JPH11139882A - Composite silicon nitride powder and its production - Google Patents
Composite silicon nitride powder and its productionInfo
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- JPH11139882A JPH11139882A JP9303853A JP30385397A JPH11139882A JP H11139882 A JPH11139882 A JP H11139882A JP 9303853 A JP9303853 A JP 9303853A JP 30385397 A JP30385397 A JP 30385397A JP H11139882 A JPH11139882 A JP H11139882A
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- silicon nitride
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、自動車部品や耐摩
耗工具等に使用される構造用セラミックス材料として、
室温から１１００℃の中低温域で強度等の優れた機械的
性質を有する窒化ケイ素焼結体の原料粉末、及びその製
造方法に関するものである。The present invention relates to a structural ceramic material used for automobile parts, wear-resistant tools and the like.
The present invention relates to a raw material powder of a silicon nitride sintered body having excellent mechanical properties such as strength in a medium to low temperature range from room temperature to 1100 ° C., and a method for producing the same.
【０００２】[0002]
【従来の技術】窒化ケイ素（Ｓｉ3Ｎ4）は、強度、破壊
靭性値、耐食性、耐摩耗性、耐熱衝撃性、耐酸化性等に
おいてバランスの取れた材料であるため、切削工具から
エンジン部品等の広い範囲で利用されている。特に最近
では、自動車エンジンやガスタービン等の構造用材料と
して注目を集めている。2. Description of the Related Art Silicon nitride (Si 3 N 4 ) is a material that is balanced in strength, fracture toughness, corrosion resistance, abrasion resistance, thermal shock resistance, oxidation resistance, and the like. Etc. are used in a wide range. In particular, recently, it has attracted attention as a structural material for automobile engines and gas turbines.
【０００３】この様な窒化ケイ素の強度を向上させる方
法として、従来から微細な窒化ケイ素の粒子からなる焼
結体の作製が試みられている。例えば、特開平６−２７
１３５８号公報には、窒化ケイ素の平均粒径を０.３μ
ｍ程度まで微細化することにより、３点曲げ強度が１７
０ｋｇ／ｍｍ2以上の窒化ケイ素焼結体が得られると記
載されている。しかしながら、同公報記載の実施例でも
明らかなように、市販のＳｉ3Ｎ4原料粉末の平均粒径は
０.７μｍ程度であるから、上記のごとく微細な窒化ケ
イ素焼結体を得るためには、この市販の原料粉末の平均
粒径を更に微細にする必要がある。[0003] As a method for improving the strength of such silicon nitride, the production of a sintered body composed of fine silicon nitride particles has been conventionally attempted. For example, JP-A-6-27
No. 1358 discloses that the average particle size of silicon nitride is 0.3 μm.
m, the three-point bending strength is 17
It is described that a silicon nitride sintered body of 0 kg / mm 2 or more can be obtained. However, as is clear from the examples described in the publication, the average particle size of the commercially available Si 3 N 4 raw material powder is about 0.7 μm. It is necessary to further reduce the average particle size of this commercially available raw material powder.
【０００４】微細な粉末を得る方法としては、従来から
ＣＶＤ法が用いられており、例えばＣｅｒａｍｉｃ Ｍ
ａｔｅｒｉａｌｓ ＆ Ｃｏｍｐｏｎｅｎｔｓ ｆｏｒ Ｅ
ｎｇｉｎｅｓ のＰ.７０、ｔａｂｌｅ II に示されてい
るように、平均粒径が２０ｎｍ程度窒化ケイ素粉末が得
られている。しかしながら、ＣＶＤ法は気相法による合
成法のため、製造コストが高く、また量産性に乏しいと
いう欠点がある。しかも、粉末の粒径が小さくなるにつ
れて表面積が増加するため、表面酸化により窒化ケイ素
粉末としての特性が損なわれたり、また粉末同士の凝集
が激しくなり、成形性が極端に低下するなどの問題点が
あった。[0004] As a method for obtaining fine powder, a CVD method has been conventionally used. For example, Ceramic M
materials & Components for E
As shown in P.70, table II of Nines, a silicon nitride powder having an average particle size of about 20 nm was obtained. However, the CVD method is disadvantageous in that the production cost is high and the mass productivity is poor because it is a synthesis method by a gas phase method. Moreover, since the surface area increases as the particle size of the powder becomes smaller, the properties of the silicon nitride powder are impaired due to surface oxidation, and the powders become more agglomerated, resulting in extremely low moldability. was there.
