JP2561866B2 - Method for producing fine particles of boron carbide - Google Patents
Method for producing fine particles of boron carbideInfo
- Publication number
- JP2561866B2 JP2561866B2 JP2006562A JP656290A JP2561866B2 JP 2561866 B2 JP2561866 B2 JP 2561866B2 JP 2006562 A JP2006562 A JP 2006562A JP 656290 A JP656290 A JP 656290A JP 2561866 B2 JP2561866 B2 JP 2561866B2
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- JP
- Japan
- Prior art keywords
- fine particles
- laser
- gas
- reaction
- particle size
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/991—Boron carbide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (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、レーザーによる炭化ホウ素（以下、B4Cと
言う）微粒子の製造に係わり、詳しくは、ガスブレーク
ダウンを利用したレーザーによるB4C微粒子の製造方法
に関する。BACKGROUND OF THE INVENTION (FIELD OF THE INVENTION) The present invention, boron carbide by laser (hereinafter, B 4 say C) relates to the production of microparticles, details, B 4 by laser utilizing a gas breakdown It relates to a method for producing C fine particles.
（従来技術） 一般に物質の粒径が１μｍ（原子数にして1010個）以
下のものは微粒子と呼ばれ、焼結原料、触媒、生物工学
等の用途に用いられる新素材として関心がもたれてい
る。この場合、用いられる微粒子に望ましい条件は、化
学的純度が高いこと、球状かつ粒径が小さいこと、粒径
が均一であること等である。このような微粒子の製造方
法としては、固相反応法、液相反応法、気相反応法等が
あるが、上記の条件に適合した微粒子の製造方法として
は気相反応法が最適である。(Prior art) Generally, a substance having a particle size of 1 μm or less (10 10 atoms in number) is called a fine particle, and is attracting attention as a new material used for sintering raw materials, catalysts, biotechnology, and the like. I have. In this case, desirable conditions for the fine particles used are high chemical purity, spherical shape and small particle size, uniform particle size, and the like. As a method for producing such fine particles, there are a solid phase reaction method, a liquid phase reaction method, a gas phase reaction method and the like, and a gas phase reaction method is most suitable as a method for producing fine particles meeting the above conditions.
従来、気相反応法とレーザー誘起反応とを組み合わせ
た微粒子生成法〔セラミックス:19（1984）、No.6 p48
2〕により、Si、SiC、Si3N4の微粒子が得られていた。Conventionally, a particle generation method combining a gas-phase reaction method and a laser-induced reaction [Ceramics: 19 (1984), No. 6 p48
According to 2], fine particles of Si, SiC and Si 3 N 4 were obtained.
一方、本発明者等は、上記のCO2レーザーの熱反応法
に代わって、気体の誘導破壊（ガスブレークダウン）、
すなわち、パルス発振レーザーを基体に照射するとレー
ザー光の時間的、空間的な高輝度のために生じる現象を
利用した微粒子生成方法を見い出し、既に、特開平１−
252515号：炭化ケイ素の微粒子製造方法、特開平１−25
2517号：ホウ素の微粒子製造方法、特開平１−252518
号：チタン化ホウ素の微粒子製造方法を提案した。特
に、ホウ素（Ｂ）の微粒子製造方法の場合には、原料気
体にハロゲン化ホウ素BX3（Ｘ＝Ｆ、Cl、Br）及び水素
の混合気体を用い、 BX3＋H2→Ｂ＋HX＋BHX2 の反応により平均粒子が0.08μｍのホウ素の微粒子を製
造するものであり、また、チタン化ホウ素（TiB2）の場
合には、原料気体にTiCl4とハロゲン化ホウ素BX3（Ｘ＝
Ｆ、Cl、Br）を用い、 TiCl4＋2BX3＋5H2→TiB2＋10HX の反応により平均粒子が0.16μｍのチタン化ホウ素の微
粒子を製造するものであった。On the other hand, the present inventors have replaced the thermal reaction method of the CO 2 laser described above with the inductive destruction of gas (gas breakdown),
That is, a method of generating fine particles utilizing a phenomenon that occurs when a pulsed laser is irradiated on a substrate due to high temporal and spatial brightness of laser light has been found.
