JPH02255537A - Production of fine powder of molybdenum disulfide - Google Patents
Production of fine powder of molybdenum disulfideInfo
- Publication number
- JPH02255537A JPH02255537A JP7751889A JP7751889A JPH02255537A JP H02255537 A JPH02255537 A JP H02255537A JP 7751889 A JP7751889 A JP 7751889A JP 7751889 A JP7751889 A JP 7751889A JP H02255537 A JPH02255537 A JP H02255537A
- Authority
- JP
- Japan
- Prior art keywords
- laser
- fine particles
- laser light
- gaseous mixture
- vessel
- 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
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000000843 powder Substances 0.000 title 1
- 239000010419 fine particle Substances 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 20
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 15
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 229910052961 molybdenite Inorganic materials 0.000 abstract description 4
- 230000001678 irradiating effect Effects 0.000 abstract description 3
- 229910001632 barium fluoride Inorganic materials 0.000 abstract description 2
- 239000011261 inert gas Substances 0.000 abstract description 2
- 239000000314 lubricant Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 229910017333 Mo(CO)6 Inorganic materials 0.000 abstract 3
- 239000008246 gaseous mixture Substances 0.000 abstract 3
- 239000002245 particle Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010574 gas phase reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000013926 blood microparticle formation Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000005372 isotope separation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、レーザーによる二硫化モリブデン（ＭＯ９２
）微粒子の製造に関し、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二硫化モリブデン微粒子の製
造法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention is directed to the production of molybdenum disulfide (MO92) by laser.
) Regarding the production of fine particles, in particular, it relates to a method for producing fine particles of molybdenum disulfide using a laser using gas breakdown.
（従来の技術）
一般に種々の材料となる物質は、原子の数が無限側の集
合体であり、その物質の大きさが極端に小さくなると、
特異な性質を示すようになる。物質の粒径が１μｍ（原
子数にして１０Ｉ０個）以下のものは微粒子と呼ばれ、
焼結原料、触媒、生物工学等の種々の用途に用いられる
新素材として関心が持たれている。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
状でありその粒径が小さいこと、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法としては気相反応法が最適で
ある。(Prior art) Substances that are used as various materials are generally aggregates with an infinite number of atoms, and when the size of the substance becomes extremely small,
It begins to exhibit unique properties. Substances with a particle size of 1 μm or less (10I0 atoms) are called fine particles.
There is interest as a new material for various uses such as sintering raw materials, catalysts, and biotechnology. In this case, desirable conditions for the fine particles used include high chemical purity, spherical shape and small particle size, and uniform particle size. Methods for producing such fine particles include a solid phase reaction method, a liquid phase reaction method, a gas phase reaction method, etc., but the gas phase reaction method is most suitable as a method for producing fine particles that meet the above conditions.
他方、レーザー技術に関する進歩は目覚ましく、広い波
長領域で強力な光を発振するレーザーが開発されている
。とりわけ、典型的な赤外レーザーである炭酸ガスレー
ザーは、その高効率、高出力のため、種々の用途が考え
られている。例えば、パルス発振ＴＥＡ−Ｃｏ□レーザ
ーの赤外多光子解離による同位体分離や連続発振ＣＤ□
レーザーの熱反応による微粒子製造等が研究されており
、すでに、第４図に示すような気相反応法とレーザー誘
起反応とを組合わせた微粒子生成法（セラミックス：１
９ （１９８４）、Ｎα６、ｐ４８２）が報告されてい
る。これは、反応ガスをＣＯ２レーザーで加熱して、以
下に示す反応によって、５ｉ１ＳｉＣ１３ｉａＮ＊の超
微粒子を生成するものである。On the other hand, progress in laser technology is remarkable, and lasers that emit powerful light in a wide wavelength range have been developed. In particular, carbon dioxide lasers, which are typical infrared lasers, are considered for various uses due to their high efficiency and high output. For example, isotope separation by infrared multiphoton dissociation of pulsed TEA-Co□ laser and continuous wave CD□
The production of fine particles through laser thermal reactions is being researched, and a fine particle production method (ceramics: 1
9 (1984), Nα6, p482) has been reported. This involves heating a reaction gas with a CO2 laser and producing ultrafine particles of 5i1SiC13iaN* through the reaction shown below.
