JP3100084B2 - Ultrafine particle manufacturing equipment - Google Patents
Ultrafine particle manufacturing equipmentInfo
- Publication number
- JP3100084B2 JP3100084B2 JP03308174A JP30817491A JP3100084B2 JP 3100084 B2 JP3100084 B2 JP 3100084B2 JP 03308174 A JP03308174 A JP 03308174A JP 30817491 A JP30817491 A JP 30817491A JP 3100084 B2 JP3100084 B2 JP 3100084B2
- Authority
- JP
- Japan
- Prior art keywords
- particles
- ultrafine particles
- powder
- plasma
- raw material
- 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 - Fee Related
Links
- 239000011882 ultra-fine particle Substances 0.000 title claims description 41
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000000843 powder Substances 0.000 claims description 37
- 239000002245 particle Substances 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 28
- 239000011147 inorganic material Substances 0.000 claims description 17
- 239000007769 metal material Substances 0.000 claims description 16
- 239000012159 carrier gas Substances 0.000 claims description 11
- 229910010272 inorganic material Inorganic materials 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 20
- 238000007599 discharging Methods 0.000 description 13
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 11
- 229910052786 argon Inorganic materials 0.000 description 10
- 229910052581 Si3N4 Inorganic materials 0.000 description 9
- 239000000956 alloy Substances 0.000 description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 230000010355 oscillation Effects 0.000 description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 5
- 229910018487 Ni—Cr Inorganic materials 0.000 description 4
- 238000011109 contamination Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- -1 WC and SiC Chemical class 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 229910002060 Fe-Cr-Al alloy Inorganic materials 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 2
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000011027 product recovery Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 229910021484 silicon-nickel alloy Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Landscapes
- Physical Or Chemical Processes And Apparatus (AREA)
- Powder Metallurgy (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、無機材料または金属材
料の超微粒子を製造する装置に関する。本発明は具体的
にはＲＦプラズマ法による無機材料または金属材料の粉
末からこれらの超微粒子を製造する装置における粉末原
料の放出装置の改良に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for producing ultrafine particles of an inorganic or metallic material. More specifically, the present invention relates to an improvement in an apparatus for discharging a powder raw material in an apparatus for producing these ultrafine particles from powder of an inorganic material or a metal material by an RF plasma method.
【０００２】また本発明は、無機材料または金属材料の
超微粒子で表面が被覆された無機材料または金属材料の
粒子の製造装置にも関する。[0002] The present invention also relates to an apparatus for producing particles of an inorganic or metallic material whose surface is coated with ultrafine particles of an inorganic or metallic material.
【０００３】[0003]
【従来の技術】ＲＦプラズマを用いる超微粒子の製造は
これまでに多くの先行技術文献中に示されている。これ
らの技術文献中で、例えば特開昭６２−１７１９０２号
公報、特開昭６３−８５００７号公報には原料供給管が
プラズマ焔とは離れた場所に設けられている装置が示さ
れているが、この装置では生成する超微粒子の装置への
付着により円滑な操業が妨げられることから、これら装
置を改良するものとして特開平２−２０３９３２号公報
において、原料供給管をプラズマ焔中に設けた装置が提
案されている。2. Description of the Related Art The production of ultrafine particles using RF plasma has been described in many prior art documents. Among these technical documents, for example, JP-A-62-171902 and JP-A-63-85007 disclose apparatuses in which a raw material supply pipe is provided at a place away from a plasma flame. In this apparatus, the smooth operation is hindered by the adhesion of the generated ultrafine particles to the apparatus. To improve these apparatuses, Japanese Patent Application Laid-Open No. 2-203932 discloses an apparatus in which a raw material supply pipe is provided in a plasma flame. Has been proposed.
