JPH06329404A - Silicon nitride powder - Google Patents
Silicon nitride powderInfo
- Publication number
- JPH06329404A JPH06329404A JP5122595A JP12259593A JPH06329404A JP H06329404 A JPH06329404 A JP H06329404A JP 5122595 A JP5122595 A JP 5122595A JP 12259593 A JP12259593 A JP 12259593A JP H06329404 A JPH06329404 A JP H06329404A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- nitride powder
- oxygen
- amount
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- 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
- C01B21/0687—After-treatment, e.g. grinding, purification
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、高温強度と耐摩耗性に
優れた窒化珪素焼結体の原料として好適な易焼結性の窒
化珪素粉末に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an easily sinterable silicon nitride powder suitable as a raw material for a silicon nitride sintered body having excellent high temperature strength and wear resistance.
【０００２】[0002]
【従来技術及びその問題点】窒化珪素焼結体は、高強
度、耐蝕性、耐熱衝撃性等に優れているため、近年ガス
タービン部品、自動車エンジン部品等の高温構造材料と
して注目されている。このような窒化珪素焼結体は、通
常、窒化珪素粉末に焼結助剤を混合し、プレス成形、射
出成形、押し出し成形等によって成形体とし、この成形
体を焼結することによって製造される。2. Description of the Related Art Sintered silicon nitride has been attracting attention as a high-temperature structural material for gas turbine parts, automobile engine parts, etc. in recent years because it is excellent in high strength, corrosion resistance and thermal shock resistance. Such a silicon nitride sintered body is usually produced by mixing a silicon nitride powder with a sintering aid to obtain a molded body by press molding, injection molding, extrusion molding or the like, and sintering the molded body. .
【０００３】これらの各手法において、窒化珪素焼結体
を製造する場合、原料となる窒化珪素粉末の粉体特性、
特に酸素量が焼結性及び得られる焼結体の特性に大きく
影響することが知られている。In each of these methods, when a silicon nitride sintered body is manufactured, powder characteristics of silicon nitride powder as a raw material,
In particular, it is known that the amount of oxygen greatly affects the sinterability and the properties of the obtained sintered body.
【０００４】即ち、一般に酸素量の多い窒化珪素粉末は
易焼結性であるが十分な高温強度が得られない。また、
酸素量の少ない窒化珪素粉末は難焼結性であり、十分に
緻密化させることが難しい。That is, in general, a silicon nitride powder containing a large amount of oxygen is easy to sinter, but sufficient high temperature strength cannot be obtained. Also,
Silicon nitride powder having a small amount of oxygen is difficult to sinter, and it is difficult to sufficiently densify it.
【０００５】[0005]
【発明の目的】本発明の目的は、前記問題点を解決し、
易焼結性で高温強度等の焼結体特性に優れた窒化珪素焼
結体を得ることができる窒化珪素粉末を提供するもので
ある。The object of the present invention is to solve the above problems,
Provided is a silicon nitride powder capable of obtaining a silicon nitride sintered body that is easily sintered and has excellent sintered body characteristics such as high temperature strength.
【０００６】[0006]
【問題点を解決するための手段】本発明者らは、窒化珪
素粉末における酸素量及び酸素の形態が、焼結性及び焼
結体特性、特に高温強度に及ぼす影響について種々検討
した結果、易焼結性で高温強度等の焼結体特性に優れた
窒化珪素焼結体を得ることができる窒化珪素粉末を見出
した。The inventors of the present invention have made various studies as to the influence of the amount of oxygen and the form of oxygen in the silicon nitride powder on the sinterability and the properties of the sintered body, especially the high temperature strength. The inventors have found a silicon nitride powder capable of obtaining a silicon nitride sintered body having excellent sinterability and excellent sintered body characteristics such as high temperature strength.
