JPH02137774A - Production of sintered ceramics - Google Patents
Production of sintered ceramicsInfo
- Publication number
- JPH02137774A JPH02137774A JP63288320A JP28832088A JPH02137774A JP H02137774 A JPH02137774 A JP H02137774A JP 63288320 A JP63288320 A JP 63288320A JP 28832088 A JP28832088 A JP 28832088A JP H02137774 A JPH02137774 A JP H02137774A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- ceramic
- dense film
- pressure
- treatment
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000005240 physical vapour deposition Methods 0.000 claims abstract description 5
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 4
- 238000007733 ion plating Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract 3
- 230000002706 hydrostatic effect Effects 0.000 abstract 2
- 229910003910 SiCl4 Inorganic materials 0.000 abstract 1
- 238000005299 abrasion Methods 0.000 abstract 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 abstract 1
- 239000002775 capsule Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000008393 encapsulating agent Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はセラミックス焼結体の製造方法に関り、更に詳
しくは信頼性、耐摩耗特性に優れた緻密なセラミックス
焼結体を熱間静水圧処理（ＨｏｔＩｓｏｓｔａｔｉｃ
Ｐｒｅｓｓｉｎｇ、以下略してＨＩＰ処理という）によ
って得る方法に関する。Detailed Description of the Invention (Industrial Field of Application) The present invention relates to a method for producing a ceramic sintered body, and more specifically, a method for producing a dense ceramic sintered body with excellent reliability and wear resistance by hot static heating. Hydraulic treatment (HotIsostatic)
Pressing (hereinafter abbreviated as HIP processing).
（従来の技術）
セラミックス予備焼結体等の被成形物をより高密度に焼
結する方法にいわゆるホウドブレス法があるが、このホ
ットプレス法では一方向のみしか加圧されない為に、焼
結体の構成粒子に配向性を生じる。すなわち、焼結体に
おいてホットプレス焼結時の加圧方向に垂直な面と平行
な面とでは機械的、物理的性質が異なるという欠点があ
った。(Prior art) The so-called hot press method is a method for sintering objects to be formed, such as ceramic pre-sintered bodies, to a higher density. However, since this hot press method only applies pressure in one direction, gives an orientation to the constituent particles. That is, there is a drawback that the mechanical and physical properties of the sintered body are different between a plane perpendicular to the pressing direction during hot press sintering and a plane parallel to it.
そこでこの焼結体の異方性をなくす焼結方法として発達
してきたのが気体（主として不活性ガス）を圧力媒体と
して用い、被成形物を等分圧縮を行うという方法はＨｔ
ｐ処理である。Therefore, a sintering method that has been developed to eliminate this anisotropy of the sintered body is a method that uses gas (mainly inert gas) as a pressure medium and compresses the molded object in equal parts.
p treatment.
従来セラミックスにＨＩＰ処理を施し、Ｗ１密化する場
合、ＨＩＰ処理前の焼結体密度に応じて２通りの方法が
とられている。その１つは被処理体か高密度焼結体の場
合であり、この場合は被処理を直接高圧ガスにより加圧
してＨＩＰ処理を行う、もう１つの方法は被処理体が特
に理論密度の９６％を下回るような低密度焼結体の場合
であり、この場合は焼結体内部に開気孔が形成されてい
るため単に直接加圧すると、開気孔内にガス圧力が浸透
し、これが内部圧力として逆に働くため全く緻密化しな
いか、又は表面近くのボアーを残すことになる。このよ
うな場合セラミ・ンクス予備焼結体等の被処理体を適当
なカプセル内に封入しカプセルごと加圧してＨＩＰ処理
する方法がとられている。Conventionally, when performing HIP treatment on ceramics to increase the W1 density, two methods have been used depending on the density of the sintered body before HIP treatment. One method is when the object to be processed is a high-density sintered body, in which case the object to be processed is directly pressurized with high-pressure gas to perform HIP treatment. In this case, open pores are formed inside the sintered body, so if pressure is applied directly, gas pressure will penetrate into the open pores, which will increase the internal pressure. This works in the opposite way, resulting in either no densification or leaving a bore near the surface. In such cases, a method is used in which the object to be processed, such as a pre-sintered body of ceramic inx, is encapsulated in a suitable capsule and the capsule is pressurized to perform HIP treatment.