【０００５】一方、量産性に優れた微細粉末の合成方法
として、粉砕法がある。例えば、窒化ケイ素と金属チタ
ンを高加速度で混合することにより、窒化ケイ素とチタ
ンのナノ複合粉末を合成する方法が知られている。しか
しながら、このようなナノ複合粉末を用いても、焼結時
の加熱により結晶粒が粗大化する現象が避けられず、微
細な窒化ケイ素焼結体を得ることは困難であった。On the other hand, there is a pulverization method as a method for synthesizing a fine powder excellent in mass productivity. For example, a method of synthesizing a nanocomposite powder of silicon nitride and titanium by mixing silicon nitride and titanium metal at high acceleration is known. However, even when such a nanocomposite powder is used, a phenomenon that crystal grains become coarse due to heating during sintering is inevitable, and it has been difficult to obtain a fine silicon nitride sintered body.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、このような
従来の事情に鑑み、中低温域で強度等の優れた特性を有
する窒化ケイ素焼結体の原料粉末として、生産が比較的
容易で、焼結時における結晶粒成長を抑制することがで
きる微細粒子からなる窒化ケイ素粉末、及びその製造方
法を提供することを目的とする。SUMMARY OF THE INVENTION In view of the above-mentioned circumstances, the present invention is relatively easy to produce as a raw material powder of a silicon nitride sintered body having excellent properties such as strength in a low temperature range. It is another object of the present invention to provide a silicon nitride powder composed of fine particles capable of suppressing crystal grain growth during sintering, and a method for producing the same.
【０００７】[0007]
【課題を解決するための手段】上記目的を達成するた
め、本発明は、平均粒径が１００ｎｍ以下の窒化ケイ素
粒子と窒化チタン粒子とから構成された平均直径が１μ
ｍ以上である窒化ケイ素複合粉末を提供するものであ
る。In order to achieve the above-mentioned object, the present invention relates to a method for producing a silicon nitride particle having an average particle diameter of 100 nm or less and a titanium nitride particle having an average diameter of 1 μm.
m or more.
【０００８】また、本発明における上記窒化ケイ素複合
粉末の製造方法は、窒素雰囲気中において窒化ケイ素粉
末と金属チタン粉末とを１０〜２００Ｇの加速度で混合
することを特徴とする。また、この本発明方法において
は、金属チタン粉末の添加量を全体の１０〜５０重量％
とすること、及び混合時間を０.１時間〜１０時間とす
ることが好ましい。The method for producing a silicon nitride composite powder according to the present invention is characterized in that the silicon nitride powder and the metal titanium powder are mixed at an acceleration of 10 to 200 G in a nitrogen atmosphere. In the method of the present invention, the addition amount of the metallic titanium powder is 10 to 50% by weight of the whole.
And the mixing time is preferably from 0.1 hour to 10 hours.
【０００９】[0009]
【発明の実施の形態】本発明の窒化ケイ素複合粉末で
は、平均粒径１００ｎｍ以下の微細なＳｉ3Ｎ4粒子の界
面にＴｉＮ粒子が配置されているため、焼結中にＴｉＮ
粒子が微細なＳｉ3Ｎ4粒子をピン止めしてＳｉ3Ｎ4の粒
成長を抑制することができ、微細な結晶構造で高強度の
窒化ケイ素焼結体を得ることが可能となる。BEST MODE FOR CARRYING OUT THE INVENTION In the silicon nitride composite powder of the present invention, TiN particles are arranged at the interface of fine Si 3 N 4 particles having an average particle diameter of 100 nm or less.
The fine particles of Si 3 N 4 can be pinned to suppress the growth of Si 3 N 4 grains, and a high-strength silicon nitride sintered body having a fine crystal structure can be obtained.
