JPS6320573B2 - - Google Patents
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- Publication number
- JPS6320573B2 JPS6320573B2 JP55040142A JP4014280A JPS6320573B2 JP S6320573 B2 JPS6320573 B2 JP S6320573B2 JP 55040142 A JP55040142 A JP 55040142A JP 4014280 A JP4014280 A JP 4014280A JP S6320573 B2 JPS6320573 B2 JP S6320573B2
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- Prior art keywords
- laser beam
- gas
- inert gas
- present
- powder
- Prior art date
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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
- 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
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Electromagnetism (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Optics & Photonics (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Carbon And Carbon Compounds (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Glanulating (AREA)
Description
【発明の詳細な説明】
本発明は、金属酸化物、及び炭化物並びに半導
体等高融点、超硬物質を不活性ガス雰囲気中で
CO2ガスレーザー光線によつて加熱蒸発させて、
1000Å以下の超微粒粉を製造する方法に係わるも
のである。DETAILED DESCRIPTION OF THE INVENTION The present invention provides high melting point, ultra-hard materials such as metal oxides, carbides, and semiconductors in an inert gas atmosphere.
By heating and evaporating CO 2 gas with a laser beam,
This relates to a method for producing ultrafine powder of 1000 Å or less.
ガス蒸発法による金属及び合金の超微粒粉の製
造法は、本発明者の一部等による発明、特許（特
公昭47−27718号参照）が存在し、それによつて
種々の金属の超微粉が製造され、磁性材料、超電
導体材料、化学触媒、粉末治金材料、ロケツト燃
焼材等の固体材料としての用途に利用されてい
る。 There are inventions and patents (see Japanese Patent Publication No. 47-27718) made by some of the present inventors regarding the method for producing ultrafine powders of metals and alloys by the gas evaporation method. It is manufactured and used as a solid material such as magnetic materials, superconductor materials, chemical catalysts, powder metallurgy materials, and rocket combustion materials.
本発明では、対象とする物質を金属酸化物及び
炭化物、並びに半導体を主たるものとし、これを
不活性ガス雰囲気中において、その加熱蒸発のた
めCO2ガスレーザー光線を用いることを特徴とす
る。 The present invention is characterized in that the target substances are mainly metal oxides, carbides, and semiconductors, and a CO 2 gas laser beam is used to heat and evaporate them in an inert gas atmosphere.
例えばSi3N4，BN，SiC，Ｗ，Ｃ等の1000Å以
下の超微粒粉は焼結体材料として種々の優れた性
質を示すことが予想されているが、その実現には
純粋で、表面が清浄な超微粒粉を大量に製造する
ことが必要である。その方法は個々の物質ごとに
色色な方法が報告されているが、化学的過程を用
いているものが多く、純粋、清浄なものを得るこ
とが困難であつた。 For example, ultrafine powders of 1000 Å or less, such as Si 3 N 4 , BN, SiC, W, and C, are expected to exhibit various excellent properties as sintered materials, but in order to achieve this, pure and surface It is necessary to produce a large amount of clean ultrafine powder. Various methods have been reported for each substance, but most of them use chemical processes, making it difficult to obtain pure and clean substances.
一方ガス蒸発法によれば、対象とする物質を希
ガス中で加熱蒸発するので、その製造過程中に不
純物の混入や、表面のよごれは生ずる可能性はな
く、広範な物質に適用できることは、金属及び合
金の製造において実証されている。 On the other hand, according to the gas evaporation method, the target substance is heated and evaporated in a rare gas, so there is no possibility of contamination with impurities or surface staining during the manufacturing process, and it can be applied to a wide range of substances. Proven in metal and alloy production.
この方法を、金属酸化物、及び炭化物並びに半
導体のような金属より高融点、超硬物質で且つ、
電気絶縁体謂ゆる耐火物材料に適用るためにはそ
の加熱手段を考慮せねばならない。 This method can be applied to ultrahard substances with a higher melting point than metals, such as metal oxides and carbides, and semiconductors, and
For application to electrical insulators, so-called refractory materials, the heating means must be considered.
