JPS63158126A - Diamond synthesis - Google Patents
Diamond synthesisInfo
- Publication number
- JPS63158126A JPS63158126A JP30610186A JP30610186A JPS63158126A JP S63158126 A JPS63158126 A JP S63158126A JP 30610186 A JP30610186 A JP 30610186A JP 30610186 A JP30610186 A JP 30610186A JP S63158126 A JPS63158126 A JP S63158126A
- Authority
- JP
- Japan
- Prior art keywords
- convertible
- diamond
- carbon
- plate
- sample
- 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
- 239000010432 diamond Substances 0.000 title claims abstract description 39
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 33
- 230000015572 biosynthetic process Effects 0.000 title abstract description 3
- 238000003786 synthesis reaction Methods 0.000 title description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 7
- 239000000956 alloy Substances 0.000 claims abstract description 6
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 6
- 239000007849 furan resin Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 9
- 230000005611 electricity Effects 0.000 claims description 3
- 238000001308 synthesis method Methods 0.000 claims description 3
- 238000010030 laminating Methods 0.000 abstract 1
- 150000002739 metals Chemical class 0.000 abstract 1
- 238000007669 thermal treatment Methods 0.000 abstract 1
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 230000002093 peripheral effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910000833 kovar Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011271 tar pitch Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0605—Composition of the material to be processed
- B01J2203/061—Graphite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/0655—Diamond
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0675—Structural or physico-chemical features of the materials processed
- B01J2203/068—Crystal growth
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明はダイヤモンドの合成方法、更に詳しくドを合成
する方法の改良に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for synthesizing diamond, and more particularly to an improvement in a method for synthesizing diamond.
従来技術
ダイヤモンドに変換する変換性黒鉛板と触媒金属を積層
した試料にダイヤモンド安定領域の超高圧と温度を加え
ダイヤモンドを合成する方法はよく知られている。PRIOR ART The method of synthesizing diamond by applying ultra-high pressure and temperature in the diamond stable region to a sample in which a convertible graphite plate and a catalyst metal are layered is well known.
試料を加熱する方法としては、試料と電気的に絶縁され
た管状ヒーターに電流を通ずる間接加熱法と、試料に直
接電流を通じて加熱する直接加熱法とがある。本発明は
後者の直接加熱法に関する。Methods for heating a sample include an indirect heating method in which a current is passed through a tubular heater that is electrically insulated from the sample, and a direct heating method in which a current is passed directly through the sample to heat it. The present invention relates to the latter direct heating method.
直接加熱法は間接加熱法に比べ、反応室容積を大きくで
きる点で非常に有利である。しかしその反た試料に通電
すると、反応室の中心部に優先的に電流が流れ、また、
黒鉛は高圧下では高温になるにつれて低抵抗になる性質
があるため、昇温に伴ダイヤモンドの生成に伴い溶融触
媒金属が黒鉛中に浸入し、第３図及び第４図に示すよう
な溶融金属とダイヤモンドの混合したプリフジ部へを形
成し、低抵抗部分を作り、従って、ダイヤモンドは中心
部だけに集中的に生成する。The direct heating method is very advantageous over the indirect heating method in that the volume of the reaction chamber can be increased. However, when electricity is applied to the curved sample, the current flows preferentially to the center of the reaction chamber, and
Graphite has the property of becoming lower in resistance as the temperature increases under high pressure, so as the temperature rises, molten catalyst metal penetrates into graphite as diamonds are formed, resulting in molten metal as shown in Figures 3 and 4. A mixture of diamond and diamond is formed in the pre-fuji part, creating a low resistance part, and therefore, diamond is generated concentrated only in the center part.
また、加熱温度をさらに高温にすると、中心部に黒鉛が
晶出し、その周囲にダイヤモンドが生成する。Furthermore, when the heating temperature is raised even higher, graphite crystallizes in the center and diamond forms around it.
これらのいずれの方法においても、原料黒鉛からのダイ
ヤモンドへの変換率は低い。In any of these methods, the conversion rate of raw graphite to diamond is low.