ＳｉＨ４（ｇ） −５ｉ（ｓ）＋２Ｈｚ（ｇ）２ＳｉＨ
４（ｇ） ＋ Ｃ２Ｈ４（ｇ）→２ＳｉＣ（ｓ） ＋
６Ｈａ（ｇ）３Ｓｉ）Ｉ４（ｇ） ＋ ４Ｎ）Ｉｓ （
ｇ）→ＳｉＪ４（ｇ） ＋ １２８２ （ｇ）（発明が
解決しようとする課題）
本発明者等は、レーザ一応用技術を研究した過程で、前
述のＣ０２レーザーの熱反応法に代わって、気体の誘電
破壊（ガスブレークダウン）、すなわち、パルス発振レ
ーザーを気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て、微粒子を生成
することができることを見い出した。このブレークダウ
ンを利用すると、原料気体にレーザーを照射して種々の
反応を誘起させ粒径の非常に小さい固体生成物を製造す
ることができる。この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
よい。（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
が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。本発明は、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たＭｏＳ２
の微粒子を製造する方法を提供することを目的とする。SiH4(g) -5i(s)+2Hz(g)2SiH
4(g) + C2H4(g) → 2SiC(s) +
6Ha(g)3Si)I4(g) + 4N)Is (
g) → SiJ4(g) + 1282 (g) (Problem to be Solved by the Invention) In the process of researching laser application technology, the present inventors developed a gas-based method instead of the thermal reaction method of the C02 laser described above. We have discovered that it is possible to generate microparticles by utilizing dielectric breakdown (gas breakdown), a phenomenon that occurs when a gas is irradiated with a pulsed laser due to the temporal and spatial high brightness of the laser light. . Utilizing this breakdown, it is possible to produce solid products with extremely small particle sizes by irradiating the raw material gas with a laser to induce various reactions. The features of this method are as follows. (1) Substances that do not have an absorption band in the wavelength region of the irradiated light can also be used as raw materials. (2) Good light absorption efficiency. (3) The operating pressure is high and the reaction is chain-like, so the yield is high. (4) There is no contamination of impurities from the vessel wall. (5) A high melting point substance can be obtained in a reaction vessel at room temperature. (6) Fine particles with a narrow particle size distribution can be obtained. (7) The reaction apparatus is simple and the reaction can be carried out easily. The present invention provides MoS2 using laser breakdown having the above-mentioned features.
An object of the present invention is to provide a method for manufacturing fine particles of.
（課題を解決するための手段）
モリブデンカルボニル［Ｍｏ（ＣＯ）ｓ ］二硫化炭素
（ＣＳ２）又は硫化水素（Ｈ２Ｓ）を含む混合ガスにレ
ーザー光を照射して、ガスブレークダウン現象により二
硫化モリブデン（ＭｏＳ２）の微粒子を生成することを
特徴とする。(Means for solving the problem) Molybdenum carbonyl [Mo(CO)s] By irradiating laser light on a mixed gas containing carbon disulfide (CS2) or hydrogen sulfide (H2S), molybdenum disulfide is produced by a gas breakdown phenomenon. It is characterized by producing fine particles of (MoS2).
照射すべきレーザー光としてはパルス発振Ｃ０２レーザ
ー光を使用することができる。A pulsed C02 laser beam can be used as the laser beam to be irradiated.
（作 用） 以下本発明の詳細な説明する。(for production) The present invention will be explained in detail below.
粒径の揃った特性の良い微粒子の製法としては、気体原
料を用いる気相法が適しているが、Ｍｏ５ｔの気体の原
料として、モリブデンカルボニルＣＭｏ （ＣＤ） ｓ
）と二硫化炭素（ＣＳ２）又は硫化水素（Ｈ，Ｓ）の
混合ガスを用いる。この原料にＣ０２レーザー光を照射
すると、レーザー光の単位断面接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、原料ガス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。これは原料ガス分子の光エネルギーによる
イオン化およ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操り返しによって次ぎの反応が引
き起こされる。As a method for producing fine particles with uniform particle size and good characteristics, a gas phase method using a gaseous raw material is suitable, but as a gaseous raw material for Mo5t, molybdenum carbonyl CMo (CD)
) and carbon disulfide (CS2) or hydrogen sulfide (H,S). When this raw material is irradiated with C02 laser light, the energy per unit cross section of the laser light (
When the fluence (fluence) is small, the energy of the laser beam is hardly absorbed by the gas, but when the intensity of the laser beam exceeds a certain level, breakdown occurs within the source gas and most of the irradiated laser energy is absorbed. be done. The next reaction is caused by the ionization of source gas molecules by light energy and the subsequent manipulation of the ionization following absorption of light energy by the electrons produced thereby.