（発明が解決しようとする課８）
カプセル弐〇ＩＰのカプセルは通常ガラスが使用されて
いる。ＨＩＰ処理温度がカプセル材質の融点以下である
場合は問題とはならないが例えば炭化ケイ素のように高
温度でのＨＩＰ処理が必要となる場合、適当なカプセル
材がない、ＨＩＰ処理を施す場合１通常ルツボ内にセラ
ミックス予備焼結体等の被処理体を入れ、間にガラスを
充填し２溶融したガラス内に埋没した状態で加圧を行う
のが一般的である。このような場合、形状、寸法に制約
を生じ、場合によってはカプセル材と被処理体との反応
やカプセル材の被処理体内部への侵入等が問題となり期
待される焼結体が得られ難い、このような低密度のセラ
ミックス予備焼結体の場合にも有効なＨＩＰ処理する方
法を提供するのが本発明の目的である。(Question 8 to be solved by the invention) Capsule 2 Glass is usually used for IP capsules. This is not a problem if the HIP treatment temperature is below the melting point of the capsule material, but if HIP treatment is required at a high temperature, such as silicon carbide, there is no suitable capsule material, and if HIP treatment is performed 1. Generally, an object to be processed, such as a pre-sintered ceramic body, is placed in a crucible, glass is filled between the crucible, and pressure is applied while the object is buried in the molten glass. In such cases, there are restrictions on the shape and dimensions, and in some cases, there may be problems such as reactions between the encapsulant and the object to be processed, or penetration of the encapsulant into the object to be processed, making it difficult to obtain the expected sintered body. It is an object of the present invention to provide an effective HIP treatment method even for such low-density ceramic presintered bodies.
本件発明者は上記の目的を達成するため鋭意研究を行っ
た結果、従来のカプセルに代えて、セラミックス予備焼
結体の表面に緻密な膜を形成させてＨＩＰ処理を行うと
全体が均一で緻密な焼結体が得られることを発見して本
件発明を完成させた。As a result of intensive research to achieve the above object, the inventor of the present invention has found that, instead of using conventional capsules, a dense film is formed on the surface of a ceramic pre-sintered body and HIP treatment is performed to make the whole body uniform and dense. The present invention was completed by discovering that it is possible to obtain a sintered body.
すなわち本件発明の要旨は、セラミックス予備焼結体の
表面に同一又は異種の材質で緻密な膜を形成させ熱間静
水圧処理することを特徴とするセラミックス焼結体の製
造方法にある。That is, the gist of the present invention resides in a method for producing a ceramic sintered body, which is characterized by forming a dense film of the same or different materials on the surface of the ceramic pre-sintered body and subjecting it to hot isostatic pressure treatment.
セラミックス予備焼結体の密度が十分でない場合では予
備焼結体の内部に開気孔が存在し。If the density of the ceramic pre-sintered body is not sufficient, open pores will exist inside the pre-sintered body.
開気孔が完全に連結しているとカプセルフリー弐〇ＩＰ
処理では全く緻密化しない。また完全に連結していない
場合でも焼結体内部で生ずる圧力損失に応じて表面から
数１０ｇ■〜数■−の深さまでガスが侵入し、内部は緻
密化するが表面部のボアーはガスの侵入によりむしろ拡
大する。Capsule-free 2〇IP when open pores are completely connected
The processing does not densify it at all. In addition, even if the sintered body is not completely connected, gas will penetrate from the surface to a depth of several tens of grams to several grams depending on the pressure loss that occurs inside the sintered body, and the interior will become dense, but the bores on the surface will not allow gas to penetrate. Rather, it expands through invasion.
これに対して本発明の予備焼結体の表面に緻密な膜を形
成すると焼結体内へのガスの侵入が阻止されるため低密
度の焼結体でも均一に緻密化が生じ表面にボアーを残さ
ない。On the other hand, when a dense film is formed on the surface of the pre-sintered body of the present invention, gas infiltration into the sintered body is prevented, so even a low-density sintered body is uniformly densified and bores are formed on the surface. I won't leave anything behind.
本発明において予備焼結体の表面に形成させる膜は予備
焼結体の材質と異なる材質のものであっても良いが、同
一材質の膜の方が好ましく、この場合はガラスカプセル
の場合のような母材との反応による表面劣化の問題が生
じない。In the present invention, the film formed on the surface of the pre-sintered body may be made of a material different from that of the pre-sintered body, but it is preferable that the film is made of the same material, and in this case, as in the case of a glass capsule, There is no problem of surface deterioration due to reaction with the base material.
膜を形成する方法は上記の問題を考慮しつつＣＶ Ｄ
（Ｃｈｅｍｉｃａｌ Ｖａｐｏｒ Ｄｅｐｏｓｉｔｉｏ
ｎ ）法、ｐｖＤ （Ｐｈｙｓｉｃａｌ Ｖａｐｏｒ
Ｄｅｐｏｓｉｔｉｏｎ ）法、溶射法等を考慮しつつ行
う０例えば直流法、高周波法、クラスタイオンビーム法
、熱陰極法、ＡＲＥ法、プラズマ電子ビーム法（ＨＣＤ
）、アーク放電型高真空法などのイオンプレーティング
法、真空蒸着法、スパッタリング法などのＰＶＤ法やプ
ラズマ法、減圧法、常圧法などのＣＶＤ法であるが、と
りわけイオンプレーティングＰＶＤ法又はＣＶＤ法が好
ましい。The method of forming the film is CVD, taking into account the above problems.