【０００７】即ち、本発明は、非晶質窒化珪素粉末及び
／又は含窒素シラン化合物の熱分解により生成する窒化
珪素粉末であって、粒子表面に水酸化物あるいは酸化物
の形態で存在する酸素量が０．２〜１．０重量％、固溶
体の形態で存在する酸素量が０．５５〜１．２重量％で
あり、かつ、固溶体の形態で存在する酸素の内、粒子表
面直下３ｎｍの範囲に存在する酸素量が０．１〜０．５
重量％、粒子表面から３ｎｍ以上内部に存在する酸素量
が０．８重量％以下であることを特徴とする窒化珪素粉
末に関するものである。That is, the present invention relates to an amorphous silicon nitride powder and / or a silicon nitride powder produced by thermal decomposition of a nitrogen-containing silane compound, wherein oxygen existing in the form of hydroxide or oxide on the particle surface. The amount of oxygen present in the form of solid solution is 0.55 to 1.2% by weight, and the amount of oxygen present in the form of solid solution is 3 nm directly below the particle surface. The amount of oxygen present in the range is 0.1 to 0.5
The present invention relates to a silicon nitride powder, characterized in that the amount of oxygen present within 3% or more from the particle surface is 0.8% by weight or less.
【０００８】本発明の窒化珪素粉末の酸素量は、粒子表
面及び粒子表面直下３ｎｍの範囲に存在している酸素量
（以下、表面酸素量という）と、粒子表面から３ｎｍ以
上内部に存在している酸素量（以下、内部酸素量とい
う）により規定される。The amount of oxygen in the silicon nitride powder of the present invention is such that the amount of oxygen existing in the surface of the particle and within the range of 3 nm immediately below the surface of the particle (hereinafter referred to as the amount of surface oxygen) and the amount of oxygen existing within 3 nm or more from the surface of the particle. It is regulated by the amount of oxygen (hereinafter referred to as the amount of internal oxygen).
【０００９】本発明における窒化珪素粉末の表面酸素量
は、０．３〜１．５重量％の範囲であり、特に、粒子表
面に水酸化物あるいは酸化物の形態で存在する酸素量が
０．２〜１．０重量％、粒子表面直下３ｎｍの範囲に存
在する酸素量が０．１〜０．５重量％の範囲である。The surface oxygen content of the silicon nitride powder in the present invention is in the range of 0.3 to 1.5% by weight, and in particular, the oxygen content present in the form of hydroxide or oxide on the surface of the particles is 0. The amount of oxygen existing in the range of 2 to 1.0% by weight and 3 nm just below the particle surface is in the range of 0.1 to 0.5% by weight.
【００１０】表面酸素量が０．３重量％未満では、焼結
時における窒化珪素粒子と焼結助剤から成る液相とのぬ
れ性が低下し、十分緻密化した焼結体を得ることが難し
くなる。表面酸素量が１．５重量％を超えると、緻密化
した焼結体を得ることはできるが、窒化珪素粉末の全酸
素量（内部酸素量と表面酸素量の和）が増加し、焼結体
における粒界相の量が増え、高温強度等の焼結体特性の
低下が起こる。If the amount of surface oxygen is less than 0.3% by weight, the wettability between the silicon nitride particles and the liquid phase composed of the sintering aid during sintering is lowered, and a sufficiently densified sintered body can be obtained. It gets harder. If the surface oxygen content exceeds 1.5% by weight, a densified sintered body can be obtained, but the total oxygen content (sum of internal oxygen content and surface oxygen content) of the silicon nitride powder increases and sintering The amount of grain boundary phase in the body increases, and the characteristics of the sintered body such as high temperature strength deteriorate.
【００１１】また、窒化珪素粉末の比表面積は、２〜２
０m2／ｇの範囲であることが好ましく、さらに、窒化珪
素粉末の比表面積をＳ（m2／ｇ）、表面酸素量をＯ（重
量％）とした場合に、Ｓ／Ｏが８〜２５の範囲であるこ
とが好ましい。一方、本発明における窒化珪素粉末の内
部酸素量は、０．８重量％以下、好ましくは０．６重量
％以下である。The specific surface area of the silicon nitride powder is 2 to 2
It is preferably in the range of 0 m 2 / g, and when the specific surface area of the silicon nitride powder is S (m 2 / g) and the amount of surface oxygen is O (wt%), S / O is 8 to 25. It is preferably in the range of. On the other hand, the internal oxygen content of the silicon nitride powder in the present invention is 0.8% by weight or less, preferably 0.6% by weight or less.
