JPH0135798B2 - - Google Patents
Info
- Publication number
- JPH0135798B2 JPH0135798B2 JP57183959A JP18395982A JPH0135798B2 JP H0135798 B2 JPH0135798 B2 JP H0135798B2 JP 57183959 A JP57183959 A JP 57183959A JP 18395982 A JP18395982 A JP 18395982A JP H0135798 B2 JPH0135798 B2 JP H0135798B2
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- crystal
- concave mirror
- crystal raw
- laser beam
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/005—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method by irradiation or electric discharge
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/121—Coherent waves, e.g. laser beams
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Optics & Photonics (AREA)
- Electromagnetism (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Carbon And Carbon Compounds (AREA)
Description
【発明の詳細な説明】
産業上の利用分野
本発明は結晶製造方法に関するものであり、結
晶体を人工的に製造する場合に、超高温、高圧条
件を必要とするような物質、例えば、ダイヤモン
ド等の宝石や金属結晶等を低コストに製造する方
法を提供するものである。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for manufacturing crystals, and when artificially manufacturing crystals, materials such as those that require ultra-high temperature and high pressure conditions, such as diamond, are used. The present invention provides a method for manufacturing gemstones, metal crystals, etc. at low cost.
従来例の構成と問題点
本発明者が以前特願昭57−63744号にて提案し
た外包材料及びレーザーを用いた結晶製造方法で
は、第1図に示すように結晶原材料1を包むよう
に外包材料2となる透明材料の球体((例えば石英
やガラス等))に封入し、外部より集光したレーザ
ー光3を照射し、核となつている結晶原材料1を
主として加熱、溶融させて、冷却後、外包材料を
除去して結晶を取り出す方法が用いられていた
が、この方法では結晶原材料1を高温にすればす
る程結晶原材料より熱線4として放出される輻射
エネルギーが大きくなる。すなわち、エネルギー
ロスが大きくなる欠点があつた。Structure and Problems of Conventional Example In the crystal manufacturing method using an outer packaging material and a laser, which the present inventor previously proposed in Japanese Patent Application No. 57-63744, as shown in FIG. 2 is sealed in a sphere of transparent material (such as quartz or glass), and irradiated with a laser beam 3 focused from the outside to mainly heat and melt the crystal raw material 1, which is the core, and after cooling. In this method, the higher the temperature of the crystal raw material 1, the greater the radiant energy emitted from the crystal raw material as heat rays 4. In other words, there was a drawback that energy loss was large.
例えば、ダイヤモンドを製造する場合には、触
媒を用いない場合、30万気圧、3000〓程度の条件
を必要とするが、グラフアイト10gを結晶原材料
として用いた場合、パワー約10KWのYAGレー
ザーを必要とした。これは、3000〓ともなると、
熱輻射が、460W/cm2にもなるためである。つま
り、レーザー照射の大部分は、結晶原材料より放
出される輻射熱としてむだになつてしまつてい
た。 For example, when producing diamond, if a catalyst is not used, conditions of about 300,000 atm and 3,000 〓 are required, but if 10 g of graphite is used as the crystal raw material, a YAG laser with a power of about 10 KW is required. And so. This becomes 3000〓,
This is because the thermal radiation is as high as 460W/cm 2 . In other words, most of the laser irradiation was wasted as radiant heat emitted from the crystal raw material.
発明の目的
以上述べて来た先に提案した方法の欠点に鑑
み、本発明の目的は、結晶原材料加熱時の輻射に
よるエネルギーロスを少くし、低パワーのレーザ
ーで高効率に結晶原材料を溶融することを目的と
する。Purpose of the Invention In view of the drawbacks of the previously proposed methods described above, the purpose of the present invention is to reduce the energy loss due to radiation during heating of the crystalline raw material and to melt the crystalline raw material with high efficiency using a low-power laser. The purpose is to
発明の構成
本発明は、人造結晶を製造する方法であり、あ
らかじめ、結晶原材料および前記結晶原材料を包
囲する光学的に透明な外包材料よりなる球体を、
所定の間隔で窓を設けた凹面鏡で包囲し、前記窓
よりレーザー光を照射することにより、加熱昇温
された結晶原材料から輻射熱として放出される熱
線を、再び凹面鏡で集光して結晶原料を照射する
こと、さらに好ましくは前記凹面鏡と外包材料の
間隙に冷却ガスを流すことにより、外包材料表面
及び凹面鏡の昇温を防止することを特徴とするも
のである。Structure of the Invention The present invention is a method for manufacturing an artificial crystal, in which a sphere made of a crystal raw material and an optically transparent outer envelope material surrounding the crystal raw material is prepared in advance.