No. 252515: Method for producing fine particles of silicon carbide, JP-A-1-25
No. 2517: Method for producing fine particles of boron, JP-A-1-252518
No .: A method for producing fine particles of boron titanate was proposed. In particular, in the case of a method for producing fine particles of boron (B), a mixed gas of boron halide BX 3 (X = F, Cl, Br) and hydrogen is used as a raw material gas, and a reaction of BX 3 + H 2 → B + HX + BHX 2 is performed. It produces fine particles of boron having an average particle size of 0.08 μm. In the case of boron titanate (TiB 2 ), TiCl 4 and boron halide BX 3 (X =
F, Cl, Br) to produce fine particles of boron titanate having an average particle size of 0.16 μm by the reaction of TiCl 4 + 2BX 3 + 5H 2 → TiB 2 + 10HX.
（発明が解決しようとする課題） 上記方法の特長は次のようなものである。（１）照射
光の波長領域に吸収帯を有しない物質も原料として用い
ることができる。（２）光の吸収効率が良い。（３）操
作圧が高く、反応は連鎖的なので収量が多い。（４）器
壁からの不純物の混入がない。（５）常温の反応容器で
高融点物質が得られる。（６）粒径分布の狭い微粒子が
得られる。（７）反応装置が単純で容易に行うことがで
きる。(Problems to be Solved by the Invention) The features of the above method are as follows. (1) A substance having no absorption band in the wavelength region of irradiation light can also be used as a raw material. (2) Light absorption efficiency is good. (3) The operating pressure is high and the reaction is chained, so that the yield is high. (4) No impurities are mixed from the vessel wall. (5) A high melting point substance can be obtained in a reaction vessel at room temperature. (6) Fine particles having a narrow particle size distribution can be obtained. (7) The reaction apparatus is simple and can be easily operated.
本発明は、選択された原料気体を用いて、上記のよう
な特長を有するレーザーによるブレークダウンを利用し
てB4Cの微粒子を製造する方法を提供することを目的と
する。An object of the present invention is to provide a method for producing B 4 C fine particles using a selected source gas and utilizing laser breakdown having the above-described features.
（課題を解決するための手段） 上記の課題は、ハロゲン化ホウ素、炭化水素、及び水
素とを含む混合気体、またはハロゲン化ホウ素、四塩化
炭素、及び水素を含む混合気体にパルス発振CO2レーザ
ー光を照射して、ガスブレークダウン現象により炭化ホ
ウ素の微粒子を生成する本方法によって達成することが
できる。(Means for Solving the Problems) The above-mentioned problem is solved by using a pulsed CO 2 laser in a mixed gas containing boron halide, hydrocarbon, and hydrogen, or a mixed gas containing boron halide, carbon tetrachloride, and hydrogen. The method can be achieved by irradiating light to generate fine particles of boron carbide by a gas breakdown phenomenon.
（作 用） 以下に本発明を詳しく説明する。(Operation) Hereinafter, the present invention will be described in detail.
