable to that of the green body and the like used in the conventional method.
  • the removal process on a pre-sintered body having a higher strength than a green body or a degreased body, it is possible to achieve less breakage during processing and a high yield.
  • the sintered body obtained by further firing the pre-sintered body has an extremely small rate of change from the pre-sintered body, making it possible to manufacture silicon nitride sintered bodies with significantly excellent surface smoothness, dimensional accuracy, etc.
  • the manufacturing method of the present invention is characterized in that a green body containing silicon nitride powder and a sintering aid is pre-fired to a density of 2.5 to 2.9 g/ cm3 to obtain a pre-sintered body, the pre-sintered body is then subjected to removal processing, and then sintered at a temperature higher than that of the pre-sintering.
  • the green body basically contains silicon nitride powder and a sintering aid, and it is also possible to use additives such as binders to improve the strength of the green body.
  • any known silicon nitride powder may be used without any particular restrictions, but in order to reduce surface irregularities after the removal process described below, it is preferable to use a powder containing preferably 60% by mass or more, more preferably 80% by mass or more, of ⁇ -type silicon nitride powder, with the remainder being ⁇ -type silicon nitride powder. Whether the silicon nitride powder is ⁇ -type or not can be confirmed by X-ray diffraction measurement.
  • the average particle size of the silicon nitride powder is preferably 0.4 to 1.6 ⁇ m, and more preferably 0.8 to 1.2 ⁇ m.
  • the average particle size is the 50% value (D50) on a volume-based cumulative curve showing the particle size distribution obtained by measurement using a laser diffraction scattering method.
  • Al and Fe are preferably 75 ppm or less, and in particular 50 ppm or less, and Ca is preferably 100 ppm or less, and in particular 70 ppm or less.
  • the amount of metal impurities can be measured using an inductively coupled plasma atomic emission spectrometry (ICP-AES) or the like.
  • the sintering aid may be any known one without any particular limitation , such as Al2O3 , MgO, Y2O3 , ZrO2 , etc., which may be used alone or in combination as required, and metals or oxides of titanium, tungsten, molybdenum, etc. may be added as colorants.
  • any known binder may be used without any particular restrictions.
  • organic polymers acrylic resin, polyvinyl alcohol, etc.
  • acrylic resin polyvinyl alcohol, etc.
  • the amounts of the sintering aid, binder used as needed, and colorant used relative to the silicon nitride powder are not particularly limited, and known amounts may be used without any particular restrictions. Specifically, relative to 100 parts by mass of silicon nitride powder, the amount of the sintering aid is preferably 4 to 15 parts by mass, and more preferably 6 to 12 parts by mass, the amount of the binder is preferably 1 to 30 parts by mass, and more preferably 1 to 5 parts by mass, and the amount of the colorant is preferably 0 to 3 parts by mass.
  • the green body is formed into the desired shape of the sintered body by the removal processing of the pre-sintered body described below, so its shape is not particularly limited; however, in order to reduce the amount of removal processing of the pre-sintered body, it is preferable to form it into a shape that is close to the shape of the above-mentioned sintered body. That is, taking into account the shrinkage caused by sintering, it is preferable to mold it into a shape that is close to the desired shape of the silicon nitride sintered body.
  • the desired silicon nitride sintered body is a plate-like body, it is preferable to mold it into a plate-like shape, and if it is a sphere, it is preferable to mold it into a sphere or cube. Furthermore, if a complex shape is desired, it is preferable to form it into a shape that includes that shape, such as a cube or rectangular parallelepiped.
  • the green body can be molded by any known method without any particular restrictions.
  • methods such as the doctor blade method and the T-die method (extrusion molding) can be used, and in the case of a sphere, cube, or rectangular parallelepiped, methods such as press molding and injection molding can be used.
  • the green body when an organic substance is used as a binder, the green body is generally degreased.
  • the degreasing conditions can be any known method for decomposing the binder, without any particular restrictions.
  • the binder is decomposed and removed at 500 to 600°C in the presence of oxygen, such as in air.
  • the pre-firing conditions for the green body or degreased body may be any known firing condition without any particular restrictions. Specifically, it is preferable to perform the pre-firing in the presence of nitrogen. Although the appropriate temperature needs to be adjusted depending on the particle size of the raw materials and the amount of auxiliary agents, the firing temperature during pre-firing is preferably 1400 to 1650°C, and more preferably 1450 to 1550°C. The pressure may be reduced, normal, or increased without any particular restrictions.
  • the greatest feature of the present invention is that, in the above-mentioned pre-sintering, when the density of the pre-sintered body is 2.5 to 2.9 g/cm 3 , preferably 2.6 to 2.8 g/cm 3 , the firing is interrupted, the pre-sintered body is taken out, and the pre-sintered body is subjected to removal processing. That is, if the density of the pre-sintered body is higher than the above-mentioned range, the removal processing becomes difficult because it takes a long time to process or requires special processing techniques.