【００１２】内部酸素量が０．８重量％を超えると、窒
化珪素の焼結過程において窒化珪素粒子が焼結助剤等か
ら成る粒界相に溶解する際に粒界相の組成を変化させ、
β−柱状晶の析出と成長を阻害し、焼結体特性特に高温
強度の十分な発現が望めなくなる。When the amount of internal oxygen exceeds 0.8% by weight, the composition of the grain boundary phase is changed when the silicon nitride particles are dissolved in the grain boundary phase composed of a sintering aid or the like during the sintering process of silicon nitride. ,
This hinders the precipitation and growth of β-columnar crystals, making it impossible to expect sufficient development of the properties of the sintered body, especially high-temperature strength.
【００１３】本発明の窒化珪素粉末は、非晶質窒化珪素
粉末及び／又は含窒素シラン化合物を窒素含有不活性ガ
ス雰囲気下又は窒素含有還元性ガス雰囲気下に焼成する
に際し、非晶質窒化珪素粉末及び／又は含窒素シラン化
合物中の酸素量と焼成雰囲気中の酸素分圧を制御するこ
とにより得られる。The silicon nitride powder of the present invention is obtained by firing the amorphous silicon nitride powder and / or the nitrogen-containing silane compound in a nitrogen-containing inert gas atmosphere or a nitrogen-containing reducing gas atmosphere. It can be obtained by controlling the amount of oxygen in the powder and / or the nitrogen-containing silane compound and the oxygen partial pressure in the firing atmosphere.
【００１４】含窒素シラン化合物としては、シリコンジ
イミド、シリコンテトラアミド、シリコンニトロゲンイ
ミド、シリコンクロルイミド等が挙げられる。これら
は、公知方法、例えば、四弗化ケイ素、四塩化ケイ素、
四臭化ケイ素、四沃化ケイ素等のハロゲン化ケイ素とア
ンモニアとを気相で反応させる方法、液状の前記ハロゲ
ン化ケイ素と液体アンモニアとを反応させる方法などに
よって製造される。Examples of the nitrogen-containing silane compound include silicon diimide, silicon tetraamide, silicon nitrogen imide and silicon chlorimide. These are known methods, for example, silicon tetrafluoride, silicon tetrachloride,
It is produced by a method of reacting a silicon halide such as silicon tetrabromide or silicon tetraiodide with ammonia in a gas phase, a method of reacting the liquid silicon halide with a liquid ammonia, and the like.
【００１５】また、非晶質窒化珪素粉末は、公知方法、
例えば、前記含窒素シラン化合物を窒素又はアンモニア
ガス雰囲気下に６００〜１２００℃の範囲の温度で加熱
分解する方法、四弗化ケイ素、四塩化ケイ素、四臭化ケ
イ素、四沃化ケイ素等のハロゲン化ケイ素とアンモニア
とを高温で反応させる方法などによって製造されたもの
が挙げられる。Further, the amorphous silicon nitride powder can be obtained by a known method,
For example, a method of thermally decomposing the nitrogen-containing silane compound in a nitrogen or ammonia gas atmosphere at a temperature in the range of 600 to 1200 ° C., halogens such as silicon tetrafluoride, silicon tetrachloride, silicon tetrabromide and silicon tetraiodide. Examples include those produced by a method of reacting silicon oxide with ammonia at a high temperature.