粒径の揃った特性の良い微粒子の製法としては、気体
原料を用いた気相法が適しているが、B4Cの気体原料と
して、ハロゲン化ホウ素BX3〔Ｘ＝Ｆ、Cl、Br、Ｉ〕、
炭化水素CnHm、水素H2から成る混合気体、またはハロゲ
ン化ホウ素BX3、四塩化炭素CCl4、水素H2から成る混合
気体を用いる。ここで、炭化水素CnHmとは、鎖式炭化水
素であるCnH2n+2、CnH2n、及びCnH2n-2（ｎは整数）、
または環式炭化水素であるCnH2n、CnH2n-2、及びCnH
2n-6（ｎは整数）で表わされる化合物である。好ましい
混合気体の範囲は、気体原料として、ハロゲン化ホウ
素、炭化水素、及び水素H2を用いる場合には、ハロゲン
化ホウ素：炭化水素：水素の比率が（２〜10）:1:（100
以下）であり、気体原料として、ハロゲン化ホウ素、四
塩化炭素、及び水素を用いる場合には、ハロゲン化ホウ
素：四塩化炭素：水素の比率が（２〜10）:1:（100以
下）である。また、これらの混合気体の全圧は200〜100
0Torrであることが好ましい。この原料に室温でCO2レー
ザーのパルス光を照射すると、レーザー光の単位断面積
当たりのエネルギー（フルエンス）が小さい場合には、
レーザー光のエネルギーは混合ガスにほとんど吸収され
ないが、ある程度以上の強さのレーザー光の場合、原料
気体内でブレークダウンが起こって、照射されたレーザ
ーエネルギーのほとんどが吸収される。これは、原料気
体分子の光エネルギーによるイオン化及びそれによって
生じた電子の光エネルギー吸収に続くイオン化の繰り返
しによって、それぞれ以下に示す反応が引き起こされ
る。A gas phase method using a gaseous raw material is suitable as a method for producing fine particles having good characteristics with uniform particle diameters. However, as a gaseous raw material for B 4 C, boron halide BX 3 [X = F, Cl, Br, I],
Hydrocarbons C n H m, a mixed gas consisting of hydrogen H 2 or boron halide BX 3,, carbon tetrachloride CCl 4, a mixed gas consisting of hydrogen H 2. Here, the hydrocarbon C n H m, is a chain hydrocarbon C n H 2n + 2, C n H 2n, and C n H 2n-2 (n is an integer),
Or a cyclic hydrocarbon C n H 2n , C n H 2n-2 , and C n H
It is a compound represented by 2n-6 (n is an integer). A preferable range of the mixed gas is such that when a boron halide, a hydrocarbon, and hydrogen H 2 are used as a gaseous raw material, the ratio of boron halide: hydrocarbon: hydrogen is (2 to 10): 1: (100
Below), and when using boron halide, carbon tetrachloride, and hydrogen as the gaseous raw material, the ratio of boron halide: carbon tetrachloride: hydrogen is (2-10): 1: (100 or less) is there. In addition, the total pressure of these mixed gases is 200 to 100
Preferably, it is 0 Torr. When this material is irradiated with CO 2 laser pulse light at room temperature, if the energy (fluence) per unit sectional area of the laser light is small,
Although the energy of the laser light is hardly absorbed by the mixed gas, in the case of the laser light having a certain intensity or more, breakdown occurs in the raw material gas and most of the irradiated laser energy is absorbed. The following reactions are caused by repetition of ionization of light gas molecules by light energy and absorption of light energy of electrons generated by the light energy, respectively.
4nBX3＋CnHm＋lH2→nB4C＋12nHX 4BX3＋CCl4＋8H2→B4C＋12HX＋4HCl この場合、照射に使用するレーザーの波長は、原料気
体の吸収波長に関係なく、できるだけパルスエネルギー
の強い発振波長がよい。好ましくは9.6μｍである。ま
たCO2レーザーの他にHF、CO、YAG、エキシマレーザーを
用いることもできる。上記反応によって得られるB4Cは
気相で均一核生成とその成長によって得られるので、原
理的に球状で粒径も揃う。微粒子の粒径は0.3μｍ以下
のものが得られ、生成条件の制御によっては得られる微
粒子の特性を変えることも可能である。具体的には微粒
子の粒径は、試料圧力に依存し、圧力増大と共に粒径は
比例的に大きくなる。レーザー光のエネルギーを増加し
ても粒径は一定であるが収量は比例して大きくなる。4nBX 3 + CnHm + lH 2 → nB 4 C + 12nHX 4BX 3 + CCl 4 + 8H 2 → B 4 C + 12HX + 4HCl In this case, the wavelength of the laser used for the irradiation preferably has an oscillation wavelength with a pulse energy as strong as possible irrespective of the absorption wavelength of the raw material gas. Preferably it is 9.6 μm. In addition to the CO 2 laser, an HF, CO, YAG, or excimer laser can be used. Since B 4 C obtained by the above reaction is obtained by uniform nucleation and growth in the gas phase, it is in principle spherical and uniform in particle size. Fine particles having a particle diameter of 0.3 μm or less can be obtained, and the characteristics of the obtained fine particles can be changed by controlling production conditions. Specifically, the particle size of the fine particles depends on the sample pressure, and the particle size increases proportionally as the pressure increases. Even if the energy of the laser beam is increased, the particle size is constant, but the yield increases proportionally.