【００１０】また、微細なＳｉ3Ｎ4粒子とＴｉＮ粒子が
互いに接して複合粉末を形成しているので、Ｓｉ3Ｎ4粒
子が微細であるにも拘らず表面酸化が抑制される。しか
も、この窒化ケイ素複合粉末の平均直径は１μｍ以上と
比較的大きいので、粉末同士の凝集が抑制され、粉末の
成形性にも優れている。[0010] Further, since the fine Si 3 N 4 particles and the TiN particles are in contact with each other to form a composite powder, the surface oxidation is suppressed despite the fine Si 3 N 4 particles. In addition, since the average diameter of the silicon nitride composite powder is relatively large, 1 μm or more, aggregation of the powders is suppressed, and the powder has excellent moldability.
【００１１】上記本発明の窒化ケイ素複合粉末は、Ｓｉ
3Ｎ4粉末と金属Ｔｉ粉末とを窒素雰囲気中にて１０〜２
００Ｇの高加速度で混合することにより、製造すること
ができる。かかる方法によって微粒な窒化ケイ素粒子と
ＴｉＮ粒子の複合粉末が生成する理由は明らかではない
が、混合中に金属Ｔｉが雰囲気ガスの窒素と反応して窒
化チタンが生成し、このＴｉＮ粒子が粉砕されたＳｉ3
Ｎ4粒子の界面に分散するためと考えられる。[0011] The silicon nitride composite powder of the present invention comprises Si
3 N 4 powder and metal Ti powder are mixed in a nitrogen atmosphere for 10 to 2
It can be manufactured by mixing at a high acceleration of 00G. It is not clear why such a method produces a composite powder of fine silicon nitride particles and TiN particles, but during mixing, metal Ti reacts with nitrogen in the atmosphere gas to produce titanium nitride, and the TiN particles are pulverized. Si 3
This is considered to be due to dispersion at the interface of N 4 particles.
【００１２】Ｓｉ3Ｎ4粉末と金属Ｔｉ粉末の混合時の加
速度を１０〜２００Ｇの範囲に限定する理由は、加速度
が１０Ｇ未満ではＴｉと窒素ガスの反応が起こらず、Ｔ
ｉＮ粒子が生成せずに金属Ｔｉが残留ため、また逆に加
速度が２００Ｇを越えるとＳｉ3Ｎ4とＴｉとが反応を開
始し、ＴｉＳｉ2やＴｉ5Ｓｉ3等のＴｉとＳｉの化合物
が生成するため、いずれの場合も得られるＳｉ3Ｎ4焼結
体の強度が劣化するからである。The reason why the acceleration when mixing the Si 3 N 4 powder and the metal Ti powder is limited to the range of 10 to 200 G is that if the acceleration is less than 10 G, the reaction between Ti and nitrogen gas does not occur,
Since metal Ti remains without generating iN particles, and conversely, when the acceleration exceeds 200 G, a reaction between Si 3 N 4 and Ti starts, and a compound of Ti and Si such as TiSi 2 or Ti 5 Si 3 is formed. This is because, in each case, the strength of the obtained Si 3 N 4 sintered body is deteriorated.
【００１３】添加する金属Ｔｉ粉末の量については特に
制限はないが、Ｓｉ3Ｎ4粉末に対して１０重量％未満で
は生成するＴｉＮの量が少なくなり、焼結時にＳｉ3Ｎ4
の粒成長が発生しやすい。また、５０重量％を越える
と、雰囲気の窒素と反応せず残留するＴｉの量が多くな
る。その結果、いずれの場合もＳｉ3Ｎ4焼結体の強度等
の特性の劣化を招くので、金属Ｔｉ粉末の添加量は１０
〜５０重量％の範囲が好ましい。The amount of the metal Ti powder to be added is not particularly limited, but if it is less than 10% by weight with respect to the Si 3 N 4 powder, the amount of generated TiN will be small, and the Si 3 N 4 during sintering will be reduced.
Grains easily grow. If it exceeds 50% by weight, the amount of Ti remaining without reacting with nitrogen in the atmosphere increases. As a result, in any case, the properties such as the strength of the Si 3 N 4 sintered body are deteriorated.
The range of ５０50% by weight is preferred.
【００１４】また、Ｓｉ3Ｎ4粉末と金属Ｔｉ粉末の混合
時間については特に制限は無い。しかし、混合時間が
０.１時間未満ではＴｉと雰囲気の窒素との反応が少な
く、また１０時間を越えると粉砕メディア及びポット内
壁からの不純物の混入が顕著になるため、０.１〜１０
時間程度とすることが望ましい。The mixing time of the Si 3 N 4 powder and the metal Ti powder is not particularly limited. However, if the mixing time is less than 0.1 hour, the reaction between Ti and nitrogen in the atmosphere is small, and if the mixing time is more than 10 hours, impurities from the pulverizing media and the inner wall of the pot become conspicuous.
