JPH0230671A - Production of sintered material of silicon carbide - Google Patents
Production of sintered material of silicon carbideInfo
- Publication number
- JPH0230671A JPH0230671A JP63181081A JP18108188A JPH0230671A JP H0230671 A JPH0230671 A JP H0230671A JP 63181081 A JP63181081 A JP 63181081A JP 18108188 A JP18108188 A JP 18108188A JP H0230671 A JPH0230671 A JP H0230671A
- Authority
- JP
- Japan
- Prior art keywords
- sintered material
- silicon carbide
- processing
- sintered body
- thermal shock
- 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
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 239000000463 material Substances 0.000 title abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 238000005498 polishing Methods 0.000 claims description 17
- 238000012545 processing Methods 0.000 abstract description 13
- 229910002804 graphite Inorganic materials 0.000 abstract description 6
- 239000010439 graphite Substances 0.000 abstract description 6
- 230000035939 shock Effects 0.000 abstract description 6
- 239000006229 carbon black Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 6
- 238000009863 impact test Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は耐熱性、耐摩耗性、耐蝕性、摺動特性に優れた
炭化珪素焼結体の焼結方法に関し、研削または研磨加工
された炭化珪素焼結体よりなるメカニカルシール、釣ガ
イドリング等の製品の耐衝撃性の向上を図った炭化珪素
焼結体の製造方法に関する。[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a method for sintering a silicon carbide sintered body having excellent heat resistance, wear resistance, corrosion resistance, and sliding properties. The present invention relates to a method of manufacturing a silicon carbide sintered body that improves the impact resistance of products such as mechanical seals and fishing guide rings made of the silicon carbide sintered body.
（従来の技術〕
炭化珪素（５ｉＣ）の焼結体は、耐熱性、耐摩耗性、耐
蝕性、摺動特性に優れたセラミックス材料であることは
よく知られており、メカニカルシール、釣ガイドリング
等として早くから実用化されている。(Prior art) It is well known that sintered silicon carbide (5iC) is a ceramic material with excellent heat resistance, wear resistance, corrosion resistance, and sliding properties, and is used in mechanical seals, fishing guide rings, etc. It was put into practical use from an early stage.
しかし、耐衝撃性に劣り最近ではその改質、向上を厳し
く要求されてきている。However, it has poor impact resistance, and recently there have been strict demands for its modification and improvement.
メカニカルシール、釣ガイドリング等としてＳａｃ焼結
体を用いる場合、寸法精度、面粗度が高度に要求される
ため、焼結のままでは使用が困難であり、研削、研磨ま
たはバレル仕上げ等の加工が必要である。When using Sac sintered bodies for mechanical seals, fishing guide rings, etc., a high level of dimensional accuracy and surface roughness is required, so it is difficult to use them as they are sintered, and processing such as grinding, polishing, or barrel finishing is difficult. is necessary.
ＳｔＣ焼結体などの脆性材料は、研削、研磨またはバレ
ル仕上げ等の加工を加えると加工面にマイクロクラック
が発生し極度に強度が低下する。When a brittle material such as a StC sintered body is subjected to processing such as grinding, polishing, or barrel finishing, microcracks occur on the processed surface and the strength is extremely reduced.
その結果、チッピング、クラック等の破損が発生したり
、耐衝撃性、耐熱衝撃性の低下をきたす。As a result, damage such as chipping and cracking occurs, and impact resistance and thermal shock resistance decrease.
従って、本発明の目的とするところは、研削、研磨また
はバレル仕上げ等の加工を加えて発生するマイクロクラ
ックを出来るだけ除去し耐衝撃性の向上を図ることにあ
る。Therefore, it is an object of the present invention to improve the impact resistance by removing as much as possible the microcracks that occur when processing such as grinding, polishing, or barrel finishing is applied.
本発明は、上述の問題を解決するために鋭意検討を重ね
た結果、いったん研削または研磨加工されたＳｉＣ焼結
体を黒鉛粉末で覆い１８００〜２１５０℃の範囲で１時
間以上真空または不活性ガス雰囲気でもう一度焼結処理
することを主旨とするＳｉＣ焼結体の焼結方法で耐衝撃
性を向上させたメカニカルシール、釣ガイドリング等の
ＳｉＣ製品を提供するものである。As a result of extensive research to solve the above-mentioned problems, the present invention has been developed by covering a ground or polished SiC sintered body with graphite powder and heating it in a vacuum or inert gas at a temperature of 1800 to 2150°C for more than 1 hour. The present invention provides SiC products such as mechanical seals and fishing guide rings that have improved impact resistance using a method of sintering SiC sintered bodies that is sintered once again in an atmosphere.