実際の微粒子の製造には、回分式または連続流通式の
照射セルを使用し、生成した微粒子の補集にはフィルタ
ーやその他の補集装置を用いることができる。A batch-type or continuous-flow irradiation cell is used for the actual production of fine particles, and a filter or other collecting device can be used for collecting the generated fine particles.
（発明の効果） このように、本発明によって得られたB4C微粒子は、
ほぼ球状でしかも均一であり、また高硬度・高融点セラ
ミックスとして種々の有用な素材に利用できる。現在、
B4C微粒子は粉砕法によって製造されているが、硬度が
大であるため能率が悪く、球状の微粒子が得られにく
く、また、粉砕機からの不純物の混入も避けられない。
本法は生成原理も簡単なものであり、現行法よりも著し
く有利である。B4C粒子は研磨材、耐摩耗材、電子材
料、原子炉の制御材や遮蔽材等への用途が具体的であ
り、特に高品質が要求される原子炉材として好適であ
る。(Effect of the Invention) As described above, the B 4 C fine particles obtained by the present invention are:
It is almost spherical and uniform, and can be used for various useful materials as high hardness and high melting point ceramics. Current,
Although B 4 C fine particles are produced by a pulverizing method, the efficiency is poor due to high hardness, spherical fine particles are hardly obtained, and impurities from the pulverizer are unavoidable.
This method has a simple generation principle and has a remarkable advantage over the current method. The B 4 C particles are specifically used for abrasives, wear-resistant materials, electronic materials, control materials for nuclear reactors, shielding materials, and the like, and are particularly suitable as reactor materials requiring high quality.
（実施例） 本発明に使用した装置の概略を第１図に示す。(Example) FIG. 1 shows an outline of an apparatus used in the present invention.
適切な波数のCO2レーザー11のパルス光12をBaF2レン
ズ13で集光し、照射反応容器14内のBBr3とCH4とH2の混
合気体である試料気体15に照射する。尚、図中16は絞
り、17はKBr窓板、18は補集容器をそれぞれ示す。レー
ザー照射後、残留及び生成された副産物のガスを排気除
去し、不活性ガスで容器内を充たした後生成した微粒子
を補集容器から取り出す。A pulse light 12 of a CO 2 laser 11 having an appropriate wave number is condensed by a BaF 2 lens 13 and irradiated to a sample gas 15 in an irradiation reaction vessel 14 which is a mixed gas of BBr 3 , CH 4 and H 2 . In the drawing, 16 denotes a stop, 17 KB r window plate, 18 denotes a scavenged container. After the laser irradiation, the residual and generated by-product gases are exhausted and removed, and after filling the inside of the container with an inert gas, the generated fine particles are taken out of the collection container.
（実施例１） 反応容器内を４×10-4Torrの真空度にした後、50Torr
のBBr3と13TorrのCH4と200TorrのH2の混合ガスを導入し
た。これに、CO2レーザーの9.6μｍ帯のＰ（24）、すな
わち1043cm-1のパルス光を、４時間、繰り返し数800回
で照射した。この時のパルスエネルギーは約2.5J/puls
e、使用したレンズの焦点距離は20cmである。反応式
は、 4BBr3＋CH4＋4H2→B4C＋12HBr のように表わすことができる。(Example 1) After the inside of the reaction vessel was evacuated to 4 × 10 -4 Torr, the pressure was then reduced to 50 Torr.
