JPH0699052A - Ultra-high pressure and high temperature device - Google Patents
Ultra-high pressure and high temperature deviceInfo
- Publication number
- JPH0699052A JPH0699052A JP33751891A JP33751891A JPH0699052A JP H0699052 A JPH0699052 A JP H0699052A JP 33751891 A JP33751891 A JP 33751891A JP 33751891 A JP33751891 A JP 33751891A JP H0699052 A JPH0699052 A JP H0699052A
- Authority
- JP
- Japan
- Prior art keywords
- cylinder
- pressure
- stress
- wall
- ultra
- 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
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000000919 ceramic Substances 0.000 claims description 4
- 239000010432 diamond Substances 0.000 abstract description 14
- 229910003460 diamond Inorganic materials 0.000 abstract description 14
- 229910052582 BN Inorganic materials 0.000 abstract description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 abstract description 5
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 239000010959 steel Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 4
- 229910000997 High-speed steel Inorganic materials 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000036316 preload Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 229910052839 forsterite Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は例えばダイヤモンド、立
方晶窒化ホウ素の合成、ダイヤモンド結晶の育成、およ
びダイヤモンド、立方晶窒化ホウ素の焼結体を製造する
場合に用いられる超高圧高温装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an ultrahigh pressure and high temperature apparatus used, for example, in synthesizing diamond, cubic boron nitride, growing diamond crystals, and producing a sintered body of diamond and cubic boron nitride.
【０００２】[0002]
【従来の技術】ダイヤモンド合成などに用いられている
静的超高圧力の発生には、Ｇｅｎｅｒａｌ Ｅｌｅｃｔ
ｒｉｃ社が開発したいわゆるベルト型高圧高温装置が広
く工業的に用いられている。その他の種類の静的超高圧
力発生装置としては、ガードル型装置、マルチアンビル
装置、ピストン・シリンダー型装置が知られており、こ
れらの中で、ピストン・シリンダー型装置は、ピストン
の断面積とプレス荷重とから反応室内に発生させる圧力
を算出することができるので、正確な圧力制御に適した
装置であることが知られている。2. Description of the Related Art For the generation of static ultrahigh pressure used in diamond synthesis, etc., General Electric
The so-called belt type high-pressure high-temperature device developed by ric is widely used industrially. Other types of static ultrahigh pressure generators are known: girdle type devices, multi-anvil type devices, and piston / cylinder type devices. Since the pressure generated in the reaction chamber can be calculated from the press load, it is known that the device is suitable for accurate pressure control.
【０００３】ピストン−シリンダー型超高圧高温装置
は、米国のＧ．Ｃ．ケネディ教授による開発以来、研究
が続けられているが、装置の大型化にはまだ成功してお
らず、シリンダーの内径１インチが実用化された最大装
置と報じられいるものの、工業的に成功したとの報道は
ない。本発明は、従来の技術による装置が果たしえなか
った大型化と、シリンダーの耐用回数の増大とを可能と
した装置に関する。A piston-cylinder type ultra high pressure and high temperature apparatus is disclosed in US Pat. C. Research has continued since it was developed by Professor Kennedy, but it has not been successful in increasing the size of the device, and although it is reported that a cylinder inner diameter of 1 inch is the largest practical device, it has succeeded industrially. There is no report. The present invention relates to an apparatus that can be increased in size and increased in service life of a cylinder, which cannot be achieved by a conventional apparatus.
【０００４】この種の従来の装置において、シリンダー
用の材料としては、１５％程度のＣｏを含む超硬合金が
一般に用いられており、ダイヤモンド合成に必要な５５
ｋｂの圧力を反応室内に発生する際には、５５ｋｂの圧
力によってシリンダー内に生じる、ポアソン効果による
上下方向の引張応力にほぼ相当する圧縮荷重が、シリン
ダーの上下端面に加えられ、シリンダーの破損防止が計
られている。In a conventional apparatus of this type, a cemented carbide containing approximately 15% Co is generally used as a material for the cylinder, and 55 is necessary for diamond synthesis.