It is desirable to set it to about time.
【００１５】本発明の窒化ケイ素複合粉末を用いて製造
した窒化ケイ素焼結体は、Ｓｉ3Ｎ4の粒成長が抑制され
て微細な結晶構造を有しており、結晶室温から１１００
℃までの中低温域での強度に優れている。The silicon nitride sintered body produced by using the silicon nitride composite powder of the present invention has a fine crystal structure in which grain growth of Si 3 N 4 is suppressed,
Excellent strength in middle to low temperature range up to ° C.
【００１６】[0016]
【実施例】実施例１ 市販の平均粒径０.５μｍのＳｉ3Ｎ4粉末に、焼結助剤
としてＡｌ2Ｏ3を２重量％、ＭｇＯを１重量％、及びＹ
2Ｏ3を５重量％加え、更に平均粒径５μｍの金属Ｔｉ粉
末を全体の３０重量％添加して、ＳＵＳ３０４製ボール
とポットを用いた遊星ボールミルにより、窒素雰囲気中
にて１５０Ｇの加速度で４時間の混合を実施した。 EXAMPLE 1 Commercially available Si 3 N 4 powder having an average particle size of 0.5 μm was mixed with 2% by weight of Al 2 O 3 , 1% by weight of MgO, and Y as a sintering aid.
5% by weight of 2 O 3 and 30% by weight of a metal Ti powder having an average particle size of 5 μm were added. Time mixing was performed.
【００１７】得られた粉末はＳｉ3Ｎ4粒子とＴｉＮ粒子
の複合粉末であり、その内部をＴＥＭで観察した結果、
Ｓｉ3Ｎ4粒子及び助剤の平均粒径は共に２０ｎｍまで、
ＴｉＮ粒子の平均粒径は１０ｎｍまでそれぞれ微粒化し
ていた。次に、この複合粉末を室温で２００ｋｇ／ｍｍ
2の条件で大気中にてプレス成形を行った。その成形体
を、窒素１気圧下において１５００℃で１時間の焼結を
行いＳｉ3Ｎ4焼結体を得た。The obtained powder is a composite powder of Si 3 N 4 particles and TiN particles.
The average particle size of both the Si 3 N 4 particles and the auxiliary is up to 20 nm,
The average particle size of the TiN particles was reduced to 10 nm. Next, this composite powder was added at room temperature to 200 kg / mm.
Press molding was performed in the atmosphere under the conditions of 2 . The compact was sintered at 1500 ° C. for 1 hour under 1 atm of nitrogen to obtain a Si 3 N 4 sintered body.
【００１８】得られたＳｉ3Ｎ4焼結体を３×４×４０ｍ
ｍ相当の抗析試験片に切り出し、＃８００ダイヤモンド
砥石により切削加工仕上げをした後、ＪＩＳ Ｒ１６０
１に準拠して１５本の試験片について３点曲げ強度を測
定した。また、このＳｉ3Ｎ4焼結体を研磨した後、Ａｒ
イオンエッチングで薄膜試験片を作製し、透過型電子顕
微鏡を用いて母相のＳｉ3Ｎ4粒子及び分散粒子であるＴ
ｉＮの粒径をそれぞれ評価した。その結果、Ｓｉ3Ｎ4粒
子の平均粒径は５０ｎｍ及びＴｉＮ粒子の平均粒径は３
０ｎｍと非常に微細であり、また焼結体の平均強度は２
ＧＰａと非常に高強度であった。The obtained Si 3 N 4 sintered body is 3 × 4 × 40 m
m, which is cut out into an eutectoid test specimen equivalent to m, and cut and finished with a # 800 diamond grindstone.
The three-point bending strength of 15 test pieces was measured according to 1. After polishing the Si 3 N 4 sintered body, Ar 3
A thin film test piece was prepared by ion etching, and the matrix Si 3 N 4 particles and the dispersed particles T
Each particle size of iN was evaluated. As a result, the average particle diameter of the Si 3 N 4 particles was 50 nm and the average particle diameter of the TiN particles was 3 nm.