【０００４】[0004]
【発明が解決しようとする課題】上述した先行技術文献
の前二者における課題であった円滑な操業の達成という
観点からすれば後者の文献に記載の装置は或る程度の成
果を得るものであったが、原料供給管をプラズマ焔中に
設けるという点で致命的な欠点を有する。すなわち、プ
ラズマ焔中では不可避的に供給管自体が加熱され、これ
が気化して超微粒子中にコンタミネーションを起すこと
になる。そして超微粒子の用途によってはかかるコンタ
ミネーションは生成された超微粒子に決定的な欠陥をも
たらすのである。From the viewpoint of achieving a smooth operation, which has been a problem in the former two of the above-mentioned prior art documents, the device described in the latter document can obtain a certain result. However, it has a fatal disadvantage in that the raw material supply pipe is provided in the plasma flame. In other words, the supply tube itself is inevitably heated in the plasma flame, and this is vaporized and causes contamination in the ultrafine particles. And, depending on the application of the ultrafine particles, such a contamination causes a critical defect in the generated ultrafine particles.
【０００５】[0005]
【課題を解決するための手段】上記した課題を解決する
ために本発明者らは鋭意研究した結果ＲＦプラズマ法に
よって形成されるプラズマ焔の直上に特定の構成の粉末
原料の放出装置の放出口を設けることによって高能率で
かつなんらの原料の放出装置によるコンタミネーション
の危険なしに超微粒子を製造しうることを見出して本発
明を完成した。Means for Solving the Problems In order to solve the above-mentioned problems, the inventors of the present invention have conducted intensive studies, and as a result, a discharge port of a discharge device for a powdery raw material having a specific configuration immediately above a plasma flame formed by an RF plasma method. The present inventors have found that ultrafine particles can be produced with high efficiency and without the risk of contamination by any kind of raw material discharging device, thereby completing the present invention.
【０００６】すなわち、本発明は、ＲＦプラズマ法によ
って形成されるプラズマ焔の直上に、無機材料または金
属材料の粉末原料の放出装置の放出口が設置され、供給
される粉末原料はキャリヤガスにより旋回運動が与えら
れてプラズマ焔中に供給されるようにされた、該粉末原
料から無機材料または金属材料の超微粒子を製造する装
置に関する。That is, according to the present invention, a discharge port of a discharge device of a powder material of an inorganic material or a metal material is provided immediately above a plasma flame formed by an RF plasma method, and the supplied powder material is swirled by a carrier gas. The present invention relates to an apparatus for producing ultrafine particles of an inorganic or metallic material from a powdered raw material which is provided with a motion and supplied in a plasma flame.
【０００７】更にまた本発明は上記のようにして形成さ
れた超微粒子流と、この超微粒子で表面を被覆しようと
する無機材料また金属材料の母材粒子とを接触させ、も
って超微粒子で表面が被覆された母材粒子を製造するた
めの装置すなわち、ＲＦプラズマ法によって形成される
プラズマ焔の直上に、無機材料また金属材料の粉末原料
の放出装置の放出口が設置され、供給される粉末原料は
キャリヤガスにより旋回運動が与えられてプラズマ焔中
に供給されるようにされ、そしてプラズマ焔の下流に超
微粒子によって表面を被覆しようとする無機材料または
金属材料母材の粉末を導入する装置を備え、生成した超
微粒子と導入された母材の粉末とが接触せしめられるよ
うにされた、母材の粒子の表面を超微粒子で被覆する装
置にも関する。Further, the present invention provides a method of contacting a superfine particle stream formed as described above with a base material particle of an inorganic material or a metal material whose surface is to be coated with the ultrafine particles. An apparatus for producing a base material particle coated with, that is, an emission port of an emission apparatus for a powder material of an inorganic material or a metal material is provided immediately above a plasma flame formed by an RF plasma method, and the supplied powder is provided. The raw material is provided with a swirling motion by a carrier gas to be supplied into a plasma flame, and an apparatus for introducing a powder of an inorganic material or a metal material base material whose surface is to be coated with ultrafine particles downstream of the plasma flame. The present invention also relates to an apparatus for coating the surface of particles of a base material with ultrafine particles, wherein the generated ultrafine particles are brought into contact with the introduced base material powder.
【０００８】本発明の装置は、上記の構成によって超微
粒子の製造および母材の粒子の表面に超微粒子が被覆さ
れた粒子が、原料供給管がプラズマ焔に接することによ
る原料供給管の構成材料の超微粒子中へのコンタミネー
ションの危険がなく超微粒子を円滑に製造しうるもので
ある。[0008] The apparatus of the present invention is characterized in that ultrafine particles are produced by the above-described structure and the particles of the base material are coated with ultrafine particles. It is possible to produce ultrafine particles smoothly without risk of contamination in the ultrafine particles.