When a pressure of kb is generated in the reaction chamber, a compressive load, which is generated in the cylinder by the pressure of 55 kb and is almost equivalent to the vertical tensile stress due to the Poisson effect, is applied to the upper and lower end surfaces of the cylinder to prevent damage to the cylinder. Is being measured.
【０００５】[0005]
【発明が解決しようとする課題】ケネディ教授による装
置はこのような構成を採ることによってダイヤモンド合
成が可能にしている。しかしこの装置ではシリンダー材
料の強度限界を越えた範囲を外部からの加圧によって補
償し、補強するという思想に基づいており、液圧プレス
の能力の許す範囲内で、反応室の加圧断面積をできるだ
け大きくとるために、必要最低限の荷重をシリンダーの
補強に用いる設計となっている。従ってシリンダーは耐
圧限界ぎりぎりの条件において繰返し加圧操作を受ける
こととなり、このため、シリンダーの耐用回数は十分な
配慮がなされない限り１００回以下に過ぎず、経済的な
合成装置とはなり得ず、また装置の大型化が不可能であ
った。The apparatus by Professor Kennedy enables diamond synthesis by adopting such a configuration. However, this device is based on the idea that the range exceeding the strength limit of the cylinder material is compensated and reinforced by external pressure, and the pressure cross-sectional area of the reaction chamber should be within the range allowed by the hydraulic press capability. In order to take as much as possible, it is designed to use the minimum necessary load to reinforce the cylinder. Therefore, the cylinder is subjected to repeated pressurizing operation under the condition where the pressure limit is barely reached. Therefore, unless the sufficient consideration is given to the cylinder, the cylinder can only be used 100 times or less, making it an economical synthesizer. Moreover, it was impossible to increase the size of the device.
【０００６】[0006]
【課題を解決するための手段】本発明においては、シリ
ンダーの両端面全面に、シリンダー内部に加えられる圧
力によって発生するポアソン効果に対応する応力以上で
材質の圧縮強度以下の応力を加えることにより、逆にシ
リンダー内壁にポアソン効果による応力を発生すると共
にシリンダー外壁にもポアソン効果に対応する応力が発
生する。後者の応力は本発明においては、シリンダー外
壁に対する圧力容器の締め代として作用し、シリンダー
内壁を予圧したのに相当する効果が得られる。これら二
つの効果により、本発明装置においては、発生圧力の上
限値が従来装置に比べて飛躍的に大きくなり、５５ｋｂ
程度のダイヤモンド合成に必要な圧力を発生する使用方
法においても、相対的な圧力負担が小さいので、装置寿
命が飛躍的に増大する。本発明においては例えばダイヤ
モンド合成反応を行うときには、シリンダーに５５ｋｂ
の圧力が付加される。またシリンダー材質としては１５
％Ｃｏ−ＷＣ合金の他に、ダイス鋼・高速度鋼等の使用
が考えられている。In the present invention, by applying a stress equal to or higher than the stress corresponding to the Poisson effect generated by the pressure applied to the inside of the cylinder to the entire surfaces of both ends of the cylinder, the stress is equal to or lower than the compressive strength of the material, On the contrary, the stress due to the Poisson effect is generated on the inner wall of the cylinder, and the stress corresponding to the Poisson effect is also generated on the outer wall of the cylinder. In the present invention, the latter stress acts as a tightening margin of the pressure vessel with respect to the outer wall of the cylinder, and an effect equivalent to preloading the inner wall of the cylinder is obtained. Due to these two effects, in the device of the present invention, the upper limit value of the generated pressure is dramatically increased as compared with the conventional device, and is 55 kb.
Even in the method of use that generates the pressure necessary for synthesizing diamond to a certain degree, the relative pressure burden is small, so the life of the device is dramatically increased. In the present invention, for example, when carrying out a diamond synthesis reaction, 55 kb is added to the cylinder.