0 nm, and the average strength of the sintered body is 2
GPa and very high strength.
【００１９】一方、比較例として、金属Ｔｉ粉末を加え
ない以外は上記と同様にして、１２時間の混合を行い、
平均粒径２０ｎｍのＳｉ3Ｎ4粒子と助剤のみからなる複
合粉末を作製した。この複合粉末を上記と同一条件で成
形及び焼結したところ、得られたＳｉ3Ｎ4焼結体中のＳ
ｉ3Ｎ4粒子は２００ｎｍまで粒成長し、また焼結体の強
度は１００ｋｇ／ｍｍ2と低強度であった。On the other hand, as a comparative example, mixing was performed for 12 hours in the same manner as above except that no metal Ti powder was added.
A composite powder comprising only Si 3 N 4 particles having an average particle diameter of 20 nm and an auxiliary agent was prepared. When this composite powder was molded and sintered under the same conditions as above, the S 3 N 4
The i 3 N 4 particles grew to 200 nm, and the strength of the sintered body was as low as 100 kg / mm 2 .
【００２０】実施例２ 平均粒径０.５μｍのＳｉ3Ｎ4粉末に、実施例１と同一
の焼結助剤を加え、更に平均粒径５μｍの金属Ｔｉ粉末
を全体の５〜６０重量％添加して、ＺｒＯ2製ボールと
ＳＵＳ製ポットを用いた遊星ボールミルにより、窒素雰
囲気中において５〜２５０Ｇの加速度で混合した。下記
表１に、金属Ｔｉ粉末の添加量、混合時の雰囲気、加速
度、及び混合時間をまとめて示した。 Example 2 The same sintering aid as in Example 1 was added to Si 3 N 4 powder having an average particle size of 0.5 μm, and a metal Ti powder having an average particle size of 5 μm was 5 to 60% by weight of the whole. The mixture was added and mixed by a planetary ball mill using a ZrO 2 ball and a SUS pot at an acceleration of 5 to 250 G in a nitrogen atmosphere. Table 1 below summarizes the amount of metal Ti powder added, the atmosphere during mixing, the acceleration, and the mixing time.
【００２１】[0021]
【表１】 （注）表中の＊を付した試料は比較例である。[Table 1] (Note) Samples marked with * in the table are comparative examples.
【００２２】得られた各複合粉末について、実施例１と
同様にＳｉ3Ｎ4粒子の平均粒径を求めると共に、粉末中
に含まれる不純物のＺｒＯ2濃度及び及び残留Ｔｉ量を
ＩＣＰ法により測定し、それぞれ下記表２に示した。ま
た、各複合粉末を用いて実施例１と同様に製造したＳｉ
3Ｎ4焼結体について、実施例１と同様に測定した焼結体
の強度を表２に併せて示した。For each of the obtained composite powders, the average particle diameter of Si 3 N 4 particles was determined in the same manner as in Example 1, and the ZrO 2 concentration of impurities contained in the powder and the residual Ti amount were measured by the ICP method. The results are shown in Table 2 below. In addition, Si was manufactured in the same manner as in Example 1 using each composite powder.
Table 2 also shows the strength of the 3 N 4 sintered body measured in the same manner as in Example 1.
【００２３】[0023]
【表２】 （注）表中の＊を付した試料は比較例である。[Table 2] (Note) Samples marked with * in the table are comparative examples.
【００２４】上記の結果から分かるように、アルゴン雰
囲気中で混合した試料１、及び低加速度で混合した試料
３は共に、窒素と反応せずに複合粉末中に残留したＴｉ
濃度が非常に大きいため、焼結体強度が著しく低下して
いる。また、試料６は混合加速度が大き過ぎるため、ボ
ールに由来する不純物のＺｒＯ2濃度が高くなると共
に、混合中にＳｉ3Ｎ4と金属Ｔｉが反応してＴｉＳｉ2
が生成し、焼結体強度が非常に低くなっている。As can be seen from the above results, both the sample 1 mixed in an argon atmosphere and the sample 3 mixed at a low acceleration did not react with nitrogen and remained in the composite powder.