その上帯られるダイヤモンドの外形は不規則となり、良
好な平坦な結晶面で構成された６−８面体のダイヤモン
ドは得難く、仮に一部良質なものが生成されたとしても
その収率は極めて少ない欠点があった。Moreover, the outer shape of the banded diamonds becomes irregular, making it difficult to obtain hex-octahedral diamonds composed of good flat crystal planes, and even if some good quality diamonds are produced, the yield is extremely low. There were drawbacks.
発明の目的
本発明は従来法の欠点を改善すべくなされたもので、そ
の目的は中央部分及び周辺部にも均一に良質なダイヤモ
ンドを生成するダイヤモンドの合成方法を提供するにあ
る。OBJECTS OF THE INVENTION The present invention has been made to improve the drawbacks of the conventional methods, and its purpose is to provide a diamond synthesis method that produces diamonds of good quality uniformly in the central and peripheral areas.
発明の構成
本発明者らは前記目的を達成すべく研究の結果、フラン
樹脂を１３００℃以下で熱処理して得た炭素、また８０
０℃以上の熱処理を施さない炭素は通常のダイヤモンド
合成領域の温度、圧力では全くダイヤモンドを生成せず
、また溶融触媒金属も浸入しない。このような非変換性
炭素を変換性黒鉛板の中間に置いて、超高圧下で加熱し
てダイヤモンドを合成すると、中央部分及び周辺部分も
均一に加熱でき、かつ溶融触媒金属と黒鉛からなるブリ
ッジも生成しないで、良質なダイヤモンドを変換率よく
生成し得られることを究明し得た。この知見に基づいて
本発明を完成した。Structure of the Invention As a result of research to achieve the above object, the present inventors found that carbon obtained by heat-treating furan resin at 1300°C or less, and 80%
Carbon that has not been heat-treated above 0° C. does not produce diamond at all at the temperature and pressure in the normal diamond synthesis region, and does not penetrate molten catalyst metal. If such non-convertible carbon is placed in the middle of a convertible graphite plate and heated under ultra-high pressure to synthesize diamond, the central and peripheral parts can be heated evenly, and a bridge made of molten catalyst metal and graphite can be synthesized. It has been found that high-quality diamond can be produced at a high conversion rate without producing diamond. The present invention was completed based on this knowledge.
本発明の要旨は
ダイヤモンドに変換する変換性黒鉛板と触媒金属板を層
状に積層した試料に超高圧を加え、直接通電して加熱し
ダイヤモンドを合成する方法において、変換性黒鉛板の
中間に非変換性炭素板を置いて合成することを特゛徴と
するダイヤモンドの合成法にある。The gist of the present invention is to synthesize diamond by applying ultra-high pressure to a sample in which a convertible graphite plate and a catalytic metal plate are laminated in layers to convert into diamond, and directly applying electricity to heat the sample. The method of synthesizing diamond is characterized by placing a convertible carbon plate and synthesizing it.
本発明の方法における試料構成の例を示すと第１図の通
りである。第１図は変換性黒鉛板の中間に非変換性炭素
板を配置した例である。図中１は圧力媒体である食塩円
筒、２は触媒金属板、３は変換性黒鉛板、４は非変換性
炭素板を示す。An example of the sample structure in the method of the present invention is shown in FIG. 1. FIG. 1 shows an example in which a non-convertible carbon plate is placed between convertible graphite plates. In the figure, 1 is a salt cylinder which is a pressure medium, 2 is a catalyst metal plate, 3 is a convertible graphite plate, and 4 is a non-convertible carbon plate.
非変換性炭素としては、例えばフラン樹脂を１３００℃
以下で熱処理して生成した炭素、または８００℃以上の
熱処理を施さないカーボンが挙げられる。また触媒金属
としては、Ｆｅ、 Ｎｉ、 Ｃｏまたはそれらの合金が
挙げられる。As non-convertible carbon, for example, furan resin is heated at 1300°C.
Examples include carbon produced by heat treatment described below, and carbon that is not heat treated at 800° C. or higher. Further, examples of the catalytic metal include Fe, Ni, Co, and alloys thereof.