Pressure is applied. The cylinder material is 15
In addition to the% Co-WC alloy, use of die steel, high speed steel, etc. is considered.
【０００７】本発明の実施にあたっては、シリンダーの
材質により、例えばダイス鋼の場合には２５ｋｂに相当
する応力が、高速度鋼の場合には３２ｋｂに相当する応
力が、１５％Ｃｏ−ＷＣ合金の場合４０ｋｂに相当する
応力を限度としてシリンダー上下両端面全面に応力が加
えられる。In practicing the present invention, depending on the material of the cylinder, for example, the stress corresponding to 25 kb in the case of die steel and the stress corresponding to 32 kb in the case of high speed steel are the same as those of 15% Co-WC alloy. In this case, stress is applied to the entire upper and lower end surfaces of the cylinder with the stress corresponding to 40 kb being the limit.
【０００８】例えばシリンダー材料としてダイス鋼を使
用した場合について述べる。ダイス鋼の強度値としては
引張が１７５ｋｇ／ｍｍ２、圧縮が２５０ｋｇ／ｍｍ２
として示されている。。このシリンダー内壁面におい
て、圧縮強度の２５０ｋｇ／ｍｍ２いっぱいの予加圧が
加えられるように、締付けリングよりなる外部の圧力容
器によって締付けを行った場合、このシリンダーがポア
ソン効果により横割れが生じないとすれば、約４２ｋｂ
までの高圧力が発生可能な超高圧装置となる。For example, the case where die steel is used as the cylinder material will be described. As the strength value of the die steel, tensile is 175 kg / mm 2 and compression is 250 kg / mm 2.
As shown. . When the inner wall surface of this cylinder is tightened by an external pressure vessel consisting of a tightening ring so that a preload of 250 kg / mm 2 of compressive strength is applied, this cylinder does not cause lateral cracking due to the Poisson effect. If so, about 42 kb
It becomes an ultra-high pressure device that can generate high pressure up to.
【０００９】今シリンダーがダイス鋼の場合２５ｋｂの
応力が加えられると、ダイス鋼のポアソン比は０．３で
あるので、シリンダー内外面には７．５ｋｂに相当する
応力が発生し、外面に生じる応力は、シリンダーが外側
の圧力容器によって拘束されているので締め代となり、
シリンダー内壁に対し約６．６ｋｂに相当する予加圧を
与える。このためこのシリンダーには４２ｋｂ＋７．５
ｋｂ＋６．６ｋｂの内方に向かう応力が与えられること
となり、結局５６ｋｂの圧力に耐える装置となり、ダイ
ヤモンド合成可能な装置となる。When a stress of 25 kb is applied to the cylinder of die steel, the Poisson's ratio of the die steel is 0.3, so a stress equivalent to 7.5 kb is generated on the inner and outer surfaces of the cylinder and is generated on the outer surface. The stress is a tightening margin because the cylinder is restrained by the outer pressure vessel,
A preload of about 6.6 kb is applied to the inner wall of the cylinder. For this reason, this cylinder has 42 kb + 7.5
An inward stress of kb + 6.6 kb is applied, and the device eventually withstands a pressure of 56 kb, which makes it possible to synthesize diamond.
【００１０】同様に、高速度鋼の場合には７０ｋｂ、１
５％Ｃｏ−ＷＣ合金の場合には７３ｋｂの耐圧が得られ
ることになる。Similarly, for high speed steel, 70 kb, 1
With a 5% Co-WC alloy, a breakdown voltage of 73 kb can be obtained.