従来、金属及び合金のガス蒸発法に用いられて
いる加熱源としては、
(1) 抵抗加熱、
(2) プラズマジエツト加熱、
(3) インダクシヨン加熱、があるが、
本発明の対象とする高融点化合物に対しては、
上記(1)は、加熱抵抗体自体の融点または分解点以
上の加熱温度を必要とするため、(2)は化合物は金
属に比べて、融解した場合に粘性が小さく、且
つ、密度が低いので、プラズマジエツトの高速気
流に吹き飛ばされて、飛沫になりやすいため、(3)
は、化合物は多くが電気絶縁体であるため、イン
ダクシヨン電流が流れないため、それぞれ不適当
である。 Heat sources conventionally used in gas evaporation methods for metals and alloys include (1) resistance heating, (2) plasma jet heating, and (3) induction heating, but these are the subject of the present invention. For high melting point compounds,
(1) above requires a heating temperature higher than the melting point or decomposition point of the heating resistor itself, and (2) is because compounds have lower viscosity and density when melted than metals. (3) Because it is easily blown away by the high-speed airflow of the plasma jet and becomes droplets.
are unsuitable because most of the compounds are electrical insulators and therefore do not allow induction current to flow.
本発明者等は、上記の各欠点を除去するため、
種々研究の結果、本発明を完成したのである。 In order to eliminate each of the above-mentioned drawbacks, the present inventors have
As a result of various researches, the present invention was completed.
本発明ではCO2レーザー光線は、波長10.6μを
中心とするエネルギー密度の高い赤外光線を加熱
源として利用するものである。 In the present invention, the CO 2 laser beam uses as a heating source an infrared ray having a wavelength of 10.6 μm and having a high energy density.
CO2レーザーの発生する赤外線は、本発明の対
象とする高融点化合物には、一般によく吸収さ
れ、そのエネルギー物質の中で熱に変換される。 The infrared rays generated by the CO 2 laser are generally well absorbed by the high melting point compounds targeted by the present invention, and are converted into heat within the energetic substance.
レーザー光の理論温度は、約20000℃に達する
から、蒸発物質を充分な高温に加熱することがで
きる。また、光による非接触加熱であるから、蒸
発物質に対する不純物の混入や飛散もない。 Since the theoretical temperature of laser light reaches approximately 20,000°C, it is possible to heat the vaporized substance to a sufficiently high temperature. Furthermore, since non-contact heating is performed using light, there is no contamination or scattering of impurities into the evaporated substance.
次に本発明の実施例を図面を参照して詳述す
る。第１図にみるように、大気と隔絶密閉される
ようにした容器１中を不活性ガス雰囲気とし、こ
こで被処理物をガス蒸発せしめるのであつて、そ
の下部を微粉体の発生室２とする外型台形円筒３
とし、ここに複数個の突出部３ａ，３ｂ，３ｃ…
…を設け、その突出面にCO2レーザー光線を導入
する窓４ａ，４ｂ，４ｃ……が取付けられてい
る。 Next, embodiments of the present invention will be described in detail with reference to the drawings. As shown in Fig. 1, an inert gas atmosphere is created in a container 1 which is sealed and isolated from the atmosphere, and the object to be treated is evaporated here, and the lower part is a fine powder generation chamber 2. External trapezoidal cylinder 3
Here, a plurality of protrusions 3a, 3b, 3c...
... is provided, and windows 4a, 4b, 4c, ... for introducing the CO 2 laser beam are attached to the protruding surface thereof.
この密閉容器１の底部中心には、水冷銅製のル
ツボ７が下方から挿入自在に取付けられ、その上
方に被処理物質Ｍを載置するようになつている。
９，９はその水冷装置であり、適宜の処から冷水
を供給し、且つ、排出せしめるようにしてある。 A crucible 7 made of water-cooled copper is attached to the center of the bottom of the closed container 1 so as to be freely inserted from below, and a substance M to be treated is placed above the crucible 7.
Reference numerals 9 and 9 are water cooling devices, which supply and discharge cold water from appropriate locations.
密閉容器１の上方には、下部の微細粉発生室２
において被処理物Ｍが加熱蒸発せしめられ、発生
した超微粉が上昇する煙突状室１になつており、
ここには、上方より超微粉の採取器として、液体
窒素冷却捕集器１５が垂下挿入、取出自在に上部
蓋体１４に取付けられている。 Above the airtight container 1 is a lower fine powder generation chamber 2.
The object to be treated M is heated and evaporated in a chimney-shaped chamber 1 in which the generated ultrafine powder rises.