A mixed gas of BBr 3 , 13 Torr CH 4 and 200 Torr H 2 was introduced. This was irradiated with P (24) in the 9.6 μm band of a CO 2 laser, that is, pulsed light of 1043 cm −1 for 4 hours at 800 repetitions. The pulse energy at this time is about 2.5 J / pulse
e, The focal length of the used lens is 20cm. The reaction formula can be expressed as follows: 4BBr 3 + CH 4 + 4H 2 → B 4 C + 12HBr.
この反応で0.2gのB4Cが生成した。This reaction produced 0.2 g of B 4 C.
生成した微粒子のＸ線回折図形を第２図に示す。B4C
の既知のデータ値（Nat.Bur.Stand.（U.S.）Monogr.,2
1，（1984））と測定したＸ線回折図形を対比し、この
図形の解析から得られる面定数と元素分析の結果から、
生成微粒子はB4Cであることを確認した。更に、第３図
に示すB4C微粒子の粒径分布図からわかるように本方法
によって得られたB4Cは平均粒径が0.3μｍの比較的均一
な分布を示し、しかも、ほほ球状の微粒子であることが
走査型電子顕微鏡写真によって確認された。FIG. 2 shows an X-ray diffraction pattern of the generated fine particles. B 4 C
Known data values (Nat. Bur. Stand. (US) Monogr., 2
1 , (1984)) and the measured X-ray diffraction pattern, and from the surface constants obtained from the analysis of this pattern and the results of elemental analysis,
It was confirmed that the generated fine particles were B 4 C. Furthermore, the 3 B 4 C obtained by the present method as seen from the particle size distribution diagram of B 4 C particles shown in FIG average particle diameter indicates a relatively uniform distribution of 0.3 [mu] m, moreover, cheek spherical The particles were confirmed by a scanning electron micrograph.
本実施例では、炭化水素CnHmにメタンCH4を用いた
が、この他エチレンC2H4、アセチレンC2H2プロパンC
3H8、ベンゼンC6H6等を用いても良い。In this embodiment uses methane CH 4 in hydrocarbon CnHm, the other ethylene C 2 H 4, acetylene C 2 H 2 propane C
3 H 8 , benzene C 6 H 6 or the like may be used.
（実施例２） 反応容器内を約４×10-4Torrの真空度にした後、100T
orrのBCl3と25TorrのCCl4と300TorrのH2の混合ガスを導
入した。これに、CO2レーザーの9.6μｍ帯のＰ（24）、
すなわち1043cm-1のパルス光を、２時間、繰り返し数4,
000回で照射した。この時のパルスエネルギーは約2.5J/
pulse、使用したレンズの焦点距離は20cmである。反応
式は、 4BCl3＋CCl4＋8H2→B4C＋16HCl のように表わすことができる。(Example 2) After the inside of the reaction vessel was evacuated to a degree of vacuum of about 4 × 10 -4 Torr, 100 T
A mixed gas of orr BCl 3 , 25 Torr CCl 4 and 300 Torr H 2 was introduced. To this, P (24) of CO 2 laser of 9.6μm band,
That is, a pulse light of 1043 cm -1 is applied for 2 hours and the number of repetitions is 4,
Irradiated 000 times. The pulse energy at this time is about 2.5J /
Pulse, the focal length of the lens used is 20 cm. The reaction formula can be expressed as 4BCl 3 + CCl 4 + 8H 2 → B 4 C + 16HCl.
この反応で0.1gのB4Cが生成した。This reaction produced 0.1 g of B 4 C.