Since the concentration is very large, the strength of the sintered body is significantly reduced. In sample 6, since the mixing acceleration is too large, the ZrO 2 concentration of the impurities derived from the ball becomes high, and Si 3 N 4 reacts with metal Ti during mixing to make TiSi 2.
Are generated, and the strength of the sintered body is very low.
【００２５】一方、その他の本発明の各試料では、複合
粉末中のＳｉ3Ｎ4粒子の平均粒径が小さく、且つ残留Ｔ
ｉ濃度及びＺｒＯ2濃度も低く、その結果非常に高い強
度のＳｉ3Ｎ4焼結体が得られることが分かる。ただし、
試料７は添加Ｔｉ量が少ないため、複合粉末中のＴｉＮ
量が少なくなり、焼結時の粒成長が大きくなり、焼結体
強度が若干低下している。試料９は添加Ｔｉ量が多いた
め、及び試料１０は混合時間が短いため、それぞれ複合
粉末中にＴｉが残留し、焼結体の強度が若干低下してい
る。また、試料１２は混合時間が長いため、不純物のＺ
ｒＯ2が増え、焼結体の強度が若干低下している。On the other hand, in each of the other samples of the present invention, the average particle size of the Si 3 N 4 particles in the composite powder is small, and the residual T
It is understood that the i concentration and the ZrO 2 concentration are also low, and as a result, a Si 3 N 4 sintered body having extremely high strength can be obtained. However,
In Sample 7, the amount of Ti added was small, so that TiN
The amount is small, the grain growth during sintering is large, and the strength of the sintered body is slightly reduced. Sample 9 has a large amount of added Ti, and sample 10 has a short mixing time, so that Ti remains in the composite powder and the strength of the sintered body is slightly reduced. Since the mixing time of the sample 12 is long, the impurity Z
rO 2 is increased, and the strength of the sintered body is slightly reduced.
【００２６】[0026]
【発明の効果】本発明によれば、窒化ケイ素焼結体の原
料粉末として、生産が比較的容易で、焼結時における結
晶粒成長を抑制することが可能な、微細粒子からなる窒
化ケイ素粉末、及びその製造方法を提供することができ
る。According to the present invention, as a raw material powder for a silicon nitride sintered body, silicon nitride powder composed of fine particles, which is relatively easy to produce and can suppress crystal grain growth during sintering, , And a method for producing the same.
【００２７】本発明の窒化ケイ素複合粉末を用いること
によって、室温から１１００℃の中低温域で強度等の機
械的特性に優れ、高い信頼性が要求される自動車エンジ
ン部材をはじめ、耐摩工具等の構造用セラミックス材料
として極めて有用な窒化ケイ素焼結体を製造することが
できる。By using the silicon nitride composite powder of the present invention, it is excellent in mechanical properties such as strength in a medium to low temperature range of from room temperature to 1100 ° C., and is required for high-reliability automobile engine parts, wear-resistant tools and the like. A silicon nitride sintered body that is extremely useful as a structural ceramic material can be manufactured.
Claims (4)
粒子と窒化チタン粒子とから構成された平均直径が１μ
ｍ以上である窒化ケイ素複合粉末。An average diameter of 1 μm composed of silicon nitride particles and titanium nitride particles having an average particle diameter of 100 nm or less.
m or more.
金属チタン粉末とを１０〜２００Ｇの加速度で混合する
ことを特徴とする窒化ケイ素複合粉末の製造方法。2. A method for producing a silicon nitride composite powder, comprising mixing a silicon nitride powder and a metal titanium powder at a rate of 10 to 200 G in a nitrogen atmosphere.
５０重量％であることを特徴とする、請求項２に記載の
窒化ケイ素複合粉末の製造方法。3. The addition amount of the metal titanium powder is 10 to 10
The method for producing a silicon nitride composite powder according to claim 2, wherein the content is 50% by weight.
ことを特徴とする、請求項２又は３に記載の窒化ケイ素
複合粉末の製造方法。4. The method for producing a silicon nitride composite powder according to claim 2, wherein the mixing time is from 0.1 hour to 10 hours.
