JPH0751220B2 - Diamond synthesis method - Google Patents
Diamond synthesis methodInfo
- Publication number
- JPH0751220B2 JPH0751220B2 JP2072655A JP7265590A JPH0751220B2 JP H0751220 B2 JPH0751220 B2 JP H0751220B2 JP 2072655 A JP2072655 A JP 2072655A JP 7265590 A JP7265590 A JP 7265590A JP H0751220 B2 JPH0751220 B2 JP H0751220B2
- Authority
- JP
- Japan
- Prior art keywords
- diamond
- explosive
- water
- explosion
- present
- 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 - Lifetime
Links
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
- B01J3/08—Application of shock waves for chemical reactions or for modifying the crystal structure of substances
-
- 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
Description
【発明の詳細な説明】 （産業上の利用分野） 本考案は、ダイヤモンドの爆発合成方法に関するもので
ある。TECHNICAL FIELD The present invention relates to a method for explosive synthesis of diamond.
（従来技術及びその問題点） 爆薬の爆発を利用した従来のダイヤモンドの合成方法に
は、（１）グラファイトに爆発によって加速した物体を
衝突させてグラファイトをダイヤモンドに変換する方法
や、（２）グラファイトを爆薬の爆発で加速し水面等に
衝突させ水中等からダイヤモンド回収する方法、（３）
高性能爆薬とグラファイトの混合物を爆発させてグラフ
ァイトをダイヤモンドに変換する方法等がある。(Prior art and its problems) The conventional method for synthesizing diamond using explosive explosive includes (1) a method of colliding graphite with an object accelerated by the explosion and converting graphite into diamond, and (2) graphite To recover diamonds from underwater, etc. by accelerating blasting with explosives and colliding with water surface, etc. (3)
There is a method to explode a mixture of high explosive and graphite to convert graphite into diamond.
これらの方法のうち、（１）の方法は原料入り容器に爆
薬で加速した物体を衝突させた後、空中または水中でそ
の容器を拾い、容器内からダイヤモンドを回収する方式
であるが、その物体の加速に必要な装置は１回の爆発加
速で破壊される１回作動かぎりのものであり、またその
ダイヤモンドの原料を入れた容器はこの衝突処理により
二度と使用できなくなる。また使用爆薬量もダイヤモン
ドの原料とするグラファイトの数十倍を必要とする。従
って、この方法でダイヤモンドを合成するには多大の労
力と、多量の製造用材料及び爆薬のために費用がかかる
欠点がある。（２）の方法も加速装置の作成に多大な労
力を要し、また１回作動かぎりで破壊してしまうもので
あるので、同様に多大な費用を要する欠点がある。Among these methods, the method (1) is a method in which an object accelerated by an explosive is collided with a container containing raw materials, and then the container is picked up in the air or in water to recover the diamond from the container. The equipment required for accelerating is only one operation which is destroyed by one explosion acceleration, and the container containing the diamond raw material cannot be used again due to this collision treatment. Also, the amount of explosive used is several ten times that of graphite, which is the raw material for diamond. Therefore, synthesizing diamond by this method has the disadvantage of being labor intensive and costly due to the large amount of manufacturing materials and explosives. The method (2) also requires a great deal of labor for producing the accelerator and also destroys it only once, so that it also has a drawback that it requires a great deal of cost.