本発明の方法においては、非変換性炭素層においては、
溶融触媒金属と全く反応しないので、低電気抵抗のブリ
フジ部が形成せず、電流密度が均等化するため径方向の
温度分布が著しく小さくなる。In the method of the present invention, in the non-convertible carbon layer,
Since it does not react with the molten catalyst metal at all, no bridging portion with low electrical resistance is formed, and the current density is equalized, resulting in a significantly small radial temperature distribution.
実施例１゜
第１図に示す試料配置とし、変換性黒鉛板（直径８鰭、
厚さ１．５ ｗｍ）を用い、非変換性炭素板として、フ
ルフリルアルコールを硝酸触媒で脱水縮合し、８００℃
で熱処理して得た炭素を直径８１１、厚さ０．５０に加
工した板を用いた。また触媒金属としてコバール合金（
Ｎｉ２９％、 Ｃｏ１９％、 Ｆｅ５２％の合金）板を
使用し、内径２５ｍのベルト型高圧装置で５．８ ＧＰ
ａで５分間、加熱電力２．２ ｋＷで加熱した。Example 1 The sample arrangement was as shown in Figure 1, and a convertible graphite plate (8 fins in diameter,
As a non-convertible carbon plate, furfuryl alcohol was dehydrated and condensed using a nitric acid catalyst and heated to 800°C.
A plate made of carbon heat-treated to have a diameter of 811 mm and a thickness of 0.50 mm was used. Kovar alloy (
5.8 GP using a belt-type high-pressure device with an inner diameter of 25 m using an alloy (alloy of 29% Ni, 19% Co, 52% Fe)
Heating was performed for 5 minutes at a heating power of 2.2 kW.
ダイヤモンドの収率は２６．５！！ｉｉであった。The diamond yield is 26.5! ! It was ii.
実施例２゜
実施例１と同様な試料構成で同じ処理圧力を採用し、非
変換性炭素板の種類、加熱電力を変えダイヤモンドを合
成した。その結果は次の通りであった。Example 2 Diamond was synthesized using the same sample structure and the same processing pressure as in Example 1, but by changing the type of non-convertible carbon plate and heating power. The results were as follows.
カーボン 〃２．２ ｋＷ ２０．７％カ
ーボン 〃２．４に切 ５３．０％（註）
（１）フルフリルアルコール由来炭素は実施例１による
ものと同じ。Carbon 〃2.2 kW 20.7% Carbon 〃Cut to 2.4 53.0% (Note)
(1) Furfuryl alcohol-derived carbon is the same as in Example 1.
（２）カーボンは石油タールピッチ結合剤を用いた低結
晶質カーボンである。(2) Carbon is low crystalline carbon with petroleum tar pitch binder.
比較例１゜
黒鉛板を２Ｎ厚とし、実施例１と同様な触媒金属板を用
い、非変換性炭素板を置かないで、５．８ＧＰａ 、
２．４ ｋＷ、 ５分間加熱してダイヤモンドを合成
した。ダイヤモンドの収率は８．２％であった。Comparative Example 1 The graphite plate was made 2N thick, the same catalyst metal plate as in Example 1 was used, the non-convertible carbon plate was not placed, and the pressure was 5.8 GPa.
Diamond was synthesized by heating at 2.4 kW for 5 minutes. The diamond yield was 8.2%.
発明の効果
本発明の方法によると、中央部分及び周辺部も均一に加
熱され、良質なダイヤモンドが収率よく生成し得られる
優れた効果を奏し得られる。Effects of the Invention According to the method of the present invention, the center portion and the peripheral portion are also heated uniformly, and high quality diamonds can be produced in a high yield.