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|---|---|---|---|
| JP30385397A JP4061678B2 (en) | 1997-11-06 | 1997-11-06 | Method for producing silicon nitride composite powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30385397A JP4061678B2 (en) | 1997-11-06 | 1997-11-06 | Method for producing silicon nitride composite powder |
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| Publication Number | Publication Date |
|---|---|
| JPH11139882A true JPH11139882A (en) | 1999-05-25 |
| JP4061678B2 JP4061678B2 (en) | 2008-03-19 |
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| JP30385397A Expired - Fee Related JP4061678B2 (en) | 1997-11-06 | 1997-11-06 | Method for producing silicon nitride composite powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001139380A (en) * | 1999-11-09 | 2001-05-22 | Sumitomo Electric Ind Ltd | Silicon nitride-based composite material and method for manufacturing the same |
| WO2002057197A1 (en) * | 2001-01-22 | 2002-07-25 | Sumitomo Electric Industries, Ltd. | Electroconductive silicon nitride based composite sintered body and method for preparation thereof |
| WO2002085812A1 (en) * | 2001-04-20 | 2002-10-31 | Sumitomo Electric Industries, Ltd. | Silicon nitride based composite sintered product and method for production thereof |
| JP2002338365A (en) * | 2001-05-14 | 2002-11-27 | Sumitomo Electric Ind Ltd | Aluminum nitride-base composite powder and method of manufacturing for the same |
| EP1332816A2 (en) * | 2002-01-30 | 2003-08-06 | Sumitomo Electric Industries, Ltd. | Conductive silicon nitride composite sintered body and a process for the production thereof |
| JP2009215150A (en) * | 2008-03-07 | 2009-09-24 | Korea Inst Of Science & Technology | Method for preparation of titanium nitride powder |
-
1997
- 1997-11-06 JP JP30385397A patent/JP4061678B2/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001139380A (en) * | 1999-11-09 | 2001-05-22 | Sumitomo Electric Ind Ltd | Silicon nitride-based composite material and method for manufacturing the same |
| WO2002057197A1 (en) * | 2001-01-22 | 2002-07-25 | Sumitomo Electric Industries, Ltd. | Electroconductive silicon nitride based composite sintered body and method for preparation thereof |
| US7132061B2 (en) | 2001-01-22 | 2006-11-07 | Sumitomo Electric Industries, Ltd. | Electroconductive silicon nitride based composite sintered body and method for preparation thereof |
| EP1361202A1 (en) * | 2001-01-22 | 2003-11-12 | Sumitomo Electric Industries, Ltd. | Electroconductive silicon nitride based composite sintered body and method for preparation thereof |
| EP1361202A4 (en) * | 2001-01-22 | 2004-07-28 | Sumitomo Electric Industries | Electroconductive silicon nitride based composite sintered body and method for preparation thereof |
| US7008893B2 (en) | 2001-04-20 | 2006-03-07 | Sumitomo Electric Industries, Ltd. | Silicon nitride-based composite sintered body and producing method thereof |
| WO2002085812A1 (en) * | 2001-04-20 | 2002-10-31 | Sumitomo Electric Industries, Ltd. | Silicon nitride based composite sintered product and method for production thereof |
| US6844282B2 (en) | 2001-04-20 | 2005-01-18 | Sumitomo Electric Industries, Ltd. | Silicon nitride based composite sintered product and method for production thereof |
| JP2002338365A (en) * | 2001-05-14 | 2002-11-27 | Sumitomo Electric Ind Ltd | Aluminum nitride-base composite powder and method of manufacturing for the same |
| EP1332816A3 (en) * | 2002-01-30 | 2004-06-30 | Sumitomo Electric Industries, Ltd. | Conductive silicon nitride composite sintered body and a process for the production thereof |
| US6911162B2 (en) | 2002-01-30 | 2005-06-28 | Sumitomo Electric Industries, Ltd. | Conductive silicon nitride composite sintered body and a process for the production thereof |
| EP1332816A2 (en) * | 2002-01-30 | 2003-08-06 | Sumitomo Electric Industries, Ltd. | Conductive silicon nitride composite sintered body and a process for the production thereof |
| JP2009215150A (en) * | 2008-03-07 | 2009-09-24 | Korea Inst Of Science & Technology | Method for preparation of titanium nitride powder |
| JP4695173B2 (en) * | 2008-03-07 | 2011-06-08 | コリア インスティテュート オブ サイエンス アンド テクノロジー | Method for preparing titanium nitride powder |
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