（３）の方法には、このような１回作動かぎりの装置は
ないが、その代わりに爆発容器を使い、その中で爆薬と
グラファイトの混合物等を爆発させ、爆発容器の内壁等
に付着した生成物をかき集め、これを精製したダイヤモ
ンドを得る方法であるから、爆発容器はその爆発時には
密閉する必要があり、また反応生成物の取り出し等のた
め開閉できるようになっている必要がある。そして爆発
に耐え得る強度が必要であり、また爆発時に反応生成物
が燃焼しないように容器内の空気を不活性なガスで置換
するか、減圧にする必要がある。このように１回の爆発
処理毎に爆発容器の開閉その他の操作を行わねばならな
いので、この方法でも前述の方法と同様に多大な労力を
要しているのが現状である。The method of (3) does not have such a device that can be operated only once, but instead uses an explosive container, in which a mixture of explosive and graphite is detonated and adhered to the inner wall of the explosive container. Since this is a method of collecting the product and obtaining a purified diamond from it, the explosion container must be closed at the time of the explosion, and it must be able to be opened and closed to take out the reaction product. Then, it is necessary to have a strength that can endure the explosion, and it is necessary to replace the air in the container with an inert gas or reduce the pressure so that the reaction products do not burn during the explosion. As described above, since it is necessary to open and close the explosive container and perform other operations for each explosive treatment, this method also requires a great deal of labor in the same manner as the above-mentioned method.
（発明の課題） 本発明は、従来技術に見られる前記問題点を解決し、何
度でも容易に所望回数の爆発を繰返し行うことができ、
かつ反応生成物の回収が容易なダイヤモンドの爆発合成
法を提供し、これによりダイヤモンド合成に要する労力
の低減をはかることをその課題とする。(Problems of the invention) The present invention solves the above-mentioned problems found in the prior art, and it is possible to easily repeat a desired number of explosions any number of times,
Moreover, it is an object of the present invention to provide an explosive synthesis method of diamond in which reaction products can be easily recovered, and thereby to reduce the labor required for diamond synthesis.
（課題を解決するための手段） 本発明者らは、前記課題を解決すべく鋭意研究を重ねた
結果、本発明を完成するに到った。(Means for Solving the Problems) The present inventors have completed the present invention as a result of intensive studies to solve the above problems.
即ち、本発明は、水中において、酸素バランス値が負に
調節された有機系爆薬組成物を爆発させ、ダイヤモンド
を生成させることを特徴とするダイヤモンド合成方法を
提供するものである。That is, the present invention provides a diamond synthesizing method characterized in that an organic explosive composition having a negatively adjusted oxygen balance value is exploded in water to produce diamond.
本発明においては、ダイヤモンド製造原料としては、酸
素バランス値が負に調節された有機系爆薬組成物自体を
用い、従来のようにグラファイトは混入させない。本発
明では、組成物中に含まれる有機系爆薬化合物や、その
他の有機物質が爆発に際しての高温、高圧によってダイ
ヤモンドに変換される。In the present invention, as the diamond manufacturing raw material, the organic explosive composition itself whose oxygen balance value is adjusted to be negative is used, and graphite is not mixed as in the conventional case. In the present invention, the organic explosive compound and other organic substances contained in the composition are converted into diamond by the high temperature and high pressure during the explosion.
本明細書でいう酸素バランスは物質1gが爆発反応した場
合の酸素の余剰量をｇ単位で表わしたもので有機系爆薬
の爆発を示す反応式（Ｉ）に関し、計算式（II）で表わ
されるものである。The oxygen balance as referred to in the present specification is an excess amount of oxygen when 1 g of a substance undergoes an explosion reaction, and is expressed by a calculation formula (II) with respect to the reaction formula (I) indicating the explosion of an organic explosive. It is a thing.
CxHyOzNw →xCO2＋y/2H2O＋w/2N2−(2x+y/2-z)O2 （Ｉ） （式中、Ｍは化合物CxHyOzNwの分子量を示す） 一般の産業爆薬の多くはOBが負の可燃物やOBが正の含酸
素無機塩等を爆薬化合物に対して適量配合して、そのOB
をゼロに調節している。CxHyOzNw → xCO 2 + y / 2H 2 O ＋ w / 2N 2 − (2x + y / 2-z) O 2 (I) (In the formula, M represents the molecular weight of the compound CxHyOzNw.) In most of the general industrial explosives, a combustible substance whose OB is negative or an oxygen-containing inorganic salt whose OB is positive is mixed in an appropriate amount with respect to the explosive compound, and the OB
Is adjusted to zero.