The crystal raw material is surrounded by a concave mirror with windows at predetermined intervals, and by irradiating laser light from the window, the heated rays emitted as radiant heat from the heated crystal raw material are focused again by the concave mirror, and the crystal raw material is The present invention is characterized in that the surface of the outer envelope material and the concave mirror are prevented from increasing in temperature by irradiating the mirror, and more preferably by flowing a cooling gas into the gap between the concave mirror and the outer envelope material.
実施例の説明
以下、実施例を第2図を用いて詳細に説明す
る。あらかじめ、結晶原材料1を包囲するよう
に、ガラス等の透明物質よりなる外包材料2で封
入された球体を、所定の間隔で窓5を設けた凹面
鏡6で包み込み、窓5よりレーザー光3を照射
し、核となつている結晶原材料を加熱溶融させ
た。このとき、結晶原材料1の昇温に伴い、球体
外部へ熱線4として放出される輻射熱は、前記凹
面鏡で大部分内部に向つて反射され、再び結晶原
材料に集光された。従つて、本発明の方法を用い
ると、球体外部へ放出されるエネルギーロスがほ
とんど無いため、レーザー光のパワーを大幅に削
減できた。次にレーザー光の照射を停止し、冷却
すると、原材料は、高温、高圧下で徐冷されるこ
とになり、ダイヤモンドの結晶が形成される。な
お、このとき、外包材料は、熱線をほとんで吸収
せず、主として昇温された結晶原材料との接触に
よる熱伝導で昇温する程度であり、短時間(数秒
間)の場合には、外面はほと昇温しなかつた。ま
た、凹面鏡は熱線をほとんど反射するため、これ
また、あまり昇温することがなかつた。なお、長
時間のレーザー照射を必要とする場合には、どう
しても外包体材料表面及び凹面鏡を昇温してくる
ので、その場合には、外包体材料と凹面鏡の間隙
に冷却ガスを流すことにより、昇温を防止するこ
とができた。DESCRIPTION OF EMBODIMENTS An example will be described in detail below with reference to FIG. In advance, a sphere encapsulated with an outer packaging material 2 made of a transparent material such as glass so as to surround the crystal raw material 1 is wrapped with a concave mirror 6 provided with windows 5 at predetermined intervals, and a laser beam 3 is irradiated through the windows 5. Then, the core crystal raw material was heated and melted. At this time, as the temperature of the crystal raw material 1 increases, the radiant heat emitted to the outside of the sphere as heat rays 4 is mostly reflected inward by the concave mirror and is again focused on the crystal raw material. Therefore, when the method of the present invention is used, there is almost no energy loss emitted to the outside of the sphere, so the power of the laser beam can be significantly reduced. Next, when the laser beam irradiation is stopped and the material is cooled, the raw material is slowly cooled at high temperature and pressure, and diamond crystals are formed. In addition, at this time, the outer packaging material hardly absorbs the heat rays, and the temperature rises mainly due to heat conduction due to contact with the heated crystal raw material, and in the case of a short time (several seconds), the outer surface The temperature did not rise at all. Also, since the concave mirror reflects most of the heat rays, the temperature did not rise much. If long-term laser irradiation is required, the surface of the outer envelope material and the concave mirror will inevitably rise in temperature, so in that case, by flowing cooling gas into the gap between the outer envelope material and the concave mirror, It was possible to prevent temperature rise.