【００１１】本発明の超高圧高温装置のシリンダー内壁
の反応加熱部より長い部分にセラミック製のスリーブを
挿入する場合は、このシリンダー耐圧限が更に増大す
る。使用されるセラミックにはアルミナ、マグネシア、
ジルコニア、フォルステライト、スピネル、蝋石等が挙
げられる。When a ceramic sleeve is inserted into a portion of the inner wall of the cylinder of the ultrahigh pressure and high temperature apparatus of the present invention which is longer than the reaction heating portion, the cylinder pressure limit is further increased. The ceramics used are alumina, magnesia,
Examples include zirconia, forsterite, spinel, and rouxite.
【００１２】またセラミックの厚みとしては、その断面
積はシリンダー内径の断面積の１／２程度にとるのが好
適である。このスリーブの減衰効果としてはシリンダー
内壁を例えば１００ｍｍ、スリーブの内径を７５ｍｍに
した場合、反応室内に５５ｋｂの圧力を加えると、スリ
ーブはその厚みによりラメ（Ｌａｍｅ）の式に従ってそ
の圧力は減衰され、スリーブの外壁、即ちシリンダー内
壁には約３５ｋｂの圧力がかかるにすぎなくなるため、
このシリンダーの耐用回数は更に増大する。As for the thickness of the ceramic, it is preferable that the cross-sectional area thereof is about 1/2 of the cross-sectional area of the inner diameter of the cylinder. As for the damping effect of this sleeve, when the inner wall of the cylinder is 100 mm and the inner diameter of the sleeve is 75 mm, and when a pressure of 55 kb is applied to the reaction chamber, the pressure of the sleeve is damped according to the Lame equation due to its thickness. Since only about 35 kb of pressure is applied to the outer wall of the sleeve, that is, the inner wall of the cylinder,
The service life of this cylinder is further increased.
【００１３】[0013]
【実施例１】外径２６４ｍｍ、内径５０ｍｍ、長さ１５
０ｍｍのＳＫＤ−１１種ダイス鋼（ＨＲＣ５８）製シリ
ンダーを、外周ヘの線巻きにより補強した外径７５０ｍ
ｍ、内径２８０ｍｍの締付けリング内に、シリンダー内
面における応力が２５０ｋｇ／ｍｍ２になるように、圧
入した。これをプレス装置に装着し、約１０５０トンの
プレス荷重を用いてシリンダー内の試料を圧搾すると共
に、シリンダーの上下端面を、端面全面に接し、ピスト
ンと同期して独立に駆動される、高速度鋼製リングを介
して１３０００トンのプレス荷重を加えることにより、
シリンダーの補強を行った。この装置を用い、５４ｋｂ
の圧力を発生させてダイヤモンドの合成反応を行った。
このダイス鋼製の装置は、比較的低強度の材料で構成さ
れているにもかかわらず、５００回以上の反復使用に耐
えた。Example 1 Outer diameter 264 mm, inner diameter 50 mm, length 15
An outer diameter of 750 m in which a cylinder made of 0 mm SKD-11 type die steel (HRC58) is reinforced by wire winding on the outer circumference.
m and an inner diameter of 280 mm were press-fitted so that the stress on the inner surface of the cylinder was 250 kg / mm 2 . This was installed in a press machine, the sample in the cylinder was squeezed using a press load of about 1050 tons, the upper and lower end surfaces of the cylinder were in contact with the entire end surface, and they were driven independently in synchronization with the piston. By applying a pressing load of 13000 tons through the steel ring,
The cylinder was reinforced. 54 kb using this device
The pressure was generated to cause the synthetic reaction of diamond.
This die steel apparatus, despite being constructed of a relatively low strength material, survived over 500 repeated uses.
【００１４】上記実施例においてはシリンダー上下端面
の加圧はピストンの進行と同期して行ったが、荷重が小
さい間は非同期的に行ってもさしつかえない。In the above embodiment, the pressurization of the upper and lower end surfaces of the cylinder is performed in synchronism with the progress of the piston, but it may be applied asynchronously while the load is small.
