JPH0459660A - Production of silicon nitride ceramics - Google Patents
Production of silicon nitride ceramicsInfo
- Publication number
- JPH0459660A JPH0459660A JP2172013A JP17201390A JPH0459660A JP H0459660 A JPH0459660 A JP H0459660A JP 2172013 A JP2172013 A JP 2172013A JP 17201390 A JP17201390 A JP 17201390A JP H0459660 A JPH0459660 A JP H0459660A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- silicon nitride
- nitride ceramics
- sintering
- production
- 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.)
- Pending
Links
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 11
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 239000000919 ceramic Substances 0.000 title claims description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 238000010304 firing Methods 0.000 claims description 3
- 230000002542 deteriorative effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〔概要〕
窒化硅素系セラミックスの製造方法に関し、強度が高く
、高温での強度劣化の少ない焼結体を得ることを目的と
し、
焼結助剤を添加し、窒化硅素粉末からなる成形体をクラ
ファイト粉末中に埋没し、不活性雰囲気中で焼成して焼
結体を得ることを特徴として窒化硅素セラミックスの製
造方法を構成する。[Detailed Description of the Invention] [Summary] Regarding a method for producing silicon nitride ceramics, the purpose is to obtain a sintered body with high strength and less deterioration in strength at high temperatures. The method for manufacturing silicon nitride ceramics is characterized in that a molded body made of powder is buried in graphite powder and fired in an inert atmosphere to obtain a sintered body.
本発明は窒化硅素（以下５ｉＪ４）セラミックスの製造
方法に関する。The present invention relates to a method for manufacturing silicon nitride (hereinafter referred to as 5iJ4) ceramics.
Ｓｉ３Ｎ４は１０００°Ｃを越す高温におても高い強度
を示し、軽量であって耐薬品性、耐摩耗性および熱衝撃
性に優れた材料として知られている。Si3N4 is known as a material that exhibits high strength even at high temperatures exceeding 1000°C, is lightweight, and has excellent chemical resistance, abrasion resistance, and thermal shock resistance.
すなわち、Ｓｉ、Ｎ４は高温においても安定であって、
比重は３．１８５と軽（、モース硬度は９と高く、高温
の融解金属にも侵されないなどの特徴をもっている。That is, Si and N4 are stable even at high temperatures,
It has a light specific gravity of 3.185, a high Mohs hardness of 9, and is uncorrupted by high-temperature molten metal.
そのため、高温での耐蝕性が必要な坩堝やノズルなどの
構成材として適し、また、電子機器用としては軽量で且
つ摩耗が少ないことからプリンタなどの摺動部材として
適している。Therefore, it is suitable as a constituent material for crucibles, nozzles, etc. that require corrosion resistance at high temperatures, and it is suitable for electronic equipment as a sliding member for printers and the like because it is lightweight and has little wear.
Ｓｉ３Ｎ４の焼結温度は約１７００°Ｃであり、１８０
０℃付近から徐々に解離する性質をもっている。The sintering temperature of Si3N4 is about 1700°C, and 180°C
It has the property of gradually dissociating from around 0°C.
また、Ｓｉ、Ｎ４は共有結合しているため焼結性は低い
。Further, since Si and N4 are covalently bonded, sinterability is low.
そこで、緻密な焼結体を得るには５１３Ｎ４粉に焼結助
剤を添加して焼成を行う必要があり、アルミナ（Ａ１２
０３）やマグネシア（ＭｇＯ）などの添加が行われてい
た。Therefore, in order to obtain a dense sintered body, it is necessary to add a sintering agent to the 513N4 powder and perform firing, and alumina (A12
03) and magnesia (MgO).
然し、これらの焼結助剤を添加して焼結を行うと、粒界
にガラス相が生じ、このために高温において強度が低下
すると云う問題がある。However, when sintering is performed with the addition of these sintering aids, a glass phase is generated at the grain boundaries, which causes a problem in that the strength decreases at high temperatures.
そこで、粒界のガラス化を防ぐ方法として、焼結助剤と
してイツトリア（Ｙ２Ｏ２）とＡｌ２２０：ｌの混合物
を用い、窒化アルミニウム（ＡｆｆＮ）粉末中に埋めて
焼成する方法が開発された。Therefore, as a method for preventing vitrification of grain boundaries, a method was developed in which a mixture of yttria (Y2O2) and Al220:l is used as a sintering aid, and the mixture is buried in aluminum nitride (AffN) powder and fired.
（助剤については、特公昭４８−７４８６．４９−２１
０９１など、詰粉については、特公昭５６−０３８７．
５６−０３８８など、何れも東方）
然し、ＡＡＮ粉末を用いて焼結を行うと、製品の表面に
ＡＩ！Ｎ粉末が付着して表面の平滑性が失われると云う
問題がある。(For auxiliary agents, please refer to Special Publication No. 48-7486.49-21
For powder stuffing such as 091, Tokuko Sho 56-0387.
56-0388, etc.) However, when sintering is performed using AAN powder, AI! There is a problem that the surface smoothness is lost due to N powder adhesion.
特に、射出成形法で作った複雑な形状をした成形品につ
いては、表面に付着したＡ７Ｎ粉末の除去には非常に工
数を要し、また、焼結処理によりＡＩＮ粉末が相互に固
まっていることから、製品の取り出しにも時間を必要と
すると云う問題があった。In particular, for molded products with complex shapes made by injection molding, it takes a lot of man-hours to remove the A7N powder adhering to the surface, and the AIN powder is solidified together due to the sintering process. Therefore, there was a problem in that it took time to take out the product.