例えば、ダイヤモンドを製造する場合には、触
媒を用いない場合、30万気圧、3000〓程度の条件
を必要とするが、まず、原材料1として球状に加
圧成形したグラフアイト10gを粉末ガラス例えば
コーニンググラス社のパイリツクス7740で被覆
し、全体を加熱して外包材料となる前記ガラス粉
末を溶融・硬化して、内部にグラフアイトを核と
する透明ガラス球体を形成した。あるいはあらか
じめ、溶融したガラス中にグラフアイトを挿入し
て、徐冷硬化させても良い。なお、このとき、グ
ラフアイト核の直径はおよそ2cmとなるので、透
明ガラスよりなる外包体の直径を20cm以上にし
た。次に、この球体に凹面鏡をかぶせ、窓よりパ
ワー1〜2KWのYAGレーザーを照射すると、数
十ミリ秒から数百ミリ秒でグラフアイトは3000℃
以上になり、溶融された。なお、このとき、外包
材料はガラスでできており、、熱伝導が悪く、数
秒程度では球体外部は熱膨張は生じず、その結果
グラフアイトは高温、高圧で保持されることにな
る。また、外包体のガラスも破損しなかつた。こ
れは、グラフアイト直径2cmに対し、ガラス直径
を20cm以上((約10倍))にしたため、内部圧が50万
気圧になつても、ガラス表面にかかる圧力は、
5000気圧程度となり、ガラスのヤング率6〜8×
103Kg/cm2を考慮すると、ガラスが破壊されるこ
とはなかつたことがわかる。その後、レーザー照
射を停止して、放置すれば、球体は外部より冷却
され溶融結晶原材料は高圧に保持された状態で冷
却された結果、粒径1μm程度のダイヤモンド粉
末結晶が得られた。ここで、ダイヤモンドが生成
されたことは、表面研磨されたサフアイヤ基板に
押しつけてこすると、サフアイア基板が傷つくこ
とで確認された。 For example, when manufacturing diamonds, conditions of about 300,000 atm and 3,000 m are required without using a catalyst. It was coated with Pyrix 7740 manufactured by Glass Co., Ltd., and the whole was heated to melt and harden the glass powder serving as the outer packaging material, thereby forming a transparent glass sphere with graphite as the core inside. Alternatively, graphite may be inserted into molten glass in advance and slowly cooled to harden. At this time, the diameter of the graphite core was approximately 2 cm, so the diameter of the outer envelope made of transparent glass was set to 20 cm or more. Next, we cover this sphere with a concave mirror, and when we irradiate a YAG laser with a power of 1 to 2 KW through the window, the graphite heats up to 3000 degrees Celsius in a few tens of milliseconds to a few hundred milliseconds.
It became more than that and was melted. At this time, the outer packaging material is made of glass, which has poor thermal conductivity, and no thermal expansion occurs on the outside of the sphere for about a few seconds, resulting in the graphite being held at high temperature and high pressure. Moreover, the glass of the outer package was not damaged. This is because the glass diameter is 20 cm or more ((approximately 10 times)) compared to the graphite diameter of 2 cm, so even if the internal pressure is 500,000 atm, the pressure applied to the glass surface is
It is about 5000 atmospheres, and the Young's modulus of glass is 6 to 8×
Considering 10 3 Kg/cm 2 , it can be seen that the glass was not destroyed. After that, the laser irradiation was stopped and the sphere was allowed to stand, and the sphere was cooled from the outside, and the molten crystal raw material was cooled while being held at high pressure, resulting in diamond powder crystals with a particle size of about 1 μm. Here, the generation of diamond was confirmed by the fact that the sapphire substrate was scratched when pressed and rubbed against the surface-polished sapphire substrate.
なお、本実施例では、レーザー光3を2方向か
ら照射している図を示したが、これは一方向から
でも良いし、もつと多くのレーザー光を照射して
も良いことは明らかである。 Although this embodiment shows the laser beam 3 being irradiated from two directions, it is clear that the laser beam 3 may be irradiated from one direction or a large number of laser beams may be irradiated. .