【０００９】本発明の装置によって製造される無機材料
または金属材料の超微粒子としては、種々の無機物質、
例えば酸化物であるＡｌ2Ｏ3、ＢｅＯ、ＳｉＯ2、Ｍｇ
Ｏ、ＺｒＯ2、Ｙ2Ｏ3、ＣａＯなど、窒化物であるＳｉ3
Ｎ4、ＡｌＮ、ＢＮなど、炭化物であるＷＣ、ＳｉＣな
ど、ほう素化物であるＢＰ、ＢＮなど、酸窒化物である
ＳＩＡＬＯＮ（サイアロン）など、単体元素であるＣ、
Ｂなどおよび種々の金属例えばＳｉ、Ａｌ、Ｎｉ Ｃ
ｏ、Ｆｅ、Ｔｉ、Ｃｕ、Ａｕ、Ａｇ、Ｗなどおよび金属
間化合物および合金の種々のもの、例えばＦｅ−Ｎｉ−
Ｓｉ合金、Ｆｅ−Ｃｒ−Ａｌ合金、Ｆｅ−Ｃｒ−Ｍｏ合
金、Ｆｅ−Ｎｉ−Ｃｒ合金、Ｎｉ−Ｃｒ合金、Ａｌ−Ｔ
ｉ合金など、並びにこれらの材料を複合したものなどの
超微粒子が挙げられる。As the ultrafine particles of the inorganic or metallic material produced by the apparatus of the present invention, various inorganic substances,
For example, oxides of Al 2 O 3 , BeO, SiO 2 , Mg
Si 3 which is a nitride such as O, ZrO 2 , Y 2 O 3 and CaO
N 4 , AlN, BN, etc., carbides such as WC and SiC, borides such as BP and BN, and oxynitrides such as SIALON (Sialon)
B and various metals such as Si, Al, Ni C
o, Fe, Ti, Cu, Au, Ag, W, etc. and various intermetallic compounds and alloys, such as Fe-Ni-
Si alloy, Fe-Cr-Al alloy, Fe-Cr-Mo alloy, Fe-Ni-Cr alloy, Ni-Cr alloy, Al-T
Ultrafine particles such as an i-alloy and a composite of these materials.
【００１０】もう一つの本発明の装置によって得られる
無機材料または金属材料母材の粒子の表面を超微粒子で
被覆した粒子の、該母材の粒子を構成する材料として
は、耐火物またはセラミックスと呼ばれる総べての無機
物質、例えば酸化物であるＡｌ 2Ｏ3、ＺｒＯ2、Ｓｉ
Ｏ2、ＢｅＯ、ＭｇＯ、ＣａＯ、Ｙ2Ｏ3など、窒化物で
あるＳｉ3Ｎ4、ＡｌＮ、ＢＮなど、炭化物であるＳｉ
Ｃ、ＷＣなど、ほう素化物であるＢＰ、ＢＮなど、酸窒
化物であるＳＩＡＬＯＮ（サイアロン）など、種々の粘
土鉱物、例えばカオリナイト、モンモリロナイトなど、
各種のフェライトなどの磁性材料、ガーネット、コラン
ダム、などの天然または人工鉱物、単体元素、例えばダ
イヤモンド、黒鉛など、単体金属、例えばＳｉ、Ｎｉ、
Ｃｏ、Ｆｅ、Ｔｉ、Ａｌ、Ｃｕ、Ａｇ、Ａｕ、Ｗなど、
および金属間化合物および合金、例えばＦｅ−Ｎｉ−Ｓ
ｉ合金、Ｆｅ−Ｃｒ−Ａｌ合金、Ｆｅ−Ｃｒ−Ｍｏ合
金、Ｆｅ−Ｎｉ−Ｃｒ合金、Ｎｉ−Ｃｒ合金などの材料
並びにこれらの材料を複合したものの粉末が挙げられ
る。[0010] obtained by another device of the invention
Ultrafine particles on the surface of particles of inorganic or metallic materials
As a material constituting the particles of the base material of the coated particles
Are all inorganic materials called refractories or ceramics
Substance, for example, Al which is an oxide TwoOThree, ZrOTwo, Si
OTwo, BeO, MgO, CaO, YTwoOThreeSuch as nitride
Some SiThreeNFour, AlN, BN and other carbides
Oxynitrides such as BP and BN such as C and WC
Viscosities such as SIALON
Earth minerals such as kaolinite and montmorillonite,
Magnetic materials such as various ferrites, garnet, coran
Natural or artificial minerals such as dams, single elements, e.g.