第１図は本発明の方法における試料構成図、第２図は従
来法における試料構成図で、第３図及び第４図は従来法
における溶融金属とダイヤモンドの混合したブリッジ部
を示す。
に食塩円筒、
２：触媒金属板、
３：変換性黒鉛板、
４：非変換性炭素板、
５：ブリフジ部分。
第１図 第２図
と
第３図 第４図FIG. 1 is a diagram showing the structure of a sample in the method of the present invention, FIG. 2 is a diagram showing the structure of a sample in the conventional method, and FIGS. 3 and 4 show a bridge portion where molten metal and diamond are mixed in the conventional method. 2: catalyst metal plate, 3: convertible graphite plate, 4: non-convertible carbon plate, 5: brifuge part. Figure 1 Figure 2 and Figure 3 Figure 4
Claims (1)
板を層状に積層した試料に超高圧を加え、直接通電して
加熱しダイヤモンドを合成する方法において、変換性黒
鉛板の中間に非変換性炭素板を置いて合成することを特
徴とするダイヤモンドの合成方法。 ２）、触媒金属がＦｅ、Ｎｉ、Ｃｏまたはそれらの合金
である特許請求の範囲第１項記載のダイヤモンドの合成
方法。 ３）、非変換性炭素がフラン樹脂を１３００℃以下で熱
処理して生成した炭素、または８００℃以上の熱処理を
施さないカーボンである特許請求の範囲第１項記載のダ
イヤモンドの合成方法。[Claims] 1) In a method of synthesizing diamond by applying ultra-high pressure to a sample in which a convertible graphite plate and a catalytic metal plate are laminated in layers to be converted into diamond, and heating the sample by directly applying electricity, A diamond synthesis method characterized by placing a non-convertible carbon plate in the middle of the diamond. 2) The method for synthesizing diamond according to claim 1, wherein the catalyst metal is Fe, Ni, Co, or an alloy thereof. 3) The diamond synthesis method according to claim 1, wherein the non-convertible carbon is carbon produced by heat-treating furan resin at 1300°C or lower, or carbon that is not heat-treated at 800°C or higher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30610186A JPS63158126A (en) | 1986-12-22 | 1986-12-22 | Diamond synthesis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30610186A JPS63158126A (en) | 1986-12-22 | 1986-12-22 | Diamond synthesis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63158126A true JPS63158126A (en) | 1988-07-01 |
| JPH0475766B2 JPH0475766B2 (en) | 1992-12-01 |
Family
ID=17953051
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30610186A Granted JPS63158126A (en) | 1986-12-22 | 1986-12-22 | Diamond synthesis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63158126A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1460040A1 (en) * | 2001-12-28 | 2004-09-22 | Toyo Tanso Co., Ltd. | Graphite material for synthesizing semiconductor diamond and semiconductor diamond produced by using the same |
| CN104607107A (en) * | 2014-05-08 | 2015-05-13 | 长春师范大学 | High-quality diamond synthesized by utilizing artificial graphite and flake graphite at certain temperature and pressure in one step |
| CN106076206A (en) * | 2016-08-24 | 2016-11-09 | 中南钻石有限公司 | A kind of twin diamond and manufacture method thereof |
-
1986
- 1986-12-22 JP JP30610186A patent/JPS63158126A/en active Granted
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1460040A1 (en) * | 2001-12-28 | 2004-09-22 | Toyo Tanso Co., Ltd. | Graphite material for synthesizing semiconductor diamond and semiconductor diamond produced by using the same |
| EP1460040A4 (en) * | 2001-12-28 | 2005-06-08 | Toyo Tanso Co | Graphite material for synthesizing semiconductor diamond and semiconductor diamond produced by using the same |
| KR100742059B1 (en) | 2001-12-28 | 2007-07-23 | 도요탄소 가부시키가이샤 | Graphite material for synthesizing semiconductor diamond and semiconductor diamond produced by using the same |
| CN104607107A (en) * | 2014-05-08 | 2015-05-13 | 长春师范大学 | High-quality diamond synthesized by utilizing artificial graphite and flake graphite at certain temperature and pressure in one step |
| CN106076206A (en) * | 2016-08-24 | 2016-11-09 | 中南钻石有限公司 | A kind of twin diamond and manufacture method thereof |
| CN106076206B (en) * | 2016-08-24 | 2019-01-15 | 中南钻石有限公司 | A kind of twin diamond and its manufacturing method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0475766B2 (en) | 1992-12-01 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |