JPS6332841B2 - - Google Patents
Info
- Publication number
- JPS6332841B2 JPS6332841B2 JP55104733A JP10473380A JPS6332841B2 JP S6332841 B2 JPS6332841 B2 JP S6332841B2 JP 55104733 A JP55104733 A JP 55104733A JP 10473380 A JP10473380 A JP 10473380A JP S6332841 B2 JPS6332841 B2 JP S6332841B2
- Authority
- JP
- Japan
- Prior art keywords
- graphite
- hot press
- silicon carbide
- silicon
- press mold
- 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.)
- Expired
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 28
- 229910002804 graphite Inorganic materials 0.000 claims description 27
- 239000010439 graphite Substances 0.000 claims description 27
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 18
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 18
- 239000002344 surface layer Substances 0.000 claims description 9
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 14
- 238000000034 method Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 150000003377 silicon compounds Chemical class 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910003910 SiCl4 Inorganic materials 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
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Description
【発明の詳細な説明】
本発明は種々のセラミツクや金属を焼結させる
ための黒鉛質ホツトプレス型に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a graphite hot press mold for sintering various ceramics and metals.
高強度、高密度などのすぐれた機械的性質を有
する焼結体はホツトプレスによる加圧焼結法によ
つてつくることができる。 A sintered body having excellent mechanical properties such as high strength and high density can be produced by a pressure sintering method using a hot press.
従来ホツトプレスの型としては熱安定性にすぐ
れ熱伝導性・電気伝導性の大きな黒鉛が用いられ
てきた。 Conventionally, graphite, which has excellent thermal stability and high thermal and electrical conductivity, has been used as a hot press mold.
しかしながら、黒鉛は一般には500℃以上の酸
化性雰囲気でガス化反応を起こし急速に物性劣化
を示すものであり、特に摩擦摩耗によるホツトプ
レス型の消耗が激しくなり操作条件や製品の寸法
精度が不安定になるなどの欠点がある。 However, graphite generally undergoes a gasification reaction in an oxidizing atmosphere of 500°C or higher and shows rapid deterioration of its physical properties.In particular, hot press molds are subject to severe wear due to frictional wear, resulting in unstable operating conditions and product dimensional accuracy. There are disadvantages such as becoming
本発明はこれらの従来技術の欠点を解消するた
めに、耐摩耗性、耐酸化性にすぐれた黒鉛質ホツ
トプレス型を得ることを目的とするものである。 The object of the present invention is to obtain a graphite hot press mold having excellent wear resistance and oxidation resistance in order to eliminate these drawbacks of the prior art.
すなわち、本発明は表層を炭化硅素に転化して
なることを特徴とする黒鉛質ホツトプレス型を提
供するものである。 That is, the present invention provides a graphite hot press mold characterized in that the surface layer is converted to silicon carbide.
炭化珪素は耐摩耗性、耐酸化性にすぐれ、黒鉛
の欠点をおぎなうことができるものであり、具体
的には黒鉛の表面上にあるいは表層を炭化珪素化
して被覆することが考えられる。 Silicon carbide has excellent wear resistance and oxidation resistance, and can overcome the drawbacks of graphite. Specifically, silicon carbide can be coated on the surface or layer of graphite by converting it into silicon carbide.
そのための第１の方法として、SiCl4などの珪
素化合物とC6H6などの炭化水素を1100℃〜1400
℃に加熱された黒鉛基材表面で熱分解させ炭化珪
素を沈積させる方法があり、第２の方法として一
酸化珪素雰囲気内で黒鉛基材を1700℃〜2200℃に
加熱し黒鉛表層を炭化珪素に転化させる方法があ
る。 The first method for this purpose is to heat a silicon compound such as SiCl4 and a hydrocarbon such as C6H6 at 1100℃ to 1400℃.
There is a method in which silicon carbide is deposited by thermal decomposition on the surface of a graphite substrate heated to ℃.A second method is to heat a graphite substrate to 1700℃ to 2200℃ in a silicon monoxide atmosphere to transform the graphite surface layer into silicon carbide. There is a way to convert it into
しかし、第１の方法では沈積された炭化珪素被
膜は加熱加圧時にクラツクが入り剥離しやすい。
これは黒鉛と炭化珪素被膜との間に化学結合力が
はたらいておらず、熱膨張係数のわずかなちがい
で発生する応力に耐えられないからである。又、
黒鉛表面に沈積した炭化珪素被膜の分だけ厚みが
増すため精密に加工したホツトプレス型の精度が
そこなわれてしまう。処理操作については珪素化
合物と炭化水素および水素、アルゴンガスなどの
キヤリヤーガスとの混合、搬入が複雑である。 However, in the first method, the deposited silicon carbide film tends to crack and peel off when heated and pressurized.
This is because there is no chemical bonding force between the graphite and the silicon carbide coating, and the graphite cannot withstand the stress generated by a slight difference in coefficient of thermal expansion. or,
Since the thickness increases by the amount of silicon carbide film deposited on the graphite surface, the accuracy of the precisely machined hot press mold is impaired. Regarding processing operations, mixing and transporting silicon compounds, hydrocarbons, and carrier gases such as hydrogen and argon gas are complicated.
これに対して第２の方法は黒鉛の表層そのもの
が一酸化珪素との反応によつて炭化珪素に転換す
るため黒鉛部分との結合は強固で加熱加圧時にク
ラツクが入り剥離することはない。又、精密に加
工された黒鉛表層が炭化珪素に転換する際に寸法
変化はほとんど起こらないので、ホツトプレス型
の加工精度は保たれる。処理操作も第１の方法に
くらべ簡単で安定している。 On the other hand, in the second method, the surface layer of graphite itself is converted into silicon carbide by reaction with silicon monoxide, so the bond with the graphite portion is strong and does not crack or peel off when heated and pressurized. Furthermore, since almost no dimensional change occurs when the precisely processed graphite surface layer is converted into silicon carbide, the processing accuracy of the hot press type is maintained. Processing operations are also simpler and more stable than in the first method.
このような理由から黒鉛質ホツトプレス型の表
層を炭化珪素化する方法として一酸化珪素ガスと
の反応による転換法が望ましい。一酸化珪素は金
属珪素粉と二酸化珪素粉の混合体、あるいは炭素
粉と二酸化珪素粉の混合体を1400℃〜2200℃に加
熱させることにより発生させることができる。し
かし後者の系がより効率的に一酸化珪素を発生さ
せることができる。また、被処理物である黒鉛質
ホツトプレス型は一酸化珪素発生源と離して置
き、均一の厚さの炭化珪素に転換、被覆できる位
置を選ぶことができる。 For these reasons, a conversion method using a reaction with silicon monoxide gas is desirable as a method for converting the surface layer of a graphite hot press mold into silicon carbide. Silicon monoxide can be generated by heating a mixture of metal silicon powder and silicon dioxide powder, or a mixture of carbon powder and silicon dioxide powder to 1400°C to 2200°C. However, the latter system can generate silicon monoxide more efficiently. Furthermore, the graphite hot press mold that is the object to be treated can be placed away from the source of silicon monoxide, and a position can be selected where it can be converted and coated with silicon carbide of uniform thickness.
処理温度が1700℃以下になると一酸化珪素は雰
囲気中の一酸化炭素と優先的に反応して繊維状の
微細な炭化珪素を生じ、黒鉛表面上で成長するた
め、黒鉛表層の炭化珪素への転換は起こらない。
一方、処理温度が2200℃以上になると炭化珪素に
転換した黒鉛表層が分解を起こし始める。このこ
とから処理温度は1700〜2200℃の範囲にしなけれ
ばならないことが判明した。 When the treatment temperature is below 1700°C, silicon monoxide reacts preferentially with carbon monoxide in the atmosphere to produce fine fibrous silicon carbide, which grows on the graphite surface, causing the silicon carbide on the surface layer of the graphite to grow. No transformation occurs.
On the other hand, when the treatment temperature exceeds 2200°C, the surface layer of graphite, which has been converted to silicon carbide, begins to decompose. From this, it was found that the treatment temperature must be in the range of 1700 to 2200°C.
以下、本発明の実施例について具体的に説明す
る。 Examples of the present invention will be specifically described below.
実施例
外径150mmφ×内径60mmφ×高さ170mmφの円筒
形黒鉛質ホツトプレス型を作成した。このホツト
プレス型を金属珪素粉と二酸化珪素粉の混合成形
体（モル比1.0）と接触しないように黒鉛容器内
に入れ密閉し、黒鉛化炉で加熱した。処理温度は
2000℃とし、この温度で５時間保持した。Example A cylindrical graphite hot press mold with an outer diameter of 150 mmφ, an inner diameter of 60 mmφ, and a height of 170 mmφ was prepared. This hot press mold was placed in a graphite container and sealed so as not to come into contact with a mixed compact of metal silicon powder and silicon dioxide powder (molar ratio 1.0), and heated in a graphitization furnace. The processing temperature is
The temperature was set to 2000°C and maintained at this temperature for 5 hours.
この処理の結果、黒鉛質ホツトプレス型の表層
0.5mm〜0.8mmはβ型炭化珪素に転換していること
がわかつた。 As a result of this treatment, the surface layer of the graphite hot press mold
It was found that 0.5 mm to 0.8 mm was converted to β-type silicon carbide.
以上のようにして得たホツトプレス型と未処理
で同一寸法の黒鉛質ホツトプレス型を用いて1750
℃、150Kg／cm2の条件でアルミナ粉末のホツトプ
レス焼結を行なつた。この結果、耐用回数では本
発明品は未処理品にくらべ５倍ののびを示した。 Using an untreated graphite hot press mold with the same dimensions as the hot press mold obtained as described above, 1750
Hot press sintering of alumina powder was carried out at 150 kg/cm 2 at 150°C. As a result, the product of the present invention exhibited five times the service life as the untreated product.
本発明によつて得られた黒鉛質ホツトプレスは
上記の結果からも明らかなように、耐摩耗性が大
巾に向上し、酸化消耗による物性劣化も減少して
耐用回数が大幅に向上することができるものであ
る。 As is clear from the above results, the graphite hot press obtained by the present invention has significantly improved wear resistance, reduced physical property deterioration due to oxidative wear, and significantly increased service life. It is possible.
Claims (1)
する黒鉛質ホツトプレス型。1. A graphite hot press type characterized by having a surface layer converted to silicon carbide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10473380A JPS5729407A (en) | 1980-07-29 | 1980-07-29 | Graphitic hot press mold |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10473380A JPS5729407A (en) | 1980-07-29 | 1980-07-29 | Graphitic hot press mold |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5729407A JPS5729407A (en) | 1982-02-17 |
| JPS6332841B2 true JPS6332841B2 (en) | 1988-07-01 |
Family
ID=14388689
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10473380A Granted JPS5729407A (en) | 1980-07-29 | 1980-07-29 | Graphitic hot press mold |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5729407A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0218257U (en) * | 1988-07-19 | 1990-02-06 |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2603917B2 (en) * | 1984-09-20 | 1997-04-23 | 株式会社東芝 | Method for manufacturing electrolyte plate of molten carbonate fuel cell |
| JP2603916B2 (en) * | 1984-09-20 | 1997-04-23 | 株式会社東芝 | Heater panel for electrolyte plate production of molten carbonate fuel cell |
| JPH0633951B2 (en) * | 1986-07-15 | 1994-05-02 | イビデン株式会社 | High temperature heating furnace |
| JP2686485B2 (en) * | 1988-07-18 | 1997-12-08 | イビデン株式会社 | Carbon mold for hot pressing and manufacturing method thereof |
| JP2719814B2 (en) * | 1988-12-26 | 1998-02-25 | イビデン株式会社 | Mold |
| US5656216A (en) * | 1994-08-25 | 1997-08-12 | Sony Corporation | Method for making metal oxide sputtering targets (barrier powder envelope) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4933811A (en) * | 1972-07-31 | 1974-03-28 | ||
| JPS52100510A (en) * | 1976-02-18 | 1977-08-23 | Inoue Japax Res | Sintering method and protection sheets |
| JPS5555809A (en) * | 1978-10-20 | 1980-04-24 | Ngk Spark Plug Co | Hot press mold |
-
1980
- 1980-07-29 JP JP10473380A patent/JPS5729407A/en active Granted
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4933811A (en) * | 1972-07-31 | 1974-03-28 | ||
| JPS52100510A (en) * | 1976-02-18 | 1977-08-23 | Inoue Japax Res | Sintering method and protection sheets |
| JPS5555809A (en) * | 1978-10-20 | 1980-04-24 | Ngk Spark Plug Co | Hot press mold |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0218257U (en) * | 1988-07-19 | 1990-02-06 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5729407A (en) | 1982-02-17 |
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