Here, a liquid nitrogen cooling collector 15 is attached to the upper lid 14 so as to be freely inserted and removed from above as a collector for ultrafine powder.
また、上述の下部台形円筒部３に設けられた突
出部３ａ，３ｂ，３ｃ……には複数個のCO2レー
ザー光線導入窓４ａ，４ｂ，４ｃ……が設けら
れ、これは、ゲルマニウムまたは、NaCの結
晶からなつている。そして、これらの窓にはシヤ
ツターが設けられるか、又はCO2ガスレーザー光
線照射器１２に点滅器を取付けるか、または両者
にCO2ガスレーザー光線調整装置を取付けて、被
処理物Ｍのために必要に応じて照射光の増減を調
節自在とするものである。 In addition, a plurality of CO 2 laser beam introduction windows 4a, 4b, 4c... are provided in the protrusions 3a, 3b, 3c... provided on the lower trapezoidal cylindrical part 3, which are made of germanium or NaC. It is made of crystals. These windows are provided with shutters, or a blinker is attached to the CO 2 gas laser beam irradiator 12, or a CO 2 gas laser beam adjustment device is attached to both of them, so as to adjust the amount of light necessary for the object M to be processed. The amount of irradiated light can be increased or decreased accordingly.
図面中５は、上方排気バルブ、１０は下方排気
バルブであり、６ａ，６ｂ，６ｃ……は、台形円
筒３に取付けた突出部３′内に向つて不活性ガス
（例えばアルゴンガス）噴出管であり、８は送気
バルブであり、通常は、６ａ，６ｂ，６ｃ……と
同様の不活性ガスを送気せしめるようになつてい
る。 In the drawing, 5 is an upper exhaust valve, 10 is a lower exhaust valve, and 6a, 6b, 6c, . 8 is an air supply valve, which is normally adapted to supply inert gas similar to 6a, 6b, 6c, . . . .
１１は容器１内の圧力計であり、１２はCO2ガ
スレーザー光線源である。１３は反射鏡であり、
CO2ガスレーザー光線を窓４ａ，４ｂ，４ｃ……
から的確に微細粉発生室２内の被処理物質Ｍに照
射せしめるためのものである。１６は下方の蓋体
兼水冷銅ルツボ７の取付部である。 11 is a pressure gauge inside the container 1 , and 12 is a CO 2 gas laser beam source. 13 is a reflecting mirror;
CO 2 gas laser beam is applied to windows 4a, 4b, 4c...
This is for precisely irradiating the substance M to be treated in the fine powder generation chamber 2. Reference numeral 16 denotes a mounting portion for the lower lid and water-cooled copper crucible 7.
次に本発明の動作手順を述べると、密閉容器１
内下方の水冷銅ルツボ７上に、被処理物質Ｍを載
置し、容器１の底部蓋体６によつて固定する。次
いで本密閉容器１の５，６ａ，６ｂ，８の各バル
ブをすべて閉じ、次いで下方排気バルブ１０より
容器内部を10-5Torr程度に排気する。 Next, the operating procedure of the present invention will be described .
The substance M to be treated is placed on the inner lower water-cooled copper crucible 7 and fixed with the bottom lid 6 of the container 1 . Next, all valves 5, 6a, 6b, and 8 of the sealed container 1 are closed, and then the inside of the container is evacuated to about 10 -5 Torr using the lower exhaust valve 10.
排気が終れば、排気バルブ１０を閉じてアルゴ
ンガス等の不活性ガスを８，６ａ，６ｂ，６ｃ…
…等より導入する。この際上方の排気バルブ５を
開いて排気しながら８の送気バルブから上記不活
性ガスを送気し、容器内の圧力を圧力計１１を見
乍ら、10〜500Torrの間の一定の値になるように
調整する。 When the exhaust is finished, the exhaust valve 10 is closed and an inert gas such as argon gas is supplied to the gases 8, 6a, 6b, 6c...