  • the density of the pre-sintered body is lower than the above-mentioned range, the strength of the pre-sintered body decreases, leading to a decrease in the yield during the removal processing, and the dimensional change due to the subsequent main firing also increases, which adversely affects the accuracy of the obtained sintered body.
  • the shavings during the removal processing may firmly adhere to the pre-sintered body, causing the appearance of the obtained sintered body to be poor.
  • the pre-sintered body having the above density has a lower Vickers hardness than a sintered body that has completed sintering, but a higher Vickers hardness than a general green body or a degreased body.
  • the Vickers hardness (Hv) measured with a pressing weight of 20 kgf is preferably 800 or less, and more preferably about 300 to 600.
  • the sintered body obtained by further firing it will have an extremely small change rate from the pre-sintered body, making it possible to produce silicon nitride sintered bodies with outstanding surface smoothness, dimensional accuracy, etc.
  • the means for adjusting the density of the pre-sintered body to within the above range is not particularly limited, but it is preferable to confirm the relationship between the density of the sintered body and the sintering temperature and time in advance through experiments, and then remove the pre-sintered body from the firing furnace after firing at a temperature and time that results in the density within the above range.
  • the removal processing of the pre-sintered body can be performed by using known processing methods such as grinding, cutting, polishing, etc., without any particular restrictions.
  • known removal processing methods such as surface grinding using a grindstone, lapping, polishing, barrel processing, cylindrical grinding, grinder processing, lathe processing using carbide, etc., and milling, and methods suitable for the desired finished shape can be used alone or in combination as appropriate.
  • the removal process may be carried out either dry or wet.
  • the liquid used When using a wet removal process, the liquid used must take into consideration ease of cleaning afterwards, and it is preferable to select a liquid that does not inhibit sintering during the main firing.
  • a water-based liquid with little organic matter specifically a liquid with less than 60% organic matter by mass.
  • a silicon carbide GC (green carborundum) grindstone as the grindstone used for the removal process, as it leaves little residual abrasive grains and does not inhibit sintering during the main firing.
  • a plate-shaped body of a predetermined thickness is produced as a provisional sintered body, taking into consideration the removal processing allowance and the shrinkage allowance due to main sintering of the desired silicon nitride sintered body, and one or both sides of the plate are then removed.
  • a rectangular or cubic block is manufactured as the pre-sintered body, and then cut into a plate of a specified thickness by milling, lathe processing, etc., taking into consideration the amount of removal processing required for the desired silicon nitride sintered body and the amount of shrinkage due to the final firing, and one or both sides are further removed using a grinding wheel as necessary.
  • a rectangular or cubic block is manufactured as a pre-sintered body, which is then cut into a sphere of a given size using a lathe, taking into account the amount of removal processing and shrinkage caused by firing, and then a grindstone is used to remove the sphere so that it approaches a perfect sphere.
  • the above-mentioned removal process not only allows adjustment of dimensional accuracy, but also makes it possible to reduce warping of the plate-shaped body by setting a large amount of grinding.
  • the slag generated by the removal process can be crushed, re-nitrided, etc. as necessary, and reused as a raw material for the sintered body, thereby improving the utilization rate of the silicon nitride powder.
  • the pre-sintered body after the grinding process is further sintered to obtain the desired silicon nitride sintered body.
  • the sintering conditions are preferably such that the density of the sintered body obtained is 3.0 g/ cm3 or more, particularly 3.2 g/cm3 or more .
  • the upper limit of the density of the sintered body obtained by the sintering is not particularly limited, but is, for example, 3.5 g/ cm3 .
  • the firing conditions for the main firing may be the same as those for the pre-firing, but in order to increase the density of the resulting sintered body as much as possible, it is preferable to perform firing at a temperature higher than the temperature (firing temperature) during the pre-firing.
  • the main firing at a temperature 5°C or higher, preferably 10°C or higher than the pre-firing temperature, and at a temperature not exceeding 1800°C, which is the decomposition temperature of silicon nitride under normal pressure, and even in the case of pressurization, it is preferable to perform the main firing at less than 1900°C so that voids are not generated due to evaporation of the sintering aid.