【００１６】本発明に係る表面酸素量と内部酸素量は、
以下の方法により測定することができる。まず、窒化珪
素粉末の全酸素量Ｘ1を酸素窒素同時分析装置（ＬＥＣ
Ｏ社製ＴＣ−１３６型）により測定する。次に、窒化珪
素粉末１ｇを秤量し、１００ｍｌのイオン交換水を加え
て攪拌しながら、３時間煮沸処理する。処理液を放冷
後、開孔径０．５μｍ以下のメンブランフィルターでろ
過し、フィルター上に残った残査を６〜２４時間真空乾
燥した後、解砕し、再度、酸素窒素同時分析装置で酸素
含有量Ｘ2を測定する。処理液中のＮＨ4 +イオン濃度
は、窒化珪素粉末１ｇ当たり０．０３ｗｔ％程度であ
り、特に補正の必要はない。更に、窒化珪素粉末１ｇを
濃度５％のフッ化水素酸溶液に室温で１時間浸漬後、４
％ほう酸溶液、及び１８％塩酸を加えて５分間攪拌し、
開孔径０．５μｍ以下のメンブランフィルターを用いて
未分解残査をろ別して溶出液を得る。この一部を原子吸
光分析計にて溶出ＳｉＯ2量を求める。この場合、一部
分解する窒化珪素は、別に溶出液をアルカリ蒸留後、Ｎ
Ｈ4 +量をインドフェノール青吸光光度法により求める。
表面ＳｉＯ2量は、溶出したＳｉＯ2量より溶出ＮＨ4 +に
相当するＳｉＯ2量を差し引いた値より求め、表面酸素
量Ｘ3は、表面ＳｉＯ2量から算出する。The amount of surface oxygen and the amount of internal oxygen according to the present invention are
It can be measured by the following method. First, the total oxygen content X 1 of the silicon nitride powder was measured by an oxygen-nitrogen simultaneous analyzer (LEC
It is measured by a TC-136 type manufactured by O company). Next, 1 g of silicon nitride powder is weighed, 100 ml of ion-exchanged water is added, and the mixture is boiled for 3 hours with stirring. After allowing the treatment liquid to cool, it was filtered with a membrane filter having an opening diameter of 0.5 μm or less, the residue remaining on the filter was vacuum dried for 6 to 24 hours, then crushed, and again oxygen was analyzed with an oxygen-nitrogen simultaneous analyzer. The content X 2 is measured. The NH 4 + ion concentration in the treatment liquid is about 0.03 wt% per gram of silicon nitride powder, and no particular correction is necessary. Further, after immersing 1 g of silicon nitride powder in a hydrofluoric acid solution having a concentration of 5% at room temperature for 1 hour, 4
% Boric acid solution and 18% hydrochloric acid were added and stirred for 5 minutes,
The undecomposed residue is filtered off using a membrane filter having an opening diameter of 0.5 μm or less to obtain an eluate. A portion of this is determined by an atomic absorption spectrometer to determine the amount of eluted SiO 2 . In this case, silicon nitride that is partially decomposed is separated from the eluate by alkali distillation and then N
The amount of H 4 + is determined by the indophenol blue absorptiometry.
Surface SiO 2 amount is determined from the value obtained by subtracting the amount of SiO 2 corresponding to from elution NH 4 + eluted SiO 2 amount, the surface oxygen content X 3 is calculated from the surface SiO 2 amount.
【００１７】このようにして求めた表面酸素量が、粒子
表面直下３ｎｍ以内の範囲に存在する水酸化物、酸化
物、及び窒化珪素と酸化物との固溶体中の酸素に起因す
ることは、前記のフッ酸処理前後における粉末のＸ線光
電子スペクトルのデプス・プロファイル及び処理前後の
粉末重量変化より確認した。これより、粒子表面に水酸
化物あるいは酸化物の形態で存在する酸素量＝Ｘ1−
Ｘ2、固溶体の形態で存在する酸素量＝Ｘ2で求められ、
また、固溶体の形態で存在する酸素の内、粒子表面直下
３ｎｍの範囲に存在する酸素量＝Ｘ3−（Ｘ1−Ｘ2）、
粒子表面から３ｎｍ以上内部に存在する酸素量（内部酸
素量）＝Ｘ1−Ｘ 3で求められる。The amount of surface oxygen thus obtained is the particle size.
Hydroxide and oxidation existing within 3 nm just below the surface
And oxygen in the solid solution of silicon nitride and oxide.
That is, the X-ray light of the powder before and after the hydrofluoric acid treatment.
Electronic spectrum depth profile and before and after processing
It was confirmed from the change in powder weight. From this, the hydroxide on the particle surface
Amount of oxygen present in the form of a compound or oxide = X1−
X2, Amount of oxygen present in the form of solid solution = X2Required by
Also, of oxygen existing in the form of solid solution, directly below the particle surface
Amount of oxygen present in the range of 3 nm = X3-(X1-X2),
Amount of oxygen existing inside the particle surface of 3 nm or more (internal acid
Elementary amount) = X1-X 3Required by.