ＳｉＣ焼結体は脆性材料のため、研削、研磨またはバレ
ル仕上げ等の加工を加えると加工面にマイクロクラック
が発生し、強度を極度に低下する。Since the SiC sintered body is a brittle material, when it is processed by grinding, polishing, barrel finishing, etc., microcracks occur on the processed surface and the strength is extremely reduced.
加工後の焼結体を再焼結処理すると加工時に発生したマ
イクロクラックが埋まり、加工前の組織になるのである
。When the sintered body is re-sintered after processing, the microcracks generated during processing are filled in and the structure becomes the same as before processing.
加工時に発生したマイクロクラックが埋まり、更にＳｉ
Ｃの結晶サイズが成長し、強度を低下させない様にする
ために再焼結処理条件は１８００〜２１５０℃の温度範
囲で１時間以上焼結処理することになる。 １８００℃
未満ではマイクロクラックが埋らず。Microcracks that occurred during processing are filled, and Si
In order to prevent the crystal size of C from growing and the strength from decreasing, the resintering treatment conditions are sintering at a temperature range of 1800 to 2150° C. for 1 hour or more. 1800℃
If it is less than that, the micro cracks will not be filled.
２１５０℃を越えるとＳｉＣの結晶サイズが粗大化し。When the temperature exceeds 2150°C, the crystal size of SiC becomes coarse.
強度の低下を来たす、また再焼結処理時間は、１〜８時
間が好ましく、１時間未満ではマイクロクラックの埋ま
りが不十分で、８時間を越えると一般的に焼結エネルギ
ーの浪費につながる。The resintering treatment time is preferably from 1 to 8 hours, and if it is less than 1 hour, the filling of microcracks is insufficient, and if it exceeds 8 hours, it generally results in wasted sintering energy.
再焼結処理の雰囲気は、通常のＳｉＣの焼結と同様に真
空または不活性ガス雰囲気の必要がある。The atmosphere for the resintering process needs to be a vacuum or an inert gas atmosphere, as in normal SiC sintering.
再焼結処理の温度範囲では真空度はｌＸ１０＝Ｔｏｒｒ
程度であり、不活性ガス雰囲気の場合、空気の焼結炉へ
の流入によるＳｉＣ焼結体の酸化を防止する程度にわず
かに加圧状態にすることが必要である。In the temperature range of resintering process, the degree of vacuum is lX10=Torr
In the case of an inert gas atmosphere, it is necessary to slightly pressurize the SiC sintered body to prevent oxidation of the SiC sintered body due to air flowing into the sintering furnace.
本発明のＳｉＣ焼結体の再焼結処理により加工時に発生
したマイクロクラックが埋まるためチッピング、クラッ
ク等による破損が発生したり、耐衝撃性、耐熱衝撃性の
低下をきたすことを防止することができ、強度的な向上
を図る事が出来る。The resintering treatment of the SiC sintered body of the present invention fills in the microcracks that occur during processing, thereby preventing damage due to chipping, cracking, etc., and deterioration of impact resistance and thermal shock resistance. It is possible to improve the strength.
また、いったん研削または研磨加工されたＳｉＣ焼結体
を炭素粉末で覆い再焼結処理することにより、仕上げ面
が再焼結処理する以前とほぼ同等となり平滑でつやのあ
る外観が再現される。Further, by covering the SiC sintered body that has been ground or polished with carbon powder and subjecting it to re-sintering, the finished surface becomes almost the same as before the re-sintering process, and a smooth and glossy appearance is reproduced.
覆う炭素粉末はＳｉＣ焼結体と反応しないものならなん
でもよく、黒鉛、カーボンブラック等が好ましい、炭素
粉末で覆うことによりＳｉＣ焼結体表面より、わずかな
分圧でＳｉＣが分解を防ぐために平滑でつやのある面が
保たれるのである。The covering carbon powder may be of any material as long as it does not react with the SiC sintered body, and graphite, carbon black, etc. are preferable.By covering with carbon powder, the surface of the SiC sintered body is smoothed to prevent SiC from decomposing under a slight partial pressure. This will keep the surface shiny.