(Chemical Vapor Depositio
n) method, pvD (Physical Vapor
For example, direct current method, high frequency method, cluster ion beam method, hot cathode method, ARE method, plasma electron beam method (HCD method)
), ion plating methods such as arc discharge type high vacuum method, PVD methods such as vacuum evaporation method and sputtering method, and CVD methods such as plasma method, reduced pressure method, and normal pressure method, but especially ion plating PVD method or CVD method. law is preferred.
以下実施例を挙げて本発明をさらに詳しく説明する。The present invention will be explained in more detail below with reference to Examples.
（実施例）
炭化ケイ素にホウ素粉末０．１５重量％、アルミニウム
粉末０．５重量％、カーボン粉末２．０重量％添加し１
９００°Ｃ，１時間常圧焼結した。得られた焼結体の密
度は３．０６ｇ ／ ｃ ｍ”であった。この焼結体表
面に５ｉＣＩ４およびＣＨ４を原料としてＣＶＤ法にて
ＳｉＣの膜をコーティングした。これを２０００℃、２
０００ｋｇ／ ｃ ｒｎ”でＨＩＰ処理した。得られた
焼結体の鏡面を顕微鏡て観察したところＨＩＰ処理前と
比較すると中心部および表面部とも十分Ｗ１密化してい
るのが観察された。(Example) 0.15% by weight of boron powder, 0.5% by weight of aluminum powder, and 2.0% by weight of carbon powder were added to silicon carbide.
Normal pressure sintering was performed at 900°C for 1 hour. The density of the obtained sintered body was 3.06 g/cm''.A SiC film was coated on the surface of this sintered body by CVD using 5iCI4 and CH4 as raw materials.
When the mirror surface of the obtained sintered body was observed under a microscope, it was observed that the W1 density was sufficiently increased in both the center and the surface area when compared to before the HIP treatment.
（比較例）
実施例と同様の手順で作成した炭化ケイ素常圧焼結体を
ＣＶＤ１ｌｉをコーティングすることな〈実施例と同一
条件てＨＩＰ処理を施した。得られた焼結体の鏡面組織
を顕微鏡で観察したところ中心部はＨＩＰ処理により緻
密化しているが表面部はガスの侵入によりボアーがむし
ろ拡大しているのが観察された。(Comparative Example) A pressureless sintered silicon carbide body prepared in the same manner as in the example was subjected to HIP treatment under the same conditions as in the example without coating with CVD1li. When the specular structure of the obtained sintered body was observed under a microscope, it was observed that the center part was densified by the HIP treatment, but the bores in the surface part were rather enlarged due to the intrusion of gas.
（発明の効果）
セラミックスの大型部材を製造する場合、小型の試験片
と異なり、密度は上がりにくい。しかもこのような大型
部材をカプセル方式によりＨＩＰ処理することは困難で
ある。一方コーティング膜によれば被）ＩＩＰ処理部材
の大きさ、形状によらず均一に１！［化が可能となる。(Effect of the invention) When manufacturing a large ceramic member, unlike a small test piece, it is difficult to increase the density. Furthermore, it is difficult to perform HIP processing on such a large member using the capsule method. On the other hand, according to the coating film, 1! [It becomes possible to
また、摺動部材として利用する場合は、特に表面状態が
問題となる。単なるコーティングによる表面改質では、
使用中にコーテイング膜の剥離の問題が生じるがＨＩＰ
処理を施し母材そのものをｆｆｉ密化することにより信
頼性の高い摺動部材が得られる。Furthermore, when used as a sliding member, the surface condition becomes a particular problem. Surface modification by mere coating
There is a problem with the coating film peeling off during use, but HIP
By applying the treatment to make the base material itself ffi dense, a highly reliable sliding member can be obtained.
Claims (2)
質で緻密な膜を形成させ熱間静水圧処理することを特徴
とするセラミックス焼結体の製造方法。1. A method for producing a ceramic sintered body, which comprises forming a dense film of the same or different materials on the surface of a pre-sintered ceramic body and subjecting it to hot isostatic pressure treatment.
ィングＰＶＤ法である請求項１記載のセラミックス焼結
体の製造方法。2. 2. The method for producing a ceramic sintered body according to claim 1, wherein the method for forming the dense film is a CVD method or an ion plating PVD method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63288320A JPH02137774A (en) | 1988-11-15 | 1988-11-15 | Production of sintered ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63288320A JPH02137774A (en) | 1988-11-15 | 1988-11-15 | Production of sintered ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02137774A true JPH02137774A (en) | 1990-05-28 |
Family
ID=17728654
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63288320A Pending JPH02137774A (en) | 1988-11-15 | 1988-11-15 | Production of sintered ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02137774A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5469130A (en) * | 1992-11-27 | 1995-11-21 | Murata Mfg. Co., Ltd. | High frequency parallel strip line cable comprising connector part and connector provided on substrate for connecting with connector part thereof |
-
1988
- 1988-11-15 JP JP63288320A patent/JPH02137774A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5469130A (en) * | 1992-11-27 | 1995-11-21 | Murata Mfg. Co., Ltd. | High frequency parallel strip line cable comprising connector part and connector provided on substrate for connecting with connector part thereof |
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