結晶化した粒界を有するＳｉ、Ｎ４セラミックス焼結体
の製造に当たって、表面の平滑性を損なうことなく効率
よく焼結する方法を開発することが課題である。In producing Si, N4 ceramic sintered bodies having crystallized grain boundaries, it is a challenge to develop a method for efficiently sintering without impairing surface smoothness.
上記の課題は焼結助剤を添加した５ｉＪ４粉末からなる
成形体をグラファイト粉末中に埋没し、不活性雰囲気中
で焼成して焼結体を得ることを特徴として５ｊｓＮ４セ
ラミツクスの製造方法を構成することにより解決するこ
とができる。The above-mentioned problem constitutes a method for producing 5jsN4 ceramics, which is characterized by embedding a compact made of 5iJ4 powder to which a sintering aid has been added in graphite powder and firing it in an inert atmosphere to obtain a sintered body. This can be solved by
本発明はＳｉ、Ｎ４成形体を埋没して高温焼成する粉体
（詰め粉）としてＡβＮ粉体の代わりにグラファイト粉
末を用いるものである。The present invention uses graphite powder instead of AβN powder as the powder (stuffing powder) in which the Si, N4 molded body is buried and fired at high temperature.
すなわち、グラファイトは融点が３５００°Ｃ以上。In other words, graphite has a melting point of 3500°C or higher.
沸点は４８２７°Ｃと元素の中では最も高く、不活性ガ
ス雰囲気中で加熱する場合は最も安定な材料である。Its boiling point is 4827°C, the highest among the elements, and it is the most stable material when heated in an inert gas atmosphere.
また、グラファイト粉末自体に辷り性をもつと云う特徴
がある。In addition, graphite powder itself has the characteristic of having stickiness.
そこで、本発明はグラファイト粉末を詰め粉として使用
することにより、焼結体の表面に詰め粉が付着すると云
う問題点をなくするものである。Therefore, the present invention uses graphite powder as the filling powder to eliminate the problem of the packing powder adhering to the surface of the sintered body.
これを焼結炉に入れ、Ｎ２雰囲気中てＮ２圧を１００気
圧として１７００°Ｃで５時間焼成した。This was placed in a sintering furnace and fired at 1700°C for 5 hours in a N2 atmosphere with a N2 pressure of 100 atm.
冷却した後、坩堝を炉外に取り出し、焼結体をピンセッ
トで摘みあげたところ、グラファイト粉末は全く付着し
ておらず、表面平滑性も良好であった。After cooling, the crucible was taken out of the furnace and the sintered body was picked up with tweezers, and it was found that no graphite powder had adhered to it at all, and the surface had good smoothness.
また、焼結体のＸ線回折を行ったところ、β−３ｉＪ４
のピーク以外にも結晶粒界が結晶質になっていることを
示すピークも観察できた。In addition, when X-ray diffraction of the sintered body was performed, β-3iJ4
In addition to this peak, a peak indicating that the grain boundaries were crystalline was also observed.
セラミックスの成分として、
本体 ： ５１３Ｎ４粉末 ・・・８６重量部、焼
結助剤：Ａｊ’２０＋粉末・・・４重量部、／／
：Ｙ ２０３粉末 ・・・１０重量部、からなる板状の
成形体を圧粉プレスにより形成した。As components of the ceramics: Main body: 513N4 powder...86 parts by weight, Sintering aid: Aj'20+ powder...4 parts by weight, //
:Y203 powder: A plate-shaped molded body consisting of 10 parts by weight was formed using a powder press.
次に、グラファイト製の坩堝を平均粒径が５μｍのグラ
ファイト粉末で満たし、この中心に板状の成形体を埋没
した。Next, a graphite crucible was filled with graphite powder having an average particle size of 5 μm, and a plate-shaped molded body was embedded in the center of the crucible.
本発明によれば、高温強度に優れ、また表面平滑性に優
れた５ｉｓＮ４セラミツクスを効率が良く、また短縮し
た工程で製造することができる。According to the present invention, 5isN4 ceramics having excellent high-temperature strength and surface smoothness can be manufactured efficiently and in a shortened process.
Claims (1)
ファイト粉末中に埋没し、不活性雰囲気中で焼成して焼
結体を得ることを特徴とする窒化硅素セラミックスの製
造方法。A method for producing silicon nitride ceramics, which comprises adding a sintering aid, embedding a molded body made of silicon nitride powder in graphite powder, and firing it in an inert atmosphere to obtain a sintered body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2172013A JPH0459660A (en) | 1990-06-29 | 1990-06-29 | Production of silicon nitride ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2172013A JPH0459660A (en) | 1990-06-29 | 1990-06-29 | Production of silicon nitride ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0459660A true JPH0459660A (en) | 1992-02-26 |
Family
ID=15933912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2172013A Pending JPH0459660A (en) | 1990-06-29 | 1990-06-29 | Production of silicon nitride ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0459660A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5352395A (en) * | 1992-07-17 | 1994-10-04 | Phillips Petroleum Company | Carbon and ceramic-containing layers for use in sintering of silicon nitride article |
-
1990
- 1990-06-29 JP JP2172013A patent/JPH0459660A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5352395A (en) * | 1992-07-17 | 1994-10-04 | Phillips Petroleum Company | Carbon and ceramic-containing layers for use in sintering of silicon nitride article |
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