  • the silicon nitride sintered body obtained after the main firing may be subjected to removal processing in order to fine-tune the dimensions to the desired size or to further improve the smoothness of the surface.
  • Example 1 (plate-shaped body) ⁇ -type silicon nitride powder (average particle size 0.9 ⁇ m) and yttrium oxide powder and aluminum oxide powder as sintering aids were prepared. A water-soluble acrylic binder, a dispersant, and water were added to this raw material powder to prepare a raw material slurry. The mass% of each component when the total of the silicon nitride powder, the yttrium oxide powder, and the aluminum oxide powder is taken as 100 mass% is shown in the mixed raw material column in Table 1.
  • the prepared raw material slurry was then granulated by spray drying, and the resulting granules were pressure molded using a mold molding machine to obtain a green plate-shaped body with length: 20 mm x width: 20 mm, thickness: 8 mm, and density shown in Table 1.
  • the green body was then degreased to obtain a degreased body.
  • the degreased body was then placed in a sintering furnace, the atmosphere in the furnace was replaced with nitrogen gas, and the degreased body was then sintered at 1,520°C for 10 hours under a pressure of approximately 0.8 MPa to obtain a pre-sintered body with the density shown in Table 1.
  • the obtained pre-sintered body was subjected to removal processing (grinding) only in the thickness direction using a GC grinding wheel.
  • the target value for the grinding processing was set taking into account the shrinkage rate with respect to the final target thickness of 6.50 mm. Water was used as the grinding fluid.
  • the dimensions of the pre-sintered body obtained by the removal processing and the time required for the removal processing are shown in Table 1.
  • the sample was ultrasonically cleaned using pure water to remove grinding powder, and then dried.
  • the pre-sintered body was placed in a sintering furnace, the atmosphere in the furnace was replaced with nitrogen gas, and the temperature was raised to 1850°C under a pressure of approximately 0.8 MPa and held for 10 hours to produce a plate-shaped sintered body.
  • the thickness (final target thickness: 6.5 mm) and density of the obtained sintered body are shown in Table 1.
  • Example 2 to 4 Sintered bodies were produced in the same manner as in Example 1, except that the density of the pre-sintered body was changed by changing the amount of sintering aid and the temperature during pre-sintering as shown in Table 1. The results are shown in Table 1.
  • Example 1 (plate-shaped body)> A green body was obtained in the same manner as in Example 1 except that the amount of sintering aid was as shown in Table 1. The obtained green body was then subjected to the same grinding and cleaning as in Example 1 without being degreased or pre-fired. However, the shape was distorted and the desired sintered body shape could not be obtained.
  • Example 2 (plate-shaped body)> A degreased body was obtained in the same manner as in Example 1 except that the amount of sintering aid was as shown in Table 1. The obtained degreased body was then ground and washed in the same manner as in Example 1 without being pre-fired. However, the shape was distorted and the desired sintered body shape could not be obtained.
  • Example 3 ⁇ Comparative Example 3 (plate-shaped body)>
  • the sintered body was produced in the same manner, except that the amount of sintering aid was adjusted and the temperature during pre-sintering was changed to change the density of the pre-sintered body, as shown in Table 1.
  • the target thickness after removal processing was set to 6.58 mm in consideration of the shrinkage rate, but even after 20 hours of grinding processing, the target thickness was 7.18 mm, which was not reached. The results are shown in Table 1.
  • Examples 5 and 6 Granules were prepared in the same manner as in Example 1, except that the amount of sintering aid was as shown in Table 1. The obtained granules were then pressure-molded using a mold molding machine to obtain a roughly spherical green body having a diameter of 15 mm and a density of 2.2 g/ cm3 . The green body was degreased to obtain a degreased body having the density shown in Table 1.
  • the degreased body was placed in a firing furnace, and the inside of the firing furnace was replaced with nitrogen gas, after which the degreased body was calcined under the conditions shown in Table 1 to obtain a calcined body.
  • the densities at this time were 2.80 g/cm 3 and 2.78 g/cm 3 , respectively.
  • the obtained pre-sintered body was subjected to removal processing (grinding/polishing) on the entire surface using a GC grinding wheel.
  • the target grinding/polishing processing value was set taking into account the shrinkage rate with respect to the final target diameter of 13.0 mm. Water was used as the grinding/polishing processing liquid.
  • the dimensions of the pre-sintered body obtained by the removal processing and the time required for grinding/polishing are shown in Table 1. After the above grinding/polishing processing, ultrasonic cleaning was performed using pure water to remove grinding/polishing residue, and then the body was dried.
  • the pre-sintered body was placed in a sintering furnace, the inside of the furnace was replaced with nitrogen gas, and then it was sintered under the conditions shown in Table 1 to produce a spherical sintered body.
  • the density and thickness of the obtained sintered body (final target diameter: 13.0 mm) are shown in Table 1.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

