JPS6236965B2 - - Google Patents
Info
- Publication number
- JPS6236965B2 JPS6236965B2 JP52156389A JP15638977A JPS6236965B2 JP S6236965 B2 JPS6236965 B2 JP S6236965B2 JP 52156389 A JP52156389 A JP 52156389A JP 15638977 A JP15638977 A JP 15638977A JP S6236965 B2 JPS6236965 B2 JP S6236965B2
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- powder material
- nitride powder
- carbon
- deoxidizing
- 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.)
- Expired
Links
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 40
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 40
- 239000000463 material Substances 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 30
- 239000012535 impurity Substances 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000005452 bending Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000000516 activation analysis Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000007734 materials engineering Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- MEWCPXSDLIWQER-UHFFFAOYSA-N aluminum oxygen(2-) yttrium(3+) Chemical compound [O-2].[Y+3].[O-2].[Al+3] MEWCPXSDLIWQER-UHFFFAOYSA-N 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Description
本発明は窒化ケイ素質粉末材料に含まれている
不純物の脱酸方法に関する。窒化ケイ素質焼結体
は高温強度に優れた材料であり、ゆえに近年特に
注目を集めている。ところが市販の窒化ケイ素材
料には不純物、例えばカルシウム、鉄、マンガ
ン、ケイ素、チタン等の酸化物が含まれており、
このような原料から窒化ケイ素質焼結体を製造す
るとその焼結体は緻密ではあるが、不純物よりな
るガラス質を含んでいるため高温強度が不十分で
あつた。
この欠点を改良する方法として本発明者等は特
願昭第52−1949号において窒化アルミニウム中で
窒化ケイ素質材料を熱処理する方法を提供したが
熱処理温度が高く窒化ケイ素の粒成長の制御の点
で未だ改善の余地を残している
本発明者等は上記の点に鑑み種々検討した結
果、窒化ケイ素質粉末材料を炭素で熱処理するこ
とにより窒化ケイ素材料中の不純物、例えばカル
シウム、鉄、マンガン、ケイ素、チタン等の酸化
物（各々CaO、Fe2O3、MgO、SiO2、TiO2等）
を構成する酸素の脱酸、すなわち不純物の脱酸を
行なう方法を見出した。
したがつて本発明は窒化ケイ素粉末材料を非酸
化性雰囲気中で炭素と熱処理して窒化ケイ素質粉
末材料に含まれる不純物の脱酸方法に関するもの
であつて、高温強度に優れた窒化ケイ素質焼結体
を得るに好適な窒化ケイ素質粉末材料を提供する
ことを目的とするものである。
本発明によれば、窒化ケイ素質粉末材料を、非
酸化性雰囲気中、窒化ケイ素質粉末材料に対し
0.1〜５重量％の炭素で熱処理すると窒化ケイ素
質粉末材料に含まれる不純物の脱酸が行なわれ
る。
ここで窒化ケイ素質材料とは窒化ケイ素粉末材
料あるいは窒化ケイ素粉末材料に各種焼結助剤、
例えば酸化マグネシウム、酸化イツトリウム、酸
化イツトリウム−酸化アルミニウム、酸化ジルコ
ニウム、またはランタン系の希土類元素の酸化物
等を添加したものである。すなわち、上記脱酸の
前あるいは後に上記焼結助剤を加えるのである。
上記脱酸方法では窒化ケイ素粉末材料は市販の
ものを用いればよく、本発明に用いられる炭素と