本発明において、このようなOBがゼロに調節された産業
爆薬を原料とするためには、可燃性物質を添加し、その
組成物のOBを負、特に−0.25以下に調節する。可燃性物
質としては、パラフィン、軽油、重油、芳香族化合物、
植物油、でん粉、木粉、木炭等の炭素前駆体の酸素と反
応し得るものであればよい。In the present invention, in order to use the industrial explosive having the OB adjusted to zero as a raw material, a combustible substance is added, and the OB of the composition is adjusted to be negative, particularly −0.25 or less. As flammable substances, paraffin, light oil, heavy oil, aromatic compounds,
Any substance capable of reacting with oxygen of a carbon precursor such as vegetable oil, starch, wood flour and charcoal may be used.
本発明で用いる好ましい爆薬化合物としては、TNT（ト
リニトロトルエン）、NHX（シクロテトラメチレンテト
ラニトラミン）、RDX（シクロトリメチレントリニトラ
ミン）、PETN（ペンタエリスリトールテトラナイトレー
ト）、アミン類の硝酸塩又は過塩素酸塩、ニトログリセ
リン、ピクリン酸、テトリル等が挙げられる。本発明で
は、ダイナマイト組成物に対し、前記OBが負の可燃性物
質、特に、芳香族化合物を配合し、OBを−0.25〜−1.2
の範囲に調節したものも本発明における好ましい爆薬組
成物として使用される。Preferred explosive compounds used in the present invention include TNT (trinitrotoluene), NHX (cyclotetramethylenetetranitramine), RDX (cyclotrimethylenetrinitramine), PETN (pentaerythritol tetranitrate), nitrates of amines or Examples include perchlorate, nitroglycerin, picric acid, and tetril. In the present invention, with respect to the dynamite composition, the OB is a negative combustible substance, in particular, an aromatic compound is blended, and OB is -0.25 to -1.2.
The explosive composition adjusted to the above range is also used as a preferred explosive composition in the present invention.
本発明によりダイヤモンドを合成するには、OBが負に調
節された有機系爆薬組成物を水槽等の水中において爆発
させる。組成物を爆発させる水深は、目的とする反応生
成物のダイヤモンドが水中外に飛散しないような水深の
ところで行う必要があり、これは使用爆薬量や、使用す
る水槽の大きさ等により異なり一定しないが、一応の目
安としては50cm以上の水深のところが好ましい。この爆
発処理によりダイヤモントは水中に生成する。ダイヤモ
ンドの密度は水に比し非常に大きいので、水底に容易に
沈殿する。従って、所望回数のその爆発処理を行った
後、上澄液を取り去る方式や水底をさらう方式により、
ダイヤモンドを含む沈殿物を容易に回収することができ
る。To synthesize diamond according to the present invention, an organic explosive composition having a negatively adjusted OB is exploded in water such as an aquarium. The depth of water that explodes the composition must be such that the desired reaction product, diamond, does not scatter out of the water. This varies depending on the amount of explosive used, the size of the water tank used, etc. and is not constant. However, as a rough guide, it is preferable to have a water depth of 50 cm or more. Diamonds are generated in the water by this explosion process. The density of diamond is much higher than that of water, so it easily precipitates on the bottom of the water. Therefore, after performing the explosion treatment a desired number of times, by the method of removing the supernatant or the method of exposing the water bottom,
The precipitate containing diamond can be easily recovered.