Un procédé de production d'un corps fritté de nitrure de silicium selon la présente invention est caractérisé en ce qu'après qu'un corps vert contenant une poudre de nitrure de silicium et un auxiliaire de frittage est cuit de telle sorte que la densité devient de 2,5 à 2,9 g/cm3 pour obtenir un corps temporairement fritté, le corps temporairement fritté est soumis à un traitement d'élimination puis cuit de telle sorte que la densité devient d'au moins 3,0 g/cm3.　La présente invention peut fournir un procédé qui est destiné à produire un corps fritté de nitrure de silicium et par lequel le travail requis pour le traitement en une forme souhaitée peut être réduit et un corps fritté ayant une précision dimensionnelle élevée peut être obtenu.
PCT/JP2024/018194 2023-05-29 2024-05-16 Procédé de production d'un corps fritté de nitrure de silicium Pending WO2024247755A1 (fr)

Applications Claiming Priority (2)

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JP2023-087401 2023-05-29
JP2023087401 2023-05-29

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WO2024247755A1 true WO2024247755A1 (fr) 2024-12-05

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5996912A (ja) * 1982-11-26 1984-06-04 株式会社東芝 セラミツク製品の製造法
JPS6011261A (ja) * 1983-06-23 1985-01-21 黒崎窯業株式会社 セラミツクス焼結体の製造方法
JP2009215141A (ja) * 2008-03-12 2009-09-24 Ngk Insulators Ltd セラミックス製マイクロ精密部品の製造方法
CN109608204A (zh) * 2019-01-31 2019-04-12 山东工业陶瓷研究设计院有限公司 一种高硬度Si3N4陶瓷天线罩高效精密加工制备方法
WO2019167879A1 (fr) * 2018-02-28 2019-09-06 株式会社トクヤマ Méthode de fabrication de poudre de nitrure de silicium

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5996912A (ja) * 1982-11-26 1984-06-04 株式会社東芝 セラミツク製品の製造法
JPS6011261A (ja) * 1983-06-23 1985-01-21 黒崎窯業株式会社 セラミツクス焼結体の製造方法
JP2009215141A (ja) * 2008-03-12 2009-09-24 Ngk Insulators Ltd セラミックス製マイクロ精密部品の製造方法
WO2019167879A1 (fr) * 2018-02-28 2019-09-06 株式会社トクヤマ Méthode de fabrication de poudre de nitrure de silicium
CN109608204A (zh) * 2019-01-31 2019-04-12 山东工业陶瓷研究设计院有限公司 一种高硬度Si3N4陶瓷天线罩高效精密加工制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HIROTSURU, HIDEKI ET AL.: "Relation between Grain Growth and Phase Transformation of Silicon Nitride", JOURNAL OF THE CERAMIC SOCIETY OF JAPAN, vol. 103, no. 5, 1995, pages 464 - 469, XP093246040, ISSN: 0914-5400, DOI: 10.2109/jcersj.103.464 *

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