してはカーボンブラツク、グラフアイト等が用い
られ、窒化ケイ素質粉末材料に対する使用量は
0.1〜５重量％、好ましくは0.5〜３重量％の範囲
で用いられる。0.1重量％未満では脱酸効果はな
く、５重量％を越えると炭素が残りの窒化ケイ素
と反応して炭化ケイ素となり緻密化しにくい。ま
た上記脱酸方法は非酸化性雰囲気中例えば窒素、
アルゴン、アンモニア−窒素雰囲気中で熱処理す
ることにより行なわれるが、その処理温度は1300
〜1700℃好ましくは1400〜1600℃である。1300℃
末満では脱酸の効果は少なく、1700℃を越えると
窒化ケイ素自体が分解してしまうため好ましくな
い。
脱酸処理工程は、窒化ケイ素質粉末材料の紛砕
混合工程の前に行なうことが好ましく、粉砕を要
しない場合には成形工程の前に行なう。この脱酸
工程により、窒化ケイ素質粉末材料中の不純物、
例えばSiO2、Fe2O3、TiO2等の酸化物の脱酸を行
うことができる。このようにして得られた窒化ケ
イ素質粉末材料は不純物の酸化物を構成する酸素
が脱酸されているため、不純物よりなるガラス質
は減少し、これらを用いて成形、オツトプレス焼
結すれば高温強度が優れた窒化ケイ素質焼結体を
得ることができる。
以下実施例に基づき本発明をさらに詳細に説明
する。
実施例 １
CP−85グレート窒化ケイ素質粉末材料（英国
アドバンスト・マテリアルズ・エンジニアリング
社製平均粒径：3.5μ）をアルミナ製ポツトとア
ルミナ製ボールを用い、粉砕媒体としてノルマル
ブタノールを用いて50時間粉砕した。粉砕後の平
均粒径は1.2μであり、放射化分析による酸素分
析値は3.3wt％であつた。この様にして得られた
窒化ケイ素質粉末材料と生の窒化ケイ素粉末材料
にカーボンブラツク（コロンビアンカーボン社製
Laven1000）を一定量添加し、種々の条件下窒素
雰囲気炉で熱処理し、粒径および酸素分析値を測
定した。この粉末に酸化マグネシウム5wt％また
は酸化イツトリウム（5wt％）−酸化アルミニウ
ム（2wt％）を添加し、400Kg／cm2の圧力で金型
成形して40×40×８mmの板を作り、この板の全面
を窒化ホウ素紛末で被覆した後カーボン型に入れ
一定条件下でホツトプレス焼結した。得られた焼
結体を2.5×2.5×35mmの角棒に加工して抗折試験
を行ない抗折強度を測定した。試験条件はクロス
ヘツドスピード0.5mm／min、スパン20mm、温度
は1200℃であつた。結果を第１表に示す。また炭
素処理しないものを同一の条件で比較例として行
なつた場合の結果を第１表に併せて示す。
実施例 ２
CP−85グレードの窒化ケイ素粉末材料をアル
ミナ製ポツトとボールを用い、粉砕媒体としてノ
ルマルブタノールを用いて50時間粉砕した。粉砕
後の粒径は1.3μであり、また酸素分析値は2.9％
であつた。この粉砕した窒化ケイ素粉末材料に対
し、1.0wt％のカーボンブラツク（コロンビア
ン・カーボン製Laven1000）を添加、均一混合し
て、1550℃の窒素雰囲気炉で１時間処理した。処
理後の粒径は1.5μ、酸素分析値は1.2％であつ
た。この粉末に5wt％の酸化イツトリウムと2wt
％の酸化アルミニウムを添加し、400Kg／cm2の圧
力で金型成形して50×50×20mmの板を作り、この
板の全面を窒化ホウ素粉末で被覆した後カーボン
型に入れ1800℃、500Kg／cm2で２時間ホツトプレ
ス焼結した。この焼結体を切断切削加工して2.5
×2.5×50mmの角棒にして抗折試験を行ない抗折
強度を測定した。抗折試験条件はクロスヘツドス
ピード0.5mm／min、スパン20mm、温度は常温、
800℃、1000℃、1200℃で行なつた。また比較例
として上記窒化ケイ素粉末材料を炭素で熱処理を
しない以外はすべて同一の条件で行なつた。両方
の結果を第２表に示す。各温度での測定はすべて
５回行ない、表中の値はその平均値で示した。
The present invention relates to a method for deoxidizing impurities contained in a silicon nitride powder material. Silicon nitride sintered bodies are materials with excellent high-temperature strength, and therefore have attracted particular attention in recent years. However, commercially available silicon nitride materials contain impurities such as oxides of calcium, iron, manganese, silicon, titanium, etc.