また、水中に両端開放または一端開放の管を吊し、その
管内で爆薬組成物を爆発させる方式でもよい。この方式
では、爆発音を減少させることができる上、所望の多数
回の爆発を行うことにより反応生成物は主に管外に沈殿
するようになる。従って、上述の方式により反応生成物
は容易に回収できる。また、生成した反応生成物を管内
に回収したい時は、一端を封じた管、即ち一端が開口し
た密封管をその長軸がほぼ水平になるように水中に吊り
下げ、その管内で爆発させた後、開口部が上を向くよう
に水中から吊り上げる。そして静置後、沈殿物を回収す
る。Alternatively, a system in which both ends or one end is open is suspended in water and the explosive composition is exploded in the pipe. In this method, the explosion noise can be reduced, and the reaction products are mainly precipitated outside the tube by performing desired multiple explosions. Therefore, the reaction product can be easily recovered by the above method. Also, when it is desired to collect the generated reaction product in a tube, a tube with one end sealed, that is, a sealed tube with one end open, was suspended in water so that its major axis was almost horizontal, and exploded in the tube. Then, lift it from the water so that the opening faces upward. After standing, the precipitate is collected.
このようにして得られる反応生成物中には金属類やグラ
ファイト等の副生物が混在するので、通常のダイヤモン
ド合成方法の場合と同様にまず反応生成物から硝酸で金
属類を溶解除去してから、塩素酸と硝酸の混合液でグラ
ファイトがなくなるまで処理し、最後にフッ化水素酸と
硝酸の混合液で処理することにより純度の高いダイヤモ
ンドが得られる。Since byproducts such as metals and graphite are mixed in the reaction product thus obtained, first, like the case of the usual diamond synthesis method, the metals are first removed by dissolution with nitric acid from the reaction product. Diamond with high purity can be obtained by treating with a mixed solution of chloric acid and nitric acid until the graphite is exhausted, and finally with a mixed solution of hydrofluoric acid and nitric acid.
本発明では爆薬組成物は、成形物として用いるのが有利
である。この場合、成形物の密度はできるだけ高密度で
あるのが好ましく、通常、1.4g/cm3以上の密度になるよ
うに加圧成形するのが有利である。その形状は特に制約
されないが、通常は、円柱状成形体として用いられる。
また、この成形物には、成形助剤としてパラフィン等を
用いるのが好ましい。In the present invention, the explosive composition is advantageously used as a molded product. In this case, the density of the molded product is preferably as high as possible, and normally, it is advantageous to perform pressure molding so that the density is 1.4 g / cm 3 or more. The shape is not particularly limited, but it is usually used as a columnar molded body.
In addition, it is preferable to use paraffin or the like as a molding aid for this molded product.
本発明において、爆薬組成物の爆発は、水中で行うが、
この場合、使用する水槽の大きさや強度等は、その爆発
により破壊されないように設計する。また、水槽使用の
場合、水槽の底部の形状は、反応生成物が沈降しやす
く、またその外部への回収が容易なように、逆円錐形に
するのが有利である。In the present invention, the explosive composition is exploded in water,
In this case, the size and strength of the water tank to be used shall be designed so as not to be destroyed by the explosion. Further, in the case of using a water tank, the shape of the bottom portion of the water tank is advantageously an inverted conical shape so that the reaction products can easily settle and can be easily collected outside.
（実施例） 以下実施例に基づき、本発明を更に詳細に説明する。(Examples) The present invention will be described in more detail based on the following examples.
実施例１ 爆薬HM×76.2％、2,6-ジブロム‐4-ニトロフェノール1
9.5％、パラフィン4.3％の混合物10gを直径2cmの円柱状
に成形した。この成形物の密度は1.90g/ccであった。こ
れにHM×（粉状）1.5gと６号電気***を取り付けたもの
を、内径27cm、長さ125cmの肉厚0.6cmの一端が開放した
鉄製の円筒の内部にセットし、水深1.2mのところにその
円筒が水平になるように吊るし、６号電気***に通電に
よりその成形物を爆発させた。そして円筒の開口部が上
を向くようにして水中から引き上げ、静置し、沈殿を分
離し、これを王水処理により金属類の溶解除去し、次い
で塩素酸と硝酸の混合物で処理して混在するグラファイ
トを除去し、さらにフッ化水素酸と硝酸で処理し、水洗
した後乾燥した。Example 1 Explosive HM × 76.2%, 2,6-dibromo-4-nitrophenol 1
10 g of a mixture of 9.5% and paraffin 4.3% was molded into a column having a diameter of 2 cm. The density of this molded product was 1.90 g / cc. HM × (powder) 1.5g and No. 6 electric detonator were attached to the inside of an iron cylinder with an inner diameter of 27cm, a length of 125cm, and a wall thickness of 0.6cm, and one end of which was opened. By the way, the cylinder was hung so that it was horizontal, and the molded product was exploded by energizing the No. 6 electric detonator. Then, pull out from the water with the opening of the cylinder facing upwards, let it stand, separate the precipitate, dissolve and remove metals by aqua regia treatment, and then treat with a mixture of chloric acid and nitric acid to mix. The graphite was removed, treated with hydrofluoric acid and nitric acid, washed with water and dried.