... etc. will be introduced. At this time, while opening the upper exhaust valve 5 and exhausting air, the above-mentioned inert gas is supplied from the air supply valve 8, and the pressure inside the container is adjusted to a constant value between 10 and 500 Torr while watching the pressure gauge 11. Adjust so that
次いで、水平においたCO2レーザー光源１２の
CO2レーザー光源を作動せしめ、鏡１３を調整し
て矢印のように、レーザー光線を被処理物質Ｍ上
に集中照射すると、被処理物質は加熱されて、煙
状に超微粉が発生し、気流に乗つて上部の煙突状
室１中に上昇する。その間に該室中に垂下設置さ
れた液体窒素冷却採取器１５の表面に超微粉が熱
沈着する。 Next, the CO 2 laser light source 12 placed horizontally
When the CO 2 laser light source is activated and the mirror 13 is adjusted to irradiate the laser beam concentratedly onto the material M to be treated as shown by the arrow, the material to be treated is heated and ultrafine powder is generated in the form of smoke, which is released into the airflow. Get on it and ascend into the chimney-shaped chamber 1 at the top. During this time, ultrafine powder is thermally deposited on the surface of the liquid nitrogen cooling collector 15 suspended in the chamber.
次にこの附着した超微粉を適時本装置の作動を
止め、上記液体窒素冷却採取器を上方の蓋体１４
のフランジをぬき取つて取出し、その表面に附着
した目的の超微粉をかき落して捕集する。 Next, the attached ultrafine powder is removed from the upper cover 14 by stopping the operation of the device and moving the liquid nitrogen cooling collector to the upper lid 14.
Remove the flange and scrape off the target ultrafine powder adhering to its surface to collect it.
次に本発明方法の具体的実施例の一例あげる
と、CO2レーザー光源１２に100W光源を使用し、
試料としてSiCを用いた場合につき説明する。 Next, to give an example of a specific embodiment of the method of the present invention, a 100W light source is used as the CO 2 laser light source 12,
The case where SiC is used as a sample will be explained.
照射する試料上の面積は、レンズを用いて、１
mm2にしぼり、照射強度は10KW／cm2にした。 The area on the sample to be irradiated is 1
mm 2 and the irradiation intensity was 10KW/cm 2 .
SiCは約10μの市販の粉末をそのまゝ冷却ルツ
ボ７上にのせ、上記の手順に従つて加熱蒸発を行
つた。 A commercially available SiC powder of about 10 μm was placed as it was on the cooling crucible 7, and heated and evaporated according to the above procedure.
本件の雰囲気不活性ガスは、Arを用い、圧力
10〜500Torrで粒度はArガス圧により第３図
（グラフ）の如く100Å〜500Åと変化する。収集
量は５mg／１分である。 The inert gas atmosphere in this case is Ar, and the pressure
At 10 to 500 Torr, the particle size changes from 100 to 500 Å as shown in Figure 3 (graph) depending on the Ar gas pressure. The amount collected is 5 mg/min.
これによつてできた超微粒粉はβSiCと少量の
Siの粉状の混合物であつた。 The resulting ultrafine powder contains βSiC and a small amount of
It was a powdered mixture of Si.
その他の被処理物の実施例としては、B4C，
NbＣ，TiC，TaC，Ｗ，Ｃ，BN，Ａ2O3，
MgO，ZrO，La6B，Si3N4，HfCがあり、いず
れも、超微粉結晶の生成が確認された。 Examples of other processed materials include B 4 C,
N b C, TiC, TaC, W, C, BN, A 2 O 3 ,
There were MgO, ZrO, La 6 B, Si 3 N 4 and HfC, and the formation of ultrafine crystals was confirmed in all of them.
上記の微粉の素材物質は、いずれも耐火物また
は、超硬物質であつて、その加工はきわめて困難
で粉体の焼結により行う以外その手段がないし、
また、それも高温焼結という困難がある。 The above-mentioned fine powder materials are all refractories or super hard materials, and processing them is extremely difficult and the only way to do it is by sintering the powder.
Moreover, it also has the difficulty of high-temperature sintering.
そこで本発明方法によつて製造した超微粉を原
料とすることによつて、添加物を加えることなし
に焼結を容易にすることができる。 Therefore, by using the ultrafine powder produced by the method of the present invention as a raw material, sintering can be facilitated without adding additives.
一般に加熱手段に光学的方法を用いることは、
しばしば行なわれることである。 Generally, using an optical method as a heating means,
This is often done.
即ちアーク、イメージ炉、太陽炉等があるが、
本発明においてCO2ガスレーザーを用いた理由は
その光エネルギーがきわめて効率的に使用できる
こととその取扱いがこれ又容易であることであつ
て、今後種々の使用形態が開発され得るものであ
ることが重要な要因である。 In other words, there are arc, image furnace, solar furnace, etc.