生成した微粒子のＸ線回折図形をB4Cの既知のデータ
値（Nat.Bur.Stand.（U.S.）Monogr.,21，（1984））と
測定したＸ線回折図形を対比し、この図形の解析から得
られる面定数と元素分析の結果から、生成微粒子はB4C
であることを確認した。更に、本方法によって得られた
B4Cは第３図の粒径分布図と同様に平均粒径が0.3μｍの
比較的均一な分布を示し、しかも、ほぼ球状の微粒子で
あることが走査型電子顕微鏡写真によって確認された。Known data values of the X-ray diffraction pattern of the resulting fine particles B 4 C (Nat.Bur.Stand. (US ) Monogr., 21, (1984)) and compared to X-ray diffraction pattern measured, the graphic From the surface constants obtained from the analysis and the results of the elemental analysis, the fine particles produced were B 4 C
Was confirmed. Furthermore, the method obtained by this method
B 4 C shows a relatively uniform distribution of particle size distribution diagram as well as the average particle size of 0.3μm in Figure 3, moreover, be approximately spherical microparticles was confirmed by scanning electron micrographs.
第１図は、本発明の実施例に用いた装置の概略図であ
り、 第２図は、本発明の実施例１で得られたB4C微粒子のＸ
線回折図形である。 第３図は本発明の実施例１で得られたB4C微粒子の粒径
分布図である。 （符号の説明） 11……CO2レーザー 12……レーザー光、 13……BaF2レンズ、 14……照射反応容器、15……試料気体、 16……絞り、17、19……KBr窓板、 18……補集容器、20……コック。FIG. 1 is a schematic diagram of an apparatus used in an embodiment of the present invention, and FIG. 2 is a schematic view of X of the B 4 C fine particles obtained in the embodiment 1 of the present invention.
It is a line diffraction pattern. FIG. 3 is a particle size distribution diagram of B 4 C fine particles obtained in Example 1 of the present invention. (Code description) 11 ...... CO 2 laser 12 ...... laser light, 13 ...... BaF 2 lens, 14 ...... irradiation reaction vessel, 15 ...... gaseous sample, the diaphragm 16 ......, 17, 19 ...... KBr window plate , 18 ... collection container, 20 ... cook.
Claims (1)
を含む混合気体、またはハロゲン化ホウ素、四塩化炭
素、及び水素とを含む混合気体にパルス発振レーザー光
を照射して炭化ホウ素の粒径0.5μｍ以下の微粒子を製
造する方法。1. A method of irradiating a pulsed laser beam to a mixed gas containing boron halide, hydrocarbon and hydrogen, or a mixed gas containing boron halide, carbon tetrachloride and hydrogen to obtain a particle diameter of boron carbide A method for producing fine particles of 0.5 μm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006562A JP2561866B2 (en) | 1990-01-16 | 1990-01-16 | Method for producing fine particles of boron carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006562A JP2561866B2 (en) | 1990-01-16 | 1990-01-16 | Method for producing fine particles of boron carbide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03215309A JPH03215309A (en) | 1991-09-20 |
| JP2561866B2 true JP2561866B2 (en) | 1996-12-11 |
Family
ID=11641771
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006562A Expired - Lifetime JP2561866B2 (en) | 1990-01-16 | 1990-01-16 | Method for producing fine particles of boron carbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2561866B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2515735A (en) * | 2013-07-01 | 2015-01-07 | Metal Nanopowders Ltd | Hard Materials |
| RU2648421C2 (en) * | 2016-07-06 | 2018-03-26 | Акционерное общество "Производственное объединение Электрохимический завод" (АО "ПО ЭХЗ") | Plasma-chemical method of producing boron carbide |
| CN112897528B (en) | 2021-03-24 | 2022-11-22 | 云南华谱量子材料有限公司 | Method for synthesizing boron carbide/carbon powder material by laser sintering |
-
1990
- 1990-01-16 JP JP2006562A patent/JP2561866B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03215309A (en) | 1991-09-20 |
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