When a silicon nitride sintered body is manufactured from such raw materials, the sintered body is dense, but has insufficient high-temperature strength because it contains vitreous impurities. As a method to improve this drawback, the present inventors proposed a method of heat-treating a silicon nitride material in aluminum nitride in Japanese Patent Application No. 52-1949, but the heat treatment temperature is high and it is difficult to control the grain growth of silicon nitride. As a result of various studies in view of the above points, the inventors of the present invention have found that impurities in the silicon nitride material, such as calcium, iron, manganese, etc. can be removed by heat-treating the silicon nitride powder material with carbon. Oxides of silicon, titanium, etc. (CaO, Fe 2 O 3 , MgO, SiO 2 , TiO 2 , etc.)
We have discovered a method for deoxidizing the oxygen constituting the molecule, that is, deoxidizing the impurities. Therefore, the present invention relates to a method for deoxidizing impurities contained in a silicon nitride powder material by heat treating the silicon nitride powder material with carbon in a non-oxidizing atmosphere. The object of the present invention is to provide a silicon nitride powder material suitable for obtaining a compact. According to the present invention, a silicon nitride powder material is mixed with a silicon nitride powder material in a non-oxidizing atmosphere.
Heat treatment with 0.1 to 5% by weight of carbon deoxidizes impurities contained in the silicon nitride powder material. Here, silicon nitride material refers to silicon nitride powder material or silicon nitride powder material with various sintering aids.
For example, magnesium oxide, yttrium oxide, yttrium oxide-aluminum oxide, zirconium oxide, or lanthanum-based rare earth element oxides are added. That is, the sintering aid is added before or after the deoxidation. In the above deoxidizing method, a commercially available silicon nitride powder material may be used. Carbon black, graphite, etc. are used as the carbon used in the present invention, and the amount used relative to the silicon nitride powder material is
It is used in a range of 0.1 to 5% by weight, preferably 0.5 to 3% by weight. If it is less than 0.1% by weight, there is no deoxidizing effect, and if it exceeds 5% by weight, carbon reacts with the remaining silicon nitride to form silicon carbide, making it difficult to densify. In addition, the above deoxidizing method uses nitrogen, for example, in a non-oxidizing atmosphere.
This is done by heat treatment in an argon, ammonia-nitrogen atmosphere, and the treatment temperature is 1300
-1700°C, preferably 1400-1600°C. 1300℃
At lower temperatures, the deoxidizing effect is less, and if the temperature exceeds 1700°C, the silicon nitride itself will decompose, which is not preferable. The deoxidizing process is preferably carried out before the pulverizing and mixing process of the silicon nitride powder material, and if pulverizing is not required, it is carried out before the molding process. This deoxidation process removes impurities in the silicon nitride powder material.
For example, oxides such as SiO 2 , Fe 2 O 3 and TiO 2 can be deoxidized. In the silicon nitride powder material obtained in this way, the oxygen constituting the impurity oxide has been deoxidized, so the glassy content of the impurity is reduced. A silicon nitride sintered body with excellent strength can be obtained. The present invention will be explained in more detail below based on Examples. Example 1 CP-85 grade silicon nitride powder material (manufactured by Advanced Materials Engineering, UK, average particle size: 3.5μ) was crushed for 50 hours using an alumina pot and an alumina ball, and normal butanol as the grinding medium. Shattered. The average particle size after pulverization was 1.2μ, and the oxygen analysis value by activation analysis was 3.3wt%. Carbon black (manufactured by Columbia Carbon Co., Ltd.) was added to the silicon nitride powder material obtained in this way and the raw silicon nitride powder material.
Laven 1000) was added in a certain amount, heat treated in a nitrogen atmosphere furnace under various conditions, and the particle size and oxygen analysis values were measured. Add 5wt% of magnesium oxide or yttrium oxide (5wt%)-aluminum oxide (2wt%) to this powder, mold it with a pressure of 400Kg/ cm2 to make a 40 x 40 x 8 mm plate, and make a plate of 40 x 40 x 8 mm. After the entire surface was coated with boron nitride powder, it was placed in a carbon mold and hot press sintered under certain conditions. The obtained sintered body was processed into a square bar of 2.5 x 2.5 x 35 mm, and a bending test was conducted to measure the bending strength. The test conditions were a crosshead speed of 0.5 mm/min, a span of 20 mm, and a temperature of 1200°C. The results are shown in Table 1. In addition, Table 1 also shows the results obtained when a sample without carbon treatment was carried out under the same conditions as a comparative example. Example 2 A CP-85 grade silicon nitride powder material was ground using an alumina pot and ball for 50 hours using n-butanol as the grinding media. The particle size after crushing is 1.3μ, and the oxygen analysis value is 2.9%.