Ｍｏ（ＣＯｓ）＋Ｃ３ｉ ＝ Ｍｏ５ａ ＋ ６ＣＤ＋
ＣＭｏ（ＣＯｓ）＋ ２）＋２Ｓ＝ ＭＯ５２＋
６Ｃロ＋２Ｈ。Mo(COs)+C3i = Mo5a + 6CD+
CMo(COs)+ 2)+2S= MO52+
6Cro+2H.
この場合、照射に使用するレーザーの波長は、原料ガス
の吸収波長に関係なく、できるだけパルスエネルギーの
強い発振波長が良い。上記の反応によって得られるＭｏ
５ｓは気相で均一核生成と成長によって生成した粒子状
のもので、原理的に球状で粒径分布が狭く、粒径が０．
１μｍ以下の微粒子であり、生成条件の制御により得ら
れる微粒子の特性を変えることが可能である。In this case, the wavelength of the laser used for irradiation is preferably an oscillation wavelength with as strong a pulse energy as possible, regardless of the absorption wavelength of the source gas. Mo obtained by the above reaction
5s is a particulate material produced by uniform nucleation and growth in the gas phase, and is theoretically spherical with a narrow particle size distribution and a particle size of 0.5s.
They are fine particles with a size of 1 μm or less, and the characteristics of the fine particles obtained can be changed by controlling the production conditions.
実際の微粒子の製造には、回分式又は連続流通式の照射
セルを使用し、生成した微粒子はフィルターやその他の
補集装置で補集することができる。In actual production of fine particles, a batch type or continuous flow type irradiation cell is used, and the generated fine particles can be collected with a filter or other collection device.
（発明の効果）
このように、本発明によって得られたＭｏＳ２微粒子は
、粒径が非常に小さくしかも均一であり、また、固体潤
滑剤として利用できる。現在、ＭＯ３２微粒子は粉砕法
によって製造されているが粒径が小さく均一な微粒子が
得られにくい。また、粉砕機からの不純物の混入も避け
られない。本性では前述のように、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。(Effects of the Invention) As described above, the MoS2 fine particles obtained by the present invention have a very small and uniform particle size, and can be used as a solid lubricant. Currently, MO32 fine particles are produced by a pulverization method, but the particle size is small and it is difficult to obtain uniform fine particles. In addition, contamination with impurities from the crusher is also unavoidable. In essence, as mentioned above, the generation principle is simple, and it is significantly more advantageous than the current method.
（実施例） 本発明に使用した装置の概略を第１図に示す。(Example) An outline of the apparatus used in the present invention is shown in FIG.
ＣＯ。レーザー１１から発生された適切な波数のパルス
状レーザー光１２が絞り１６を通過した後、ＢａＦ２レ
ンズ１３で集光される。この集光されたレーザー光はＫ
Ｂｒ窓１７を通して、照射反応容器１４内のＭｏ （Ｃ
Ｄ） ａとＣ８２又はＬＳの混合気体である試料気体１
５を照射される。照射後、残留および生成ガスを排気除
去し、不活性ガスで容器内を充たした後、補集容器１８
に光反応により堆積した微粒子がこの容器から取り出さ
れる。C.O. A pulsed laser beam 12 of an appropriate wave number generated by a laser 11 passes through an aperture 16 and is then focused by a BaF2 lens 13. This focused laser light is K
Mo (C
D) Sample gas 1 which is a mixed gas of a and C82 or LS
5 is irradiated. After irradiation, residual and generated gases are exhausted and removed, and after filling the container with inert gas, the collection container 18 is
The fine particles deposited by the photoreaction are removed from this container.