得られた粉末をＸ線回折法（CuKα線、管電圧30kV、管
電流30mA）で走査した結果、これはダイヤモンドの単一
相であることを示した。得られたダイヤモンドは0.4gで
あった。これは使用したHMXの量に対して5.2％になる。The resulting powder was scanned by X-ray diffractometry (CuKα ray, tube voltage 30 kV, tube current 30 mA) and showed that it was a single phase of diamond. The obtained diamond was 0.4 g. This is 5.2% of the amount of HMX used.
実施例２ 爆薬TNT40％、爆薬RDX60％からなる組成物10gを直径2cm
の円柱状に成型した。成型物の密度は1.70g/ccである。
これを実施例１のように水中で爆発させ、生成物を回収
した。そして実施例１のように酸処理等を行い、得られ
た粉末についてＸ線回折を行ったところ、これはダイヤ
モンドの単一相であるこを示した。得られたダイヤモン
ドは0.15gであった。これは用いた爆薬の量に対し1.5％
になる。Example 2 10 g of a composition consisting of 40% of explosive TNT and 60% of explosive RDX, 2 cm in diameter
It was molded into a cylindrical shape. The density of the molded product is 1.70 g / cc.
This was exploded in water as in Example 1 to recover the product. Then, acid treatment and the like were performed as in Example 1, and X-ray diffraction was performed on the obtained powder, which showed that it was a single phase of diamond. The amount of diamond obtained was 0.15 g. This is 1.5% of the amount of explosive used
become.
実施例３ HMX76％、2,5-ジブロムニトロベンゼン14％、ステアリ
ン酸10％からなる爆発組成物10gを実施例１のように成
形した。成形物の密度は1.70g/ccであった。これを実施
例１のように水中で爆発させ、生成物を実施例１のよう
に酸処理等を行い、得られた粉末についてＸ線回折を行
ったところ、これはダイヤモンドの単一相であることを
示した。得られたダイヤモンドは用いた爆薬の量に対し
1.2％であった。Example 3 10 g of an explosive composition consisting of 76% HMX, 14% 2,5-dibromonitrobenzene and 10% stearic acid were molded as in Example 1. The density of the molded product was 1.70 g / cc. This was exploded in water as in Example 1, the product was subjected to acid treatment and the like as in Example 1, and the obtained powder was subjected to X-ray diffraction. This was a single phase of diamond. I showed that. The diamond obtained is based on the amount of explosive used
It was 1.2%.
