JPH02116675A - Production of sintered sic body - Google Patents
Production of sintered sic bodyInfo
- Publication number
- JPH02116675A JPH02116675A JP63269669A JP26966988A JPH02116675A JP H02116675 A JPH02116675 A JP H02116675A JP 63269669 A JP63269669 A JP 63269669A JP 26966988 A JP26966988 A JP 26966988A JP H02116675 A JPH02116675 A JP H02116675A
- Authority
- JP
- Japan
- Prior art keywords
- sic
- hip treatment
- sintered
- powder
- sintered body
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract 2
- 229910052796 boron Inorganic materials 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 13
- 238000001272 pressureless sintering Methods 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 9
- 239000011230 binding agent Substances 0.000 abstract description 4
- 239000005011 phenolic resin Substances 0.000 abstract description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 2
- 239000006229 carbon black Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 238000011068 loading method Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000000280 densification Methods 0.000 description 12
- 239000012752 auxiliary agent Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000254158 Lampyridae Species 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 235000015170 shellfish Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/575—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by pressure sintering
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- 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、高密度ＳｉＣ焼結体の製造方法に係り、特に
メカニカルシール等に好適な耐摩耗性ＳｉＣ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 manufacturing a high-density SiC sintered body, and particularly to a method for manufacturing wear-resistant SiC suitable for mechanical seals and the like.
「従来の技術」
ＳｉＣは共有結合性が強く、難焼結性の物質で、焼結さ
せるためには、焼結助剤の添加が必要である。"Prior Art" SiC has a strong covalent bond and is a material that is difficult to sinter, and in order to sinter it, it is necessary to add a sintering aid.
上記焼結助剤としては、加圧、常圧焼結を含めテＢ５Ｃ
５Ａｌ！ 、Ａｔ！２０１、Ｙ、０３、ＢＮ、、Ａｆｆ
Ｎ。The above sintering aids include TeB5C, including pressure and pressureless sintering.
5Al! , At! 201,Y,03,BN,,Aff
N.
ＢａＯ等が公知であり、特に、常圧焼結助剤としては、
Ｂ−Ｃ系、＋３−Ａ（！−Ｃ系、ｌ！−Ｃ系、Ａ（ｔ○
３− Ｙ 、Ｏ、系等が知られている。BaO etc. are well known, and in particular, as pressureless sintering aids,
B-C system, +3-A(!-C system, l!-C system, A(t○
3-Y, O, systems, etc. are known.
しかし、いずれの助剤を用いても、通常２〜３％のボア
（気孔）が焼結体内に残留する。焼結体内にボアが存在
すると、材料としての信頼性を低下させ、摺動摩耗特性
に悪い影響をおよぼす。However, no matter which aid is used, typically 2-3% of pores remain in the sintered body. The presence of a bore within the sintered body reduces the reliability of the material and adversely affects the sliding wear characteristics.
ボアの少ない焼結体を得るためには、加圧焼結法が有効
で、ホットプレス焼結法、或いはＨＩ Ｐ処理等の方法
が用いられている。In order to obtain a sintered body with a small bore, a pressure sintering method is effective, and methods such as a hot press sintering method or a HIP treatment are used.
［発明が解決しようとする課題］
ところで、ホットプレス法では、焼結体の形状、大きさ
に制限があり、ＨＩＰ法はホットプレス法に比して高い
生産性を有しているが、Ｂ−Ｃ系助剤を用いてＳｉＣ粉
末を焼結する場合のように、耐クリープ特性の大きなも
のに対しては、焼結体の緻密化効果が認められない。こ
れは耐クリープ特性が大であるため２０００℃を越える
温度においても粒界すベリ、あるいは拡散クリープが進
行しにく（高圧ガスにより予備焼結体に静水圧を加えて
もボアの消滅が進行しないためである。[Problem to be solved by the invention] By the way, in the hot press method, there are restrictions on the shape and size of the sintered body, and the HIP method has higher productivity than the hot press method. As in the case of sintering SiC powder using a -C-based auxiliary agent, no effect on densification of the sintered body is observed for materials with high creep resistance. This has high creep resistance, so grain boundary burr or diffusion creep does not progress even at temperatures exceeding 2000°C (bore disappearance progresses even when hydrostatic pressure is applied to the pre-sintered compact using high-pressure gas). This is to prevent it from happening.
本発明は信頼性が高く、摺動性、耐摩耗性に優れた緻密
なＳｉＣ焼結体の製造方法を提供することを目的とする
。An object of the present invention is to provide a method for manufacturing a dense SiC sintered body that is highly reliable and has excellent sliding properties and wear resistance.