１２ＴｏｒｒのＭｏ （ＣＯ） ｓと２００ Ｔｏｒｒ
のＣ３２の混合ガスにＣＯ２レーザーの９．６．ｕｍ帯
のＰ（２４）、すなわち１０４３０１１１−’のパルス
光を照射した、この時のパルスエネルギーは約Ｉ Ｊ
／ ｐｕｌｓｅ 、使用したレンズの焦点距離は７．５
ｃｍである。Mo(CO)s at 12 Torr and 200 Torr
9.6. of CO2 laser on C32 mixed gas. P(24) in the um band, that is, 10430111-' pulsed light was irradiated, and the pulse energy at this time was approximately I J
/ pulse, the focal length of the lens used is 7.5
cm.
第２図は生成した微粒子の粒径の分布を走査型電子顕微
鏡写真を用いて測定した結果のグラフである。本性によ
って得られた平均粒径が０．０７μｍの比較的均一な分
布を示すＭＯ５２微粒子であることが確言忍できた。FIG. 2 is a graph showing the results of measuring the particle size distribution of the produced fine particles using a scanning electron microscope photograph. It was confirmed that the obtained MO52 fine particles had a relatively uniform distribution with an average particle diameter of 0.07 μm.
また、生成した微粒子のＸ線回折の解析から得られた固
定数と元素分析の結果から、生成微粒子は非晶質のＭｏ
Ｓ２であることを確認した。In addition, from the fixed number obtained from X-ray diffraction analysis of the generated fine particles and the results of elemental analysis, it was found that the generated fine particles were amorphous Mo.
I confirmed that it was S2.
第１図は、本発明の実施例に用いた装置の概略図、
第２図は、本発明の実施例で得られたＭｏ微粒子の粒径
分布を示すグラフ、
第３図は、従来の連続発振Ｃ０２レーザーを用いた気相
法による微粒子生成法の反応容器の概略図。
（符号の説明）
１１・・・・・・０口、レーザー
１２・・・・・・レーザー光、
１３・・・・・・ＢａＦｚレンズ、
・・・・・・照射反応容器、
・・・・・・試料気体、
・・・・・・絞り、
・・・・・・にＢｒ窓板、
・・・・・・補集容器。
第１図
第２図
粒径
（ｐｍ）
第３図
フィルターへ
↑
反応ガス導入口Fig. 1 is a schematic diagram of the apparatus used in the example of the present invention, Fig. 2 is a graph showing the particle size distribution of Mo fine particles obtained in the example of the present invention, and Fig. 3 is a graph showing the particle size distribution of Mo fine particles obtained in the example of the present invention. FIG. 2 is a schematic diagram of a reaction vessel for a gas-phase microparticle generation method using an oscillating C02 laser. (Explanation of symbols) 11...0 mouth, laser 12...laser light, 13...BaFz lens, ...irradiation reaction vessel, ... ...sample gas, ...diaphragm, ...Br window plate, ...collection container. Figure 1 Figure 2 Particle size (pm) Figure 3 To the filter ↑ Reaction gas inlet
Claims (1)
素（ＣＳ＿２）又は硫化水素（Ｈ＿２Ｓ）とを含む混合
ガスにレーザー光を照射して二硫化モリブデン（ＭｏＳ
＿２）の微粒子を製造する方法。[Claims] A mixed gas containing molybdenum carbonyl [Mo(CO)_6] and carbon disulfide (CS_2) or hydrogen sulfide (H_2S) is irradiated with laser light to produce molybdenum disulfide (MoS).
_2) A method for producing fine particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7751889A JPH0637304B2 (en) | 1989-03-29 | 1989-03-29 | Method for producing molybdenum disulfide fine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7751889A JPH0637304B2 (en) | 1989-03-29 | 1989-03-29 | Method for producing molybdenum disulfide fine particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02255537A true JPH02255537A (en) | 1990-10-16 |
| JPH0637304B2 JPH0637304B2 (en) | 1994-05-18 |
Family
ID=13636188
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7751889A Expired - Lifetime JPH0637304B2 (en) | 1989-03-29 | 1989-03-29 | Method for producing molybdenum disulfide fine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0637304B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001038940A3 (en) * | 1999-11-24 | 2002-01-10 | Yeda Res & Dev | Method for surface patterning using a focused laser |
-
1989
- 1989-03-29 JP JP7751889A patent/JPH0637304B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001038940A3 (en) * | 1999-11-24 | 2002-01-10 | Yeda Res & Dev | Method for surface patterning using a focused laser |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0637304B2 (en) | 1994-05-18 |
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