発明の効果
本発明の方法を用いることにより、結晶の製造
におけるエネルギーロスを大幅に低減できるの
で、レーザーを小型化でき、エネルギー効率を向
上することができる。また、レーザー照射時間を
長くする必要がある場合でも、外包材料表面及び
凹面鏡を容易に冷却することができる。Effects of the Invention By using the method of the present invention, energy loss in crystal production can be significantly reduced, so the laser can be downsized and energy efficiency can be improved. Further, even if it is necessary to increase the laser irradiation time, the surface of the outer packaging material and the concave mirror can be easily cooled.
第1図は本発明者が以前提案したレーザーを用
いた結晶製造方法を説明するための概略図、第2
図は本発明の一実施例にかかる窓付き凹面鏡を用
いた結晶製造方法を説明するための概略断面構成
図である。
1……結晶原材料、2……外包体材料、3……
レーザー、4……熱線、5……窓、6……凹面
鏡。
Figure 1 is a schematic diagram for explaining the crystal manufacturing method using a laser previously proposed by the present inventor;
The figure is a schematic cross-sectional configuration diagram for explaining a crystal manufacturing method using a windowed concave mirror according to an embodiment of the present invention. 1...Crystal raw material, 2...Outer envelope material, 3...
Laser, 4...heat ray, 5...window, 6...concave mirror.
Claims (1)
光学的に透明な外包材料よりなる球体を、所定の
間隔で窓を設けた凹面鏡で包囲し、前記窓より入
射させたレーザー光および前記レーザー光の前記
凹面鏡からの反射光を前記外包材料にて集光して
前記結晶材料に照射して、前記結晶原材料を加
熱、溶融、冷却することを特徴とした結晶製造方
法。 2 凹面鏡と外包材料の間隙に冷却ガスを流すこ
とを特徴とした特許請求の範囲第1項に記載の結
晶製造方法。[Scope of Claims] 1. A sphere made of a crystal raw material and an optically transparent outer covering material surrounding the crystal raw material is surrounded by a concave mirror provided with windows at predetermined intervals, and a laser beam and a laser beam incident through the windows are surrounded. A crystal manufacturing method comprising: heating, melting, and cooling the crystal raw material by condensing the reflected light of the laser beam from the concave mirror on the outer packaging material and irradiating the crystal material. 2. The crystal manufacturing method according to claim 1, characterized in that cooling gas is caused to flow through the gap between the concave mirror and the outer packaging material.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57183959A JPS5973490A (en) | 1982-10-19 | 1982-10-19 | Crystal manufacturing method |
| US06/485,506 US4522680A (en) | 1982-04-15 | 1983-04-15 | Method for producing crystals |
| EP83302154A EP0092405B1 (en) | 1982-04-15 | 1983-04-15 | Method for producing crystals |
| DE8383302154T DE3364653D1 (en) | 1982-04-15 | 1983-04-15 | Method for producing crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57183959A JPS5973490A (en) | 1982-10-19 | 1982-10-19 | Crystal manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5973490A JPS5973490A (en) | 1984-04-25 |
| JPH0135798B2 true JPH0135798B2 (en) | 1989-07-27 |
Family
ID=16144808
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57183959A Granted JPS5973490A (en) | 1982-04-15 | 1982-10-19 | Crystal manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5973490A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS623095A (en) * | 1985-06-07 | 1987-01-09 | モリソン・パンプス・エスエイ・(プロプライアタリ−)・リミテツド | Crystal growth |
| JPH01294599A (en) * | 1988-05-20 | 1989-11-28 | Honda Motor Co Ltd | Diamond synthesis method |
| JP2600833B2 (en) * | 1988-08-18 | 1997-04-16 | 三菱マテリアル株式会社 | Manufacturing method of artificial diamond powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5511605A (en) * | 1978-07-11 | 1980-01-26 | Tamura Electric Works Ltd | Regeneration system for intermediate gradation |
-
1982
- 1982-10-19 JP JP57183959A patent/JPS5973490A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5973490A (en) | 1984-04-25 |
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