「課題を解決するための手段」
Ｂ、Ｃを添加したＳｉＣ焼結体は耐クリープ性が大きい
ためＨＩＰ処理で緻密かしないが、Ａ（を添加したＳｉ
ＣはＢ−Ｃ系ＳｉＣに較べて高温強度は低下するが、高
温で軟化するため高温においてクリープ変形が進行し易
く、ＨＩＰによる緻密化が可能であることを見い出した
。"Means for solving the problem" SiC sintered bodies with B and C added have high creep resistance and are not densified by HIP treatment, but SiC with A (added)
Although C has lower high-temperature strength than B--C SiC, it has been found that since it softens at high temperatures, creep deformation progresses easily at high temperatures, and densification by HIP is possible.
ＨＩＰ処理を可能にするためには高温においてクリープ
変形が進行する助剤系を選べばよい。具体的にはＡ Ｑ
＝０３ Ｙ ｔｏ ３系、Ａｌ−Ｃ系、Ｂ−ＡＱ−Ｃ
系等が上げられる。これらの中で特にＢ１−Ｃ系につい
てはＢ１Ａｌ２ｅＣｔ化合物の存在により１８００℃に
て液相が生成すると云われており、より低温でのＨＩＰ
処理効果が大きい。しかも他の助剤に較べて強度等の特
性低下が少ない。In order to enable HIP treatment, an auxiliary agent system that undergoes creep deformation at high temperatures may be selected. Specifically, AQ
=03 Y to 3 system, Al-C system, B-AQ-C
System etc. are mentioned. Among these, especially for the B1-C system, it is said that a liquid phase is generated at 1800°C due to the presence of the B1Al2eCt compound, and HIP at lower temperatures is not possible.
Great processing effect. Furthermore, compared to other auxiliary agents, properties such as strength are less likely to deteriorate.
本発明はこれらの知見に基づいてなされたものでその要
旨は、Ｂ、ＡＱＳＣを含有するＳｉＣ粉末を成形し、常
圧焼結した後、ざらにＨＩ Ｐ処理することを特徴とす
るＳｉＣ焼結体の製造法である。The present invention has been made based on these findings, and the gist thereof is to form a SiC powder containing B and AQSC, sinter it under normal pressure, and then perform a rough HIP treatment. It is a method of manufacturing the body.
用いられるＳｉＣ粉末は、α、βいずれでもよ（、その
粒度は３μｍ以下が適当である。またその純度はＳ ｉ
Ｃ９５重量％以上のものが望ましい。The SiC powder used may be either α or β (the particle size is suitably 3 μm or less, and the purity is Si
It is desirable that the content is C95% by weight or more.
Ｂは単体のほう素粉末でもよく、またＢ、Ｃの粉末でも
よい。B may be a single boron powder, or B and C powders.
Ｃは成形体に加えたフェノール樹脂などの焼成による炭
化物、カーホンブラ、り、黒鉛粉末なとが用いられる。As C, a carbide obtained by firing phenol resin added to the molded body, carbon black, phosphor, graphite powder, etc. are used.
ＡＱは単体粉末の外１！、Ｃ，Ａｉ、などの形で加えて
もよい。AQ is 1 other than single powder! , C, Ai, etc.
これらの添加ｍはＢ：０．０３〜５ｍＷ１％（以下％は
すべで重量基′Ｉ＄）、ＡＱ： Ｏ，１〜５％、Ｃ二０
．３〜５％が適当である。化合物として添加した場合、
例えばＢ、Ｃでは夫々Ｂ、Ｃとして計算される。These addition m are B: 0.03 to 5 mW1% (all percentages below are based on weight), AQ: O, 1 to 5%, C20
．． 3 to 5% is appropriate. When added as a compound,
For example, B and C are calculated as B and C, respectively.
成形にはＰＶＡなどの一次結合材を添加し、貝類粒化し
た後所望の形に加圧成形するのが一般的である。ＰＶＡ
などの結合材に代えてフェノール樹脂などを用い、−次
結合材兼焼成後の炭化カーボンとすることもできる。For molding, it is common to add a primary binder such as PVA, granulate the shellfish, and then pressure mold it into the desired shape. PVA
It is also possible to use a phenol resin or the like instead of a binder such as, and use it as a secondary binder and carbonized carbon after firing.
成形体は先ず常圧焼成する。この焼成は非酸化性雰囲気
下で１８００〜２３００ ’Ｃで行なう。The molded body is first fired under normal pressure. This calcination is carried out at 1800-2300'C in a non-oxidizing atmosphere.
次にここで得られた焼結体を常法によりＨＩＰ処理する
。この温度は１６００〜２２００℃１圧力は２００〜２
０００ｋｇ／ｃｍ’の範囲が適当である。Next, the sintered body obtained here is subjected to HIP treatment by a conventional method. This temperature is 1600~2200℃ 1 pressure is 200~2
A range of 000 kg/cm' is suitable.
「実施例」
ＳｉＣ焼結体のＨＩＰ処理を可能とするためには、添加
する助剤の種類、配合量を選択しなければならない。助
剤としては、例えばＡｌ２ｔ０３Ｙ、Ｏ，系、ＡＱ−Ｃ
系、Ｂ−Ａ１２−Ｃ系等が挙げられるが、特にＢ−、ｌ
！−Ｃ系助剤は、比較的低温でのＨＩ Ｐ処理を可能と
する。"Example" In order to enable HIP processing of a SiC sintered body, the type and amount of the auxiliary agent to be added must be selected. As the auxiliary agent, for example, Al2t03Y, O, type, AQ-C
system, B-A12-C system, etc., but especially B-, l
! -C-based auxiliary agents enable HIP treatment at relatively low temperatures.
ＳｉＣ中にＢとＡ［が共存すると、低融点の化合物が形
成されるため、異常粒成長を生じ粗大粒が形成されるが
、この粒子の成長はＣの添加によって制御することが出
来る。When B and A[ coexist in SiC, a compound with a low melting point is formed, resulting in abnormal grain growth and formation of coarse grains, but this grain growth can be controlled by adding C.
Ｂ−ＡＱ−Ｃ系助剤を添加する場合、Ｂの量が０．０３
％未満、或いはＡＱの量が０．１％未満では、例え一方
の量が多くとも、低融点物の爪が少なく、ＨＩＰ処理に
よる緻密化効果は得られない。When adding B-AQ-C type auxiliary agent, the amount of B is 0.03
% or the amount of AQ is less than 0.1%, even if one of the amounts is large, there will be few nails of low melting point substances, and the densification effect by HIP treatment will not be obtained.
またＣの量が０．３％未満では、粗大粒子を制御するこ
とが出来ない。Moreover, if the amount of C is less than 0.3%, coarse particles cannot be controlled.
また、Ｂまたは八〇、の蛍が５％を越えると一方の里を
制限範囲内で減少しても、余剰分のＢまたはＡＱが緻密
化を阻害し、Ｃの世も、５％を越えると緻密化が低下す
る。In addition, if the number of B or 80 fireflies exceeds 5%, even if one village is reduced within the limit, the surplus B or AQ will inhibit densification, and the number of fireflies in C will also exceed 5%. and densification decreases.
また、ＨＩＰ処理の温度が１６００℃未満では、助剤が
溶融しないので、緻密化が行なわれず、２２００℃を越
えても、緻密化効果は変わらず、経済的にも不利となる
。Furthermore, if the temperature of the HIP treatment is less than 1,600°C, the auxiliary agent will not melt, so densification will not occur, and even if it exceeds 2,200°C, the densification effect will not change, which is economically disadvantageous.
実施例１〜６
平均粒径０，４μｍのαＳｉＣに助剤としてＢ、ＡＱ、
Ｃをそれぞれ種々な量添加し、２ ｔ／ ａｍ２の圧力
により成形した後、２０００ ’Ｃ１１ｈｒの条件でＡ
ｒ気流中で常圧焼結した。これらを、２０００’Ｃ，２
０００ｋｇ／ｃｍ”、 ｌ ｈｒの条件でＨＩＰ処理
し、ＨＩＰ処理の前および後における焼結体の密度を測
定してＨＩＰ処理による緻密化の程度を調べた。結果を
第１表に示す。Examples 1 to 6 αSiC with an average particle size of 0.4 μm was supplemented with B, AQ,
After adding various amounts of C and molding under a pressure of 2 t/am2, A
Normal pressure sintering was carried out in r air flow. these at 2000'C, 2
The sintered body was subjected to HIP treatment under conditions of 000 kg/cm" and 1 hr, and the density of the sintered body was measured before and after the HIP treatment to examine the degree of densification caused by the HIP treatment. The results are shown in Table 1.
第１表
第１表から、ＨＩＰ処理によって、いずれも緻密化が進
行していることがわかる。Table 1 From Table 1, it can be seen that densification progresses in all cases by the HIP treatment.
実施例７
実施例２と同じ加圧成形体を、２０００’Ｃ，５ｈｒで
常圧焼結し、２２００℃１２０００ｋｇ／ ａｆｆｉ’
、ｌｈｒの条件でＨ！Ｐ処理した。ＨＩＰ処理前密度は
、３．１３ｇ／ｃｍｔに対し、ＨＩ Ｐ処理後の密度は
３ 、１７ ｇ／ ａｍ３であった。Example 7 The same pressure-molded body as in Example 2 was sintered under normal pressure at 2000'C for 5 hours, and 12000 kg/affi' at 2200°C.
, H under the condition of lhr! P-treated. The density before HIP treatment was 3.13 g/cmt, while the density after HIP treatment was 3.17 g/am3.
ＡＱ： ０．７％に対して、Ｃを最低４％添加すれば、
粗大粒の生成はな（なるが、反面、不要なＣにより緻密
化が阻害され、２２００℃までＨＩＰ処理温度を高めて
も３．１７ｇ／ｃｍ’までしか緻密化しない。AQ: If you add at least 4% of C to 0.7%,
No coarse grains are formed (but on the other hand, densification is inhibited by unnecessary C, and even if the HIP treatment temperature is increased to 2200° C., densification is only achieved to 3.17 g/cm').
実施例８〜２５
平均粒径０．４μｍのα−３ｉＣに助剤としてＢ、ＡＱ
、Ｃを添加し、２ｔ／ｃｆｆｉ′で加圧成形し、これら
を１９００〜２０００’Ｃ，ｌ 〜５ｈｒの条件で常圧
焼結した後、１９００ ’Ｃ１２０００ｋｇ／ ａｍ’
、Ｉｈｒの条件でＨＩＰ処理を行なった。ＨＩＰ処理前
、後の焼結体の密度を第２表に示す。Examples 8 to 25 B and AQ as auxiliaries to α-3iC with an average particle size of 0.4 μm
, C was added, pressure molded at 2t/cffi', and these were sintered at normal pressure under conditions of 1900 to 2000'C, l to 5hr.
The HIP process was performed under the conditions of , Ihr. Table 2 shows the density of the sintered body before and after HIP treatment.
第２表
第２表より、１９００℃のＨＩＰ処理温度においても充
分緻密化が進行していることがわかる。From Table 2, it can be seen that densification progresses sufficiently even at the HIP treatment temperature of 1900°C.
「発明の効果」
以上述べたように、本発明に係るＳｉＣ焼結体の！！ｉ
２遣方法は、Ｂ−ＡＱ−Ｃ系助剤のそれぞれの成分添加
量を規制することによって、常圧焼結した焼結体をＨＩ
Ｐ処理を施して効率よく緻密化することが可能となり、
さらにＨＩＰ処理温度を所定の範囲とすることによって
その効果が助長され、耐摩耗性の焼結体が容易に得られ
る優れた方法である。"Effects of the Invention" As described above, the SiC sintered body according to the present invention! ! i
In the 2-way method, the sintered body sintered under normal pressure is HI
It becomes possible to efficiently densify by applying P treatment,
Furthermore, the HIP treatment temperature is within a predetermined range to enhance its effect, making it an excellent method for easily obtaining a wear-resistant sintered body.
Claims (2)
結し、さらにＨＩＰ処理を施すことを特徴とするＳｉＣ
焼結体の製造方法。1. SiC characterized by molding SiC powder containing B, Al, and C, pressureless sintering, and further performing HIP treatment.
A method for producing a sintered body.
ある請求項１記載のＳｉＣ焼結体の製造方法。2. The method for manufacturing a SiC sintered body according to claim 1, wherein the temperature of the HIP treatment is in the range of 1600 to 2200°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63269669A JPH02116675A (en) | 1988-10-26 | 1988-10-26 | Production of sintered sic body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63269669A JPH02116675A (en) | 1988-10-26 | 1988-10-26 | Production of sintered sic body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02116675A true JPH02116675A (en) | 1990-05-01 |
Family
ID=17475560
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63269669A Pending JPH02116675A (en) | 1988-10-26 | 1988-10-26 | Production of sintered sic body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02116675A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100475258B1 (en) * | 1998-09-11 | 2005-03-10 | 도요탄소 가부시키가이샤 | Mechanical seal member |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6158861A (en) * | 1984-08-27 | 1986-03-26 | イ−グル工業株式会社 | Silicon carbide material and manufacture |
| JPS6355162A (en) * | 1986-08-22 | 1988-03-09 | 株式会社日立製作所 | High heat conductivity sintered body and manufacture |
-
1988
- 1988-10-26 JP JP63269669A patent/JPH02116675A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6158861A (en) * | 1984-08-27 | 1986-03-26 | イ−グル工業株式会社 | Silicon carbide material and manufacture |
| JPS6355162A (en) * | 1986-08-22 | 1988-03-09 | 株式会社日立製作所 | High heat conductivity sintered body and manufacture |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100475258B1 (en) * | 1998-09-11 | 2005-03-10 | 도요탄소 가부시키가이샤 | Mechanical seal member |
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