It was hot. To this pulverized silicon nitride powder material, 1.0 wt % of carbon black (Laven 1000 manufactured by Columbia Carbon) was added, mixed uniformly, and treated in a nitrogen atmosphere furnace at 1550° C. for 1 hour. The particle size after treatment was 1.5μ, and the oxygen analysis value was 1.2%. This powder contains 5wt% yttrium oxide and 2wt%
% of aluminum oxide and molded with a pressure of 400Kg/cm 2 to make a 50 x 50 x 20mm plate. After coating the entire surface of this plate with boron nitride powder, it was placed in a carbon mold at 1800℃, 500Kg Hot press sintering was carried out at /cm 2 for 2 hours. This sintered body is cut and processed to yield 2.5
A bending test was conducted using a square bar of 2.5 x 50 mm to measure the bending strength. The bending test conditions were a crosshead speed of 0.5 mm/min, a span of 20 mm, and a temperature of room temperature.
It was conducted at 800℃, 1000℃, and 1200℃. As a comparative example, the silicon nitride powder material was treated under the same conditions except that it was not heat treated with carbon. Both results are shown in Table 2. All measurements at each temperature were performed five times, and the values in the table are the average values.
【表】【table】
【表】
実施例 ３
CP−85グレード窒化ケイ素質粉末材料（英国
アドバンスト・マテリアルズ・エンジニアリング
社製平均粒径：3.5μ）をアルミナ製ポツトとア
ルミナ製ボールを用い、粉砕媒体としてノルマル
ブタノールを用いて50時間粉砕した。粉砕後の平
均粒径は1.2μであり、放射化分析による酸素分
析値は2.5wt％であつた。この用にして得られた
窒化ケイ素質材料と生の窒化ケイ素材料にカーボ
ンブラツク（コロンビアンカーボン社製
Laven1000）を0.5％添加し、種々の条件下窒化
雰囲気で熱処理し、粒径および酸素分析値を測定
した。この結果を第３表に示す。[Table] Example 3 CP-85 grade silicon nitride powder material (manufactured by Advanced Materials Engineering, UK, average particle size: 3.5μ) was crushed using an alumina pot and an alumina ball, and normal butanol was used as the grinding medium. The mixture was ground for 50 hours. The average particle size after pulverization was 1.2μ, and the oxygen analysis value by activation analysis was 2.5wt%. Carbon black (manufactured by Columbia Carbon Co., Ltd.) was added to the silicon nitride material obtained for this purpose and the raw silicon nitride material.
Laven 1000) was added at 0.5%, heat treated in a nitriding atmosphere under various conditions, and the particle size and oxygen analysis values were measured. The results are shown in Table 3.
【表】【table】
【表】
第３表において1800℃×1Hの熱処理を行つた
場合は、窒化ケイ素の分解が起こり測定困難であ
つた。
上記結果より明らかなように熱処理温度があま
り低い場合は脱酸の効果が少なく、あまり高い場
合は窒化ケイ素が分解してしまう。
以上の実施例から明らかな様に炭素で処理した
窒化ケイ素質粉末材料は、不純物の酸化物を構成
する酸素が脱酸されているため、不純物よりなる
ガラス質は減少し。これにより得られた焼結体は
高温強度が優れていることがわかる。[Table] In Table 3, when heat treatment was performed at 1800°C for 1 hour, silicon nitride decomposed and measurement was difficult. As is clear from the above results, if the heat treatment temperature is too low, the deoxidizing effect will be small, and if it is too high, silicon nitride will decompose. As is clear from the above examples, in the silicon nitride powder material treated with carbon, the oxygen constituting the impurity oxide is deoxidized, so the glassiness made of the impurity is reduced. It can be seen that the sintered body thus obtained has excellent high-temperature strength.