以下、本発明を実施例により詳細に説明する。 Hereinafter, the present invention will be explained in detail with reference to Examples.
実施例１
ＳｉＣ焼結体よりなる外径１８ｍｍ、内径１１１層、高
さ３■の釣ガイドリングを荒バレル研磨および仕上げバ
レル研磨後、黒鉛ルツボに入れ更に黒鉛粉末で覆い焼結
炉に投入し、Ａｒ雰囲気にて２０５０℃、３時間再焼結
をおこない、鏡面仕上げを行った縦２５０ｓｖ、横２０
０１■、厚さ５０■腸のＳｉＣ板上に落下衝撃試験を行
った結果、５０％破壊率の落下高さは、１００ｃ鵬であ
った。Example 1 A fishing guide ring made of a SiC sintered body with an outer diameter of 18 mm, an inner diameter of 111 layers, and a height of 3 cm was subjected to rough barrel polishing and final barrel polishing, and then placed in a graphite crucible and further covered with graphite powder and placed in a sintering furnace. , re-sintered at 2050°C for 3 hours in an Ar atmosphere to give a mirror finish.
As a result of performing a drop impact test on a SiC plate of 0.01 cm and thickness of 50 cm, the drop height at a 50% failure rate was 100 cm.
また、落下衝撃試験を行う前の釣ガイドリングはつやが
あり、鏡面状態を維持していた。In addition, the fishing guide ring before the drop impact test was shiny and maintained a mirror finish.
比較例１
ＳｉＣ焼結体よりなる外径ＩＥｌｕ＋、内径１１ｍｍ、
高さ３■の釣ガイドリングを荒バレル研磨および仕上げ
バレル研磨後、鏡面仕上げを行った縦２５０■騰、横２
００１、厚さ５０層層のＳｉＣ板上に落下衝撃試験を行
った結果、５０％破壊率の落下高さは＋ ５０ｃｍであ
った。Comparative Example 1 Made of SiC sintered body, outer diameter IElu+, inner diameter 11 mm,
After rough barrel polishing and finishing barrel polishing, a fishing guide ring with a height of 3 cm was finished with a mirror finish.
001, a drop impact test was conducted on a 50-layer SiC plate, and the drop height at 50% failure rate was +50 cm.
また、 ＳｉＣ焼結体よりなる外径１８層■、内径１１
■、高さ３ｍｍの釣ガイドリングを荒バレル研磨および
仕上げバレル研磨後、黒鉛ルツボに入れ黒鉛粉末で覆わ
ず焼結炉に投入し、Ａｒ雰囲気にて２０５０℃、３時間
再焼結をおこなった結果、つやは失われ鏡面状態は維持
されなかった。In addition, the outer diameter is 18 layers and the inner diameter is 11 layers made of SiC sintered body.
■After rough barrel polishing and final barrel polishing, a fishing guide ring with a height of 3 mm was placed in a graphite crucible, placed in a sintering furnace without being covered with graphite powder, and re-sintered at 2050℃ for 3 hours in an Ar atmosphere. As a result, the gloss was lost and the mirror finish was not maintained.
実施例２
ＳｉＣ焼結体よりなる外径８■■、内径５．８ｍｍ、高
さ２ｍ嘗の釣ガイドリングを荒バレル研磨および仕上げ
バレル研磨後、黒鉛ルツボに入れ更に黒鉛粉末で覆い焼
結炉に投入し、Ａｒ雰囲気にて２０５０℃、３時間再焼
結をおこない、鏡面仕上げを行った縦２５０■騰、横２
０軸１．厚さ５０ｍ■のＳｉＣ板上に落下衝撃試験を行
った結果、５０％破壊率の落下高さは、３００ｃｍであ
った。Example 2 A fishing guide ring made of a SiC sintered body with an outer diameter of 8 mm, an inner diameter of 5.8 mm, and a height of 2 m was subjected to rough barrel polishing and final barrel polishing, and then placed in a graphite crucible and further covered with graphite powder in a sintering furnace. and re-sintered in an Ar atmosphere at 2050℃ for 3 hours to give a mirror finish.