The reason for using a CO 2 gas laser in the present invention is that its light energy can be used extremely efficiently and that it is easy to handle, and it is believed that various forms of use can be developed in the future. This is an important factor.
第１図は、本発明方法の実施例装置の縦断面図
であり、第２図は上方からみた平面図、第３図
（グラフ）は、不活性ガス圧力と発生する微粒粉
の粒度の関係を示すものである。（即ちガス圧が
大きい程大きい粒子が得られることを示すもので
ある。）
１……密閉容器、１……煙突状室、２……微細
粉発生室、３……台形円筒部、４ａ，４ｂ，４ｃ
……窓、５……上方排気バルブ、６ａ，６ｂ，６
ｃ……不活性ガス噴出管、７……水冷銅ルツボ、
８……排気バルブ、１２……CO2レーザー光源、
１５……液体窒素冷却採集器。
Fig. 1 is a longitudinal cross-sectional view of an example device of the method of the present invention, Fig. 2 is a plan view seen from above, and Fig. 3 (graph) is the relationship between inert gas pressure and particle size of generated fine powder. This shows that. (In other words, this indicates that the larger the gas pressure, the larger the particles obtained.) 1 ... Sealed container, 1... Chimney-shaped chamber, 2... Fine powder generation chamber, 3... Trapezoidal cylindrical part, 4a, 4b, 4c
...Window, 5...Upper exhaust valve, 6a, 6b, 6
c...Inert gas ejection pipe, 7...Water-cooled copper crucible,
8... Exhaust valve, 12... CO 2 laser light source,
15...Liquid nitrogen cooling collector.
Claims (1)
活性ガス雰囲気中においてCO2ガスレーザー光線
によつて加熱蒸発せしめ、超微粒子となし、これ
を適宜採集することを特徴とするレーザー光線を
用いた超微粒粉の製造方法。1. A process for producing ultrafine powder using a laser beam, characterized in that metal oxides, carbides, and semiconductor substances are heated and evaporated using a CO 2 gas laser beam in an inert gas atmosphere to form ultrafine particles, which are appropriately collected. Production method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4014280A JPS56136634A (en) | 1980-03-29 | 1980-03-29 | Production of ultra-fine powder and particle using laser beam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4014280A JPS56136634A (en) | 1980-03-29 | 1980-03-29 | Production of ultra-fine powder and particle using laser beam |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS56136634A JPS56136634A (en) | 1981-10-26 |
| JPS6320573B2 true JPS6320573B2 (en) | 1988-04-28 |
Family
ID=12572520
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4014280A Granted JPS56136634A (en) | 1980-03-29 | 1980-03-29 | Production of ultra-fine powder and particle using laser beam |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS56136634A (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5953607A (en) * | 1982-09-22 | 1984-03-28 | Sintokogio Ltd | Production of metallic powder or metallic oxide powder |
| JPS5985808A (en) * | 1982-11-08 | 1984-05-17 | Pioneer Electronic Corp | Production of ultrafine metallic particle |
| JPS59129701A (en) * | 1983-01-13 | 1984-07-26 | Tanaka Kikinzoku Kogyo Kk | Production of powder of metal or nonmetal or alloy thereof |
| JPS59129702A (en) * | 1983-01-13 | 1984-07-26 | Tanaka Kikinzoku Kogyo Kk | Production of powder of metal or nonmetal or alloy thereof |
| JPS59206042A (en) * | 1983-05-07 | 1984-11-21 | Sumitomo Electric Ind Ltd | Fine powder manufacturing method and manufacturing equipment |
| JPS6254005A (en) * | 1985-09-02 | 1987-03-09 | Hitachi Ltd | Production of hyperfine particles |
| CN1250701A (en) * | 1999-11-18 | 2000-04-19 | 华中理工大学 | Process and equipment for preparing superfine powder by heating and evaporation |
| CN107225242A (en) * | 2017-05-19 | 2017-10-03 | 淮阴工学院 | The method and implant of 3D printing in-situ authigenic multi-stage nano ceramic phase reinforcing titanium alloy bone implant |
-
1980
- 1980-03-29 JP JP4014280A patent/JPS56136634A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS56136634A (en) | 1981-10-26 |
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