【００１８】[0018]
【実施例】以下に実施例及び比較例を示し、本発明をさ
らに具体的に説明する。 実施例１ 表１に示す各種シリコンジイミド粉末及び非晶質窒化珪
素粉末を原料として、表１に示す各種条件にて熱分解及
び焼成を行って結晶質窒化珪素粉末を製造した。得られ
た結晶質窒化珪素粉末の粉体特性を表２に示す。次に、
得られた結晶質窒化珪素粉末９３重量部に、焼結助剤と
してイットリア５重量部及びアルミナ２重量部を添加し
た配合粉を、媒体としてエタノールを用いて４８時間ボ
ールミルで湿式混合した後、減圧乾燥した。得られた混
合物を５００ｋｇ／ｃｍ2の成形圧で６×４５×７５ｍ
ｍ形状に金型成形した後、１５００ｋｇ／ｃｍ2の成形
圧でＣＩＰ成形した。得られた成形体を窒化珪素製坩堝
に入れ、窒素ガス雰囲気下１７８０℃で２時間焼結し
た。得られた焼結体を切り出し、研削後、相対密度、４
点曲げ強度を測定した。それらの結果を表３に示す。相
対密度はアルキメデス法により測定した。また、４点曲
げ強度は、島津製作所製オートグラフＧＳＳ−５００型
により測定した。EXAMPLES The present invention will be described more specifically by showing Examples and Comparative Examples below. Example 1 Using various silicon diimide powders and amorphous silicon nitride powders shown in Table 1 as raw materials, thermal decomposition and firing were performed under various conditions shown in Table 1 to produce crystalline silicon nitride powders. The powder characteristics of the obtained crystalline silicon nitride powder are shown in Table 2. next,
93 parts by weight of the obtained crystalline silicon nitride powder, 5 parts by weight of yttria and 2 parts by weight of alumina as a sintering additive were wet-mixed in a ball mill for 48 hours using ethanol as a medium, and then the pressure was reduced. Dried. The obtained mixture is 6 × 45 × 75 m under a molding pressure of 500 kg / cm 2.
After mold forming into an m-shape, CIP molding was carried out at a molding pressure of 1500 kg / cm 2 . The obtained compact was put in a silicon nitride crucible and sintered at 1780 ° C. for 2 hours in a nitrogen gas atmosphere. The obtained sintered body was cut out and ground, and then the relative density was 4
The point bending strength was measured. The results are shown in Table 3. The relative density was measured by the Archimedes method. The four-point bending strength was measured by Shimadzu Corporation Autograph GSS-500 type.
【００１９】[0019]
【表１】 [Table 1]
【００２０】[0020]
【表２】 [Table 2]
【００２１】[0021]
【表３】 [Table 3]
【００２２】[0022]
【発明の効果】本発明によれば、易焼結性で高温強度等
の焼結体特性に優れた窒化珪素焼結体を得ることができ
る窒化珪素粉末が得られる。EFFECTS OF THE INVENTION According to the present invention, a silicon nitride powder capable of obtaining a silicon nitride sintered body which is easily sintered and is excellent in sintered body characteristics such as high temperature strength can be obtained.
Claims (2)
ラン化合物の熱分解により生成する窒化珪素粉末であっ
て、粒子表面に水酸化物あるいは酸化物の形態で存在す
る酸素量が０．２〜１．０重量％、固溶体の形態で存在
する酸素量が０．５５〜１．２重量％であり、かつ、固
溶体の形態で存在する酸素の内、粒子表面直下３ｎｍの
範囲に存在する酸素量が０．１〜０．５重量％、粒子表
面から３ｎｍ以上内部に存在する酸素量が０．８重量％
以下であることを特徴とする窒化珪素粉末。1. A silicon nitride powder produced by thermal decomposition of an amorphous silicon nitride powder and / or a nitrogen-containing silane compound, wherein the amount of oxygen present in the form of hydroxide or oxide on the surface of the particle is 0.1. 2 to 1.0% by weight, the amount of oxygen present in the form of solid solution is 0.55 to 1.2% by weight, and of the oxygen present in the form of solid solution, it is present in the range of 3 nm just below the particle surface. The amount of oxygen is 0.1 to 0.5% by weight, and the amount of oxygen existing inside the particle surface of 3 nm or more is 0.8% by weight.
The following is a silicon nitride powder.