0 axis 1. As a result of performing a drop impact test on a SiC plate with a thickness of 50 m, the drop height for a 50% failure rate was 300 cm.
また、落下衝撃試験を行う前の釣ガイドリングはつやが
あり、鏡面状態を維持していた。In addition, the fishing guide ring before the drop impact test was shiny and maintained a mirror finish.
比較例２
ＳｉＣ焼結体よりなる外径８ｔｓ、内径５．８ｍｍ、高
さ２履■の釣ガイドリングを荒バレル研磨および仕上げ
バレル研磨後、鏡面仕上げを行った縦２５０ｍｍ、横２
００ｍｍ、厚さ５０ｍｍノＳｉＣ板上に落下ｍｓ試験を
行った結果、５０％破壊率の落下高さは、８Ｑｃ■であ
った・
また、 ＳｉＣ焼結体よりなる外径１８■層、内径ｌＩ
Ｉ、高さ３■嘗の釣ガイドリングを荒バレル研磨および
仕上げバレル研磨後、黒鉛ルツボに入れ黒鉛粉末で覆わ
ず焼結炉に投入し、Ａｒ雰囲気にて２０５０℃、３時間
再焼結をおこなった結果、つやは失われ鏡面状態は維持
されなかった。Comparative Example 2 A fishing guide ring made of a SiC sintered body with an outer diameter of 8 ts, an inner diameter of 5.8 mm, and a height of 2 mm was subjected to rough barrel polishing and finish barrel polishing, and then mirror-finished to a length of 250 mm and width of 2 mm.
As a result of conducting a drop ms test on a SiC plate with a thickness of 00 mm and a thickness of 50 mm, the drop height at 50% failure rate was 8 Qc. Also, the outer diameter of the layer made of SiC sintered body was 18 cm, and the inner diameter was lI.
After rough barrel polishing and final barrel polishing, a fishing guide ring with a height of 3 cm was placed in a graphite crucible, placed in a sintering furnace without being covered with graphite powder, and re-sintered at 2050℃ in an Ar atmosphere for 3 hours. As a result, the gloss was lost and the mirror finish was not maintained.
本発明によれば、焼結後の研削、研磨加工したＳｉＣ焼
結体の耐衝撃性、耐熱衝撃性を数段向上させるとともに
、研削、研磨加工されたＳｉＣ焼結体の仕上げ面も再焼
結処理前とほぼ同等となり平滑でつやのある外観をも再
現できるものである。According to the present invention, the impact resistance and thermal shock resistance of the SiC sintered body that has been ground and polished after sintering are improved several times, and the finished surface of the ground and polished SiC sintered body is also re-sintered. It is almost the same as before the binding process, and it is possible to reproduce a smooth and glossy appearance.
Claims (1)
い１８００〜２１５０℃の温度範囲で１時間以上真空ま
たは不活性ガス雰囲気で再焼結処理することを特徴とす
る炭化珪素焼結体の製造方法。A silicon carbide sintered body, which is characterized in that the silicon carbide sintered body after grinding or polishing is covered with carbon powder and resintered in a vacuum or inert gas atmosphere at a temperature range of 1800 to 2150°C for 1 hour or more. Production method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63181081A JPH0230671A (en) | 1988-07-20 | 1988-07-20 | Production of sintered material of silicon carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63181081A JPH0230671A (en) | 1988-07-20 | 1988-07-20 | Production of sintered material of silicon carbide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0230671A true JPH0230671A (en) | 1990-02-01 |
| JPH0527592B2 JPH0527592B2 (en) | 1993-04-21 |
Family
ID=16094480
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63181081A Granted JPH0230671A (en) | 1988-07-20 | 1988-07-20 | Production of sintered material of silicon carbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0230671A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5315068A (en) * | 1991-07-11 | 1994-05-24 | Houston Industries Incorporated | Terminal block insulator extender |
-
1988
- 1988-07-20 JP JP63181081A patent/JPH0230671A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5315068A (en) * | 1991-07-11 | 1994-05-24 | Houston Industries Incorporated | Terminal block insulator extender |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0527592B2 (en) | 1993-04-21 |
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