Simple metals such as earmond and graphite, for example, Si, Ni,
Co, Fe, Ti, Al, Cu, Ag, Au, W, etc.
And intermetallic compounds and alloys such as Fe-Ni-S
i alloy, Fe-Cr-Al alloy, Fe-Cr-Mo alloy
Materials such as gold, Fe-Ni-Cr alloy, Ni-Cr alloy
And powders of composites of these materials
You.
【００１１】上記した構成の本発明の超微粒子の製造装
置の一つの具体例は、図１で示される。One specific example of the apparatus for producing ultrafine particles of the present invention having the above-mentioned structure is shown in FIG.
【００１２】図１において、装置の全体はプラズマトー
チＡ、反応チャンバーＢ、冷却部Ｃ、原料粉末放出装置
Ｄおよび製品回収部Ｅより成るものである。In FIG. 1, the whole apparatus is composed of a plasma torch A, a reaction chamber B, a cooling section C, a raw material powder discharging apparatus D and a product recovery section E.
【００１３】プラズマトーチＡは水冷式の石英二重管と
その外側を取巻く高周波発振コイルとで構成され、コイ
ルへの高周波電流の印加によって石英二重管内にプラズ
マ焔が生成する。このプラズマトーチの上部にガス導入
口を設けてプラズマ焔が集束するようにすることが好ま
しい。The plasma torch A comprises a water-cooled quartz double tube and a high-frequency oscillation coil surrounding the outside thereof, and a plasma flame is generated in the quartz double tube by applying a high-frequency current to the coil. It is preferable to provide a gas inlet on the upper part of the plasma torch so that the plasma flame is focused.
【００１４】このプラズマ焔の直上に原料粉末放出装置
Ｄが設置される。この原料粉末放出装置は図２で示され
る構成を有する。この原料粉末放出装置は適当な材質例
えば銅製の三重管より成り、外側管には冷却水が流れる
ように、中間管には旋回流発生用のガスが流れるよう
に、そして内管には原料粉末が搬送用ガスと共にプラズ
マトーチ内に導入されるように構成されている。すなわ
ち、冷却水は入口ａから外側管内に導入され、原料放出
装置を冷却して出口ｂから排出される。中間管には旋回
流発生用のガスがガス入口ｃから導入されるがその導入
方向はガス流路の断面のリング状の空間に対して接線方
向となるようにされ、そのことによって導入されたガス
流は旋回しながら下降し、その出口で旋回流となって放
出される。原料粉末は内管の上部からキャリアガスと共
に導入され、その出口で上記した旋回流となって放出さ
れた中間管からのガスの働きで旋回運動が与えられてプ
ラズマ焔中に供給されることになる。この原料粉末放出
装置Ｄを示す図２において、Ａ−Ａで切断した断面は図
３で示され、Ｂ−Ｂで切断した断面は図４で示される。
上記原料粉末放出装置の材質が耐熱材料の場合には冷却
水は不要である。A raw material powder discharging device D is installed immediately above the plasma flame. This raw material powder discharging apparatus has a configuration shown in FIG. This raw material powder discharging device is composed of a triple tube made of a suitable material such as copper, so that cooling water flows through the outer tube, gas for generating a swirling flow flows through the intermediate tube, and raw material powder flows through the inner tube. Is introduced into the plasma torch together with the carrier gas. That is, the cooling water is introduced from the inlet a into the outer pipe, cools the raw material discharger, and is discharged from the outlet b. The gas for generating a swirling flow is introduced into the intermediate pipe from the gas inlet c, and the introduction direction is set to be tangential to the ring-shaped space in the cross section of the gas flow path, thereby being introduced. The gas flow descends while swirling, and is discharged as a swirling flow at the outlet. The raw material powder is introduced together with the carrier gas from the upper part of the inner tube, and is swirled by the action of the gas emitted from the intermediate tube at the outlet as the above-mentioned swirling flow to be supplied into the plasma flame. Become. In FIG. 2 showing the raw material powder discharging apparatus D, a cross section cut along AA is shown in FIG. 3, and a cross section cut along BB is shown in FIG.