（発明の効果） 本発明は、水中、または水中にセットした管内でダイヤ
モンドの爆発合成を行う方法であるから、その爆発音は
大気中の場合と比べて小さい。特に水中にセットした管
内で行う場合は、爆発エネルギーの大部分が管の運動エ
ネルギーに変換されてしまうので爆発音は極めて小さ
い。本発明によれば、ダイヤモンドを簡単、かつ容易に
得ることができる。(Effect of the Invention) Since the present invention is a method of performing explosive synthesis of diamond in water or in a tube set in water, the explosion sound is smaller than in the atmosphere. Especially when performed in a pipe set in water, most of the explosion energy is converted into kinetic energy of the pipe, so the explosion sound is extremely small. According to the present invention, diamond can be obtained easily and easily.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 飯田 光明 茨城県つくば市東１丁目１番地 工業技術 院化学技術研究所内 (72)発明者 田中 克己 茨城県つくば市東１丁目１番地 工業技術 院化学技術研究所内 (56)参考文献 特開 昭60−48133（ＪＰ，Ａ) 特表 昭57−501080（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Mitsuaki Iida 1-1, Higashi, Tsukuba, Ibaraki Industrial Technology Institute, Institute of Chemical Technology (72) Inventor Katsumi Tanaka 1-1, East, Tsukuba, Ibaraki Institute of Industrial Technology In-house (56) References JP-A-60-48133 (JP, A) Special table S57-501080 (JP, A)
Claims (2)
された有機系爆薬組成物を爆発させ、ダイヤモンドを生
成させることを特徴とするダイヤモンド合成方法。1. A method of synthesizing diamond, which comprises detonating an organic explosive composition having a negatively adjusted oxygen balance value in water to produce diamond.
て爆発させる請求項１の方法。2. The method according to claim 1, wherein the explosive composition is preliminarily mounted in a tubular body and exploded.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2072655A JPH0751220B2 (en) | 1990-03-22 | 1990-03-22 | Diamond synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2072655A JPH0751220B2 (en) | 1990-03-22 | 1990-03-22 | Diamond synthesis method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03271109A JPH03271109A (en) | 1991-12-03 |
| JPH0751220B2 true JPH0751220B2 (en) | 1995-06-05 |
Family
ID=13495612
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2072655A Expired - Lifetime JPH0751220B2 (en) | 1990-03-22 | 1990-03-22 | Diamond synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0751220B2 (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2051092C1 (en) * | 1991-12-25 | 1995-12-27 | Научно-производственное объединение "Алтай" | Diamond-containing substance and a method of its preparing |
| JP4245310B2 (en) | 2001-08-30 | 2009-03-25 | 忠正 藤村 | Diamond suspension aqueous solution excellent in dispersion stability, metal film containing this diamond, and product thereof |
| JP2006102656A (en) * | 2004-10-06 | 2006-04-20 | Asahi Kasei Chemicals Corp | Method for synthesizing diamond |
| WO2007001031A1 (en) * | 2005-06-29 | 2007-01-04 | Nippon Kayaku Kabushiki Kaisha | Process for producing fine diamond and fine diamond |
| US7862792B2 (en) * | 2005-12-30 | 2011-01-04 | Federal State Insitution “Federal Agency for Legal Protection of Military, Special and Dual Use Intellectual Activity Results” Under Ministry of Justics of the Russian Federation | Diamond-carbon material and a method for the production thereof |
| EP2072666B1 (en) | 2007-09-28 | 2011-11-16 | Venex Co., Ltd. | Fiber containing nano-sized diamond and platinum nanocolloid, and bedding product comprising the fiber |
| US8940267B2 (en) * | 2012-06-28 | 2015-01-27 | The Arizona Board Of Regents On Behalf Of The University Of Arizona | Method of purifying nanodiamond powder and purified nanodiamond powder |
| JP6114717B2 (en) | 2014-05-30 | 2017-04-12 | 株式会社神戸製鋼所 | Production method of carbon particles by detonation method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4483836A (en) * | 1980-07-31 | 1984-11-20 | Institut Khimicheskoi Fiziki Akademii Nauk Sssr | Method of producing diamond and/or diamond-like modifications of boron nitride |
| JPS6048133A (en) * | 1983-08-25 | 1985-03-15 | Yasuyuki Koshi | Process and structure of device for preparing diamond from graphite |
-
1990
- 1990-03-22 JP JP2072655A patent/JPH0751220B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03271109A (en) | 1991-12-03 |
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| Date | Code | Title | Description |
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| EXPY | Cancellation because of completion of term |