ｇであり、粒子表面に水酸化物あるいは酸化物の形態で
存在する酸素量と表面直下３ｎｍの範囲内に固溶体の形
態で存在する酸素の合計量をＯ（重量％）、比表面積を
Ｓ（m2／ｇ）とした場合に、Ｓ／Ｏが８〜２５であるこ
とを特徴とする請求項１の窒化珪素粉末。2. The specific surface area of the silicon nitride powder is 2 to 20 m 2 /
g, the total amount of oxygen existing in the form of hydroxide or oxide on the surface of the particle and the total amount of oxygen existing in the form of solid solution within 3 nm just below the surface is O (wt%), and the specific surface area is S ( The silicon nitride powder according to claim 1, wherein S / O is 8 to 25 when m 2 / g).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5122595A JP2872528B2 (en) | 1993-05-25 | 1993-05-25 | Silicon nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5122595A JP2872528B2 (en) | 1993-05-25 | 1993-05-25 | Silicon nitride powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06329404A true JPH06329404A (en) | 1994-11-29 |
| JP2872528B2 JP2872528B2 (en) | 1999-03-17 |
Family
ID=14839825
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5122595A Expired - Lifetime JP2872528B2 (en) | 1993-05-25 | 1993-05-25 | Silicon nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2872528B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5595718A (en) * | 1993-05-18 | 1997-01-21 | Ube Industries Ltd. | Process for producing a crystalline silicon nitride powder |
| WO2013146713A1 (en) | 2012-03-28 | 2013-10-03 | 宇部興産株式会社 | Silicon nitride powder production method, silicon nitride powder, silicon nitride sintered body and circuit substrate using same |
| WO2015005390A1 (en) * | 2013-07-11 | 2015-01-15 | 宇部興産株式会社 | Silicon nitride powder for mold release agent of casting mold for casting polycrystalline silicon ingot and method for manufacturing said silicon nitride powder, slurry containing said silicon nitride powder, casting mold for casting polycrystalline silicon ingot and method for manufacturing same, and method for manufacturing polycrystalline silicon ingot cast using said casting mold |
-
1993
- 1993-05-25 JP JP5122595A patent/JP2872528B2/en not_active Expired - Lifetime
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5595718A (en) * | 1993-05-18 | 1997-01-21 | Ube Industries Ltd. | Process for producing a crystalline silicon nitride powder |
| WO2013146713A1 (en) | 2012-03-28 | 2013-10-03 | 宇部興産株式会社 | Silicon nitride powder production method, silicon nitride powder, silicon nitride sintered body and circuit substrate using same |
| KR20140136002A (en) | 2012-03-28 | 2014-11-27 | 우베 고산 가부시키가이샤 | Silicon nitride powder production method, silicon nitride powder, silicon nitride sintered body and circuit substrate using same |
| CN104203813A (en) * | 2012-03-28 | 2014-12-10 | 宇部兴产株式会社 | Silicon nitride powder production method, silicon nitride powder, silicon nitride sintered body and circuit substrate using same |
| US9085462B2 (en) | 2012-03-28 | 2015-07-21 | Ube Industries, Inc. | Silicon nitride powder production method, silicon nitride powder, silicon nitride sintered body and circuit substrate using same |
| JPWO2013146713A1 (en) * | 2012-03-28 | 2015-12-14 | 宇部興産株式会社 | Method for producing silicon nitride powder, silicon nitride powder, silicon nitride sintered body, and circuit board using the same |
| WO2015005390A1 (en) * | 2013-07-11 | 2015-01-15 | 宇部興産株式会社 | Silicon nitride powder for mold release agent of casting mold for casting polycrystalline silicon ingot and method for manufacturing said silicon nitride powder, slurry containing said silicon nitride powder, casting mold for casting polycrystalline silicon ingot and method for manufacturing same, and method for manufacturing polycrystalline silicon ingot cast using said casting mold |
| JP5975176B2 (en) * | 2013-07-11 | 2016-08-23 | 宇部興産株式会社 | Silicon nitride powder for mold release agent of polycrystalline silicon ingot casting mold and manufacturing method thereof, slurry containing silicon nitride powder, casting mold for polycrystalline silicon ingot and manufacturing method thereof, and polycrystalline silicon using the mold Manufacturing method of ingot casting |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2872528B2 (en) | 1999-03-17 |
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