When the material of the raw material powder discharging device is a heat-resistant material, cooling water is unnecessary.
【００１５】このようにしてプラズマトーチ内に導入さ
れた原料粉末は生成したプラズマ焔内において、および
反応チャンバーＢ内において気化し、冷却部Ｃ内におい
て急冷されて超微粒子を生成する。このようにして生成
した超微粒子は製品回収部Ｅにおいて回収され取り出さ
れる。The raw material powder thus introduced into the plasma torch is vaporized in the generated plasma flame and in the reaction chamber B, and is rapidly cooled in the cooling section C to generate ultrafine particles. The ultrafine particles generated in this way are collected and taken out in the product collection section E.
【００１６】本発明の装置のもう一つの具体例は図５で
示される。この装置では、図１で示した装置に更にプラ
ズマ焔の下流に超微粒子によって表面を被覆しようとす
る無機材料または金属材料母材の粉末を導入するための
装置Ｆが設けられている。この装置Ｆから導入される母
材粉末はガス流で搬送されて反応チャンバーＢ内で生成
した超微粒子と流動状態で接触し、母材粉末の粒子の表
面が超微粒子で被覆されることになる。Another embodiment of the device of the present invention is shown in FIG. In this apparatus, the apparatus shown in FIG. 1 is further provided with an apparatus F for introducing a powder of an inorganic material or a metal material base material whose surface is to be coated with ultrafine particles downstream of the plasma flame. The base material powder introduced from the apparatus F is conveyed by a gas flow and comes into contact with the ultrafine particles generated in the reaction chamber B in a flowing state, so that the surfaces of the particles of the base material powder are coated with the ultrafine particles. .
【００１７】次に実施例によって本発明を更に詳細に説
明する。Next, the present invention will be described in more detail by way of examples.
【００１８】実施例１ この実施例で用いた装置は下記の構成を有する。すなわ
ち、図１において、プラズマトーチＡは内径５５mm、外
径７０mm、長さ２２０mmの石英二重管から成り、この外
側には高周波発振コイルが取付けられている。そしてこ
のプラズマトーチの上部にガス導入口が設けられてい
る。反応チャンバーＢは水冷式のステンレス二重管から
成り、その内径は１１０mm、長さは２００mmである。ま
た冷却部Ｃは水冷式のステンレス二重管から成り、その
内径は４４０mm、長さは８００mmである。冷却部Ｃの下
部に製品回収部Ｅが設けられ、吸引ポンプに接続されて
いて冷却部Ｃ内の超微粒子を吸引し、回収部Ｅ内に設け
られたフィルター上で超微粒子が取り出される。Embodiment 1 The apparatus used in this embodiment has the following configuration. That is, in FIG. 1, the plasma torch A is composed of a quartz double tube having an inner diameter of 55 mm, an outer diameter of 70 mm, and a length of 220 mm, and a high-frequency oscillation coil is mounted on the outside thereof. A gas inlet is provided above the plasma torch. The reaction chamber B is made of a water-cooled stainless steel double tube, and has an inner diameter of 110 mm and a length of 200 mm. The cooling section C is composed of a water-cooled stainless steel double tube, and has an inner diameter of 440 mm and a length of 800 mm. A product collection unit E is provided below the cooling unit C, and is connected to a suction pump to suck ultra-fine particles in the cooling unit C and to extract ultra-fine particles on a filter provided in the collection unit E.
【００１９】プラズマ焔の直上に設置される原料粉末放
出装置Ｄは銅製の三重管で内管の直径２mm、中間管の直
径４mm、外側管の直径２０mmを有し、外側管には冷却水
の入口および出口が設けられている。The raw material powder discharging device D installed immediately above the plasma flame is a copper triple tube having a diameter of an inner tube of 2 mm, a diameter of an intermediate tube of 4 mm, and a diameter of an outer tube of 20 mm. An inlet and an outlet are provided.