Claims (1)
素を添加し、非酸化性雰囲気中1300〜1700℃で熱
処理することを特徴とする窒化ケイ素質粉末材料
に含まれる不純物の脱酸方法。 ２ 不純物の脱酸は、カルシウム、鉄、マンガ
ン、ケイ素、チタンの酸化物を構成する酸素の脱
酸である特許請求の範囲第１項に記載の窒化ケイ
素質粉末材料に含まれる不純物の脱酸方法。[Claims] 1. Impurities contained in a silicon nitride powder material, which is characterized in that 0.1 to 5% by weight of carbon is added to the silicon nitride powder material and heat treated at 1300 to 1700°C in a non-oxidizing atmosphere. deoxidation method. 2. The deoxidation of impurities contained in the silicon nitride powder material according to claim 1 is deoxidation of oxygen constituting oxides of calcium, iron, manganese, silicon, and titanium. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15638977A JPS5488913A (en) | 1977-12-27 | 1977-12-27 | Deoxidation of impurity contained in silicon nitride based material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15638977A JPS5488913A (en) | 1977-12-27 | 1977-12-27 | Deoxidation of impurity contained in silicon nitride based material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5488913A JPS5488913A (en) | 1979-07-14 |
| JPS6236965B2 true JPS6236965B2 (en) | 1987-08-10 |
Family
ID=15626666
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15638977A Granted JPS5488913A (en) | 1977-12-27 | 1977-12-27 | Deoxidation of impurity contained in silicon nitride based material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5488913A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01226768A (en) * | 1988-03-07 | 1989-09-11 | Toshiba Ceramics Co Ltd | Manufacture of silicon nitride sintered compact |
| JP6720053B2 (en) * | 2016-11-04 | 2020-07-08 | 株式会社Maruwa | Method for manufacturing silicon nitride sintered body |
-
1977
- 1977-12-27 JP JP15638977A patent/JPS5488913A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5488913A (en) | 1979-07-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4908171A (en) | Method of sintering articles of silicon nitride | |
| EP0540642B1 (en) | Preparing alpha-phase silicon nitride, converting to beta-phase | |
| EP0540671B1 (en) | Preparing silicon nitride with densification aid, and results | |
| JPS6236965B2 (en) | ||
| US4801414A (en) | Production of silicon nitride sintered body | |
| JP2649220B2 (en) | Silicon nitride / silicon carbide composite powder, composite compact, method for producing them, and method for producing silicon nitride / silicon carbide composite sintered body | |
| JP2786719B2 (en) | Method for producing rare earth oxide sintered body | |
| JPH0699192B2 (en) | Manufacturing method of high toughness silicon nitride sintered body | |
| JP2531871B2 (en) | Method for manufacturing high-density boron nitride pressureless sintered body | |
| JPH0532405A (en) | Silicon nitride powder, method for producing silicon nitride powder, and silicon nitride sintered body | |
| JP2671535B2 (en) | Method of treating silicon nitride powder | |
| JP2944787B2 (en) | SiC-based oxide sintered body and method for producing the same | |
| JPH06263410A (en) | Method for increasing beta-fraction of powdery silicon nitride | |
| JPH0712980B2 (en) | Silicon carbide sintered body and method for producing the same | |
| JPH0520387B2 (en) | ||
| JP2573720B2 (en) | Manufacturing method of silicon nitride sintered body | |
| JPH03261659A (en) | Black sintered zirconia-based ceramics and production thereof | |
| JP2661743B2 (en) | Method for producing silicon nitride ingot and silicon nitride powder | |
| JPH02307871A (en) | Production of ceramic sintered compact | |
| JPH0442862A (en) | Preparation of aln sintered product | |
| JPH0579625B2 (en) | ||
| JPH0511064B2 (en) | ||
| JPH02157112A (en) | Production of silicon nitride raw powder | |
| JPS6038351B2 (en) | Manufacturing method of high-strength silicon nitride sintered body | |
| JPH05221617A (en) | Method for producing silicon nitride powder |