【００１５】[0015]
【発明の効果】以上詳述したように、本発明装置におい
ては、超高圧発生時にシリンダー内壁に加わる応力を打
消す作用が得られるので、シリンダーの耐用回数は著し
く増大し、装置の大型化が可能になり、経済的にダイヤ
モンドと立方晶窒化硼素の合成・育成・これらの焼結体
の製造が可能になった。As described above in detail, in the apparatus of the present invention, the effect of canceling the stress applied to the inner wall of the cylinder when an ultrahigh pressure is generated can be obtained, so that the life of the cylinder is remarkably increased and the apparatus becomes large in size. It has become possible and economically possible to synthesize and grow diamond and cubic boron nitride and to manufacture sintered bodies thereof.
Claims (5)
に整列配置された筒状内壁を有するシリンダーを有し、
少なくとも一方のピストンの進行によりシリンダー内壁
内に超高圧力を発生させ、また高温を発生させる超高圧
高温装置において、このシリンダーに軸方向の圧縮応力
を付加し、この際圧縮応力を、超高圧の発生に伴いシリ
ンダー材質のポアソン比に応じて発生する軸方向応力以
上で、かつこの材質の強度以下に設定したことを特徴と
する超高圧高温装置。1. A cylinder having a pair of opposed pistons and a cylindrical inner wall aligned between the pistons,
In an ultrahigh-pressure high-temperature device that generates ultrahigh pressure in the cylinder inner wall by advancing at least one piston and also produces high temperature, an axial compressive stress is applied to this cylinder, in which case the compressive stress is An ultrahigh-pressure high-temperature device characterized in that the stress is set to be not less than the axial stress generated according to the Poisson's ratio of the cylinder material and less than the strength of this material.
て、軸方向の圧縮応力をこのシリンダーの全水平断面に
付加するようにした装置。2. The ultrahigh pressure and high temperature apparatus according to claim 1, wherein an axial compressive stress is applied to the entire horizontal cross section of the cylinder.
て、軸方向の圧縮応力をこのシリンダーの水平断面内方
に部分的に付加するようにした装置。3. The ultrahigh pressure and high temperature apparatus according to claim 1, wherein the compressive stress in the axial direction is partially applied to the inside of the horizontal section of the cylinder.
て、軸方向の圧縮応力をこのシリンダーの水平断面外方
に部分的に付加するようにした装置。4. The ultrahigh pressure high temperature apparatus according to claim 1, wherein an axial compressive stress is partially applied to the outside of the horizontal section of the cylinder.
て、上記シリンダー内壁の最高温に供される部分および
その近傍にセラミック製のスリーブを密着配置したこと
を特徴とする装置。5. The apparatus according to claim 1, wherein a ceramic sleeve is disposed in close contact with a portion of the inner wall of the cylinder subjected to the maximum temperature and in the vicinity thereof.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33751891A JPH0699052A (en) | 1991-10-21 | 1991-10-21 | Ultra-high pressure and high temperature device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33751891A JPH0699052A (en) | 1991-10-21 | 1991-10-21 | Ultra-high pressure and high temperature device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0699052A true JPH0699052A (en) | 1994-04-12 |
Family
ID=18309412
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33751891A Pending JPH0699052A (en) | 1991-10-21 | 1991-10-21 | Ultra-high pressure and high temperature device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0699052A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102580619A (en) * | 2012-03-06 | 2012-07-18 | 河南飞孟金刚石工业有限公司 | Hinge sleeve for cubic presses and manufacturing method thereof |
-
1991
- 1991-10-21 JP JP33751891A patent/JPH0699052A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102580619A (en) * | 2012-03-06 | 2012-07-18 | 河南飞孟金刚石工业有限公司 | Hinge sleeve for cubic presses and manufacturing method thereof |
| CN102580619B (en) * | 2012-03-06 | 2013-12-18 | 河南飞孟金刚石工业有限公司 | Hinge sleeve for cubic presses and manufacturing method thereof |
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