【００２０】この装置の、高周波発振コイルに４MHz、
８０KVAの高周波電流を印加し、プラズマトーチの上部
のガス導入口からアルゴンガス４０リットル／分、酸素
ガス５０リットル／分を噴出させてアルゴン−酸素プラ
ズマを発生させた。そして原料粉末の酸化イットリウム
（比表面積４.０m2／ｇ、比表面積径３１３nm）２０ｇ
／分をキャリアガス１０リットル／分と共に原料粉末放
出装置Ｄの内管より供給すると共に、旋回流発生のため
にアルゴンガス１０リットル／分を同装置の中間管より
供給した。高温プラズマ中で気化した酸化イットリウム
は、チャンバー内で凝縮し、生成した酸化イットリウム
超微粒子はフィルター上に集められ回収した。In this device, the high-frequency oscillation coil has a frequency of 4 MHz,
A high-frequency current of 80 KVA was applied, and argon-oxygen plasma was generated by ejecting 40 l / min of argon gas and 50 l / min of oxygen gas from a gas inlet above the plasma torch. 20 g of raw material powder yttrium oxide (specific surface area 4.0 m 2 / g, specific surface area diameter 313 nm)
/ Min together with 10 l / min of the carrier gas from the inner tube of the raw material powder discharging device D, and 10 l / min of the argon gas from the intermediate tube of the device to generate a swirling flow. The yttrium oxide vaporized in the high-temperature plasma was condensed in the chamber, and the generated ultrafine yttrium oxide particles were collected and collected on a filter.
【００２１】上記した操作によって比表面積（ＢＥＴ
法）２５m2／ｇ、比表面積径５０nmの酸化イットリウム
超微粒子が得られた。これを電子顕微鏡で観察したとこ
ろ、超微粒子は球形で未蒸発の原料粒子は認められなか
った。The specific surface area (BET)
Method) Yttrium oxide ultrafine particles having a specific surface area of 50 nm and a surface area of 25 m 2 / g were obtained. When this was observed with an electron microscope, the ultrafine particles were spherical and no unevaporated raw material particles were observed.
【００２２】比較例１ 上記実施例１と同様の操作を行なったが、旋回流発生の
ためのアルゴンガスは供給せず、その代りにキャリアガ
スとしてアルゴンガスを２０リットル／分の量で用い
た。Comparative Example 1 The same operation as in Example 1 was performed, except that argon gas for generating a swirling flow was not supplied, and instead, argon gas was used as a carrier gas at a rate of 20 l / min. .
【００２３】この条件によって比表面積１２m2／ｇ、比
表面積径１０４nmの酸化イットリウム超微粒子が得られ
た。これを電子顕微鏡により観察したところ、多数の未
蒸発の原料粒子が認められた。Under these conditions, ultrafine yttrium oxide particles having a specific surface area of 12 m 2 / g and a specific surface area of 104 nm were obtained. When this was observed with an electron microscope, a large number of unevaporated raw material particles were found.
【００２４】実施例 ２ この実施例では、窒化ケイ素に酸化アルミニウムを被覆
した。この実施例で用いた装置は、下記の構成を有す
る。すなわち、図５において、プラズマトーチＡは内径
５５mm、外径７０mm、長さ２２０mmの石英二重管から成
り、この外側には高周波発振コイルが取付けられてい
る。そして、このプラズマトーチの上部にガス導入口が
設けられている。反応チャンバーＢは、内径１１０mm、
長さは２００mmのステンレス二重管から成り、その中央
部に設けられた粉体供給口から、Ｆから供給される母材
粒子がキャリアガスに担持されて導入される。また冷却
部Ｃは水冷式のステンレス二重管から成り、その内径は
４４０mm、長さは８００mmである。冷却部Ｃの下部に製
品回収部Ｅが設けられ、吸引ポンプに接続されていて、
ＣおよびＤの場所において流動状態で超微粒子で被覆さ
れた母材粒子を吸引して、回収部Ｅ内に設けられたフィ
ルター上で集められ回収される。Example 2 In this example, silicon nitride was coated with aluminum oxide. The device used in this example has the following configuration. That is, in FIG. 5, the plasma torch A is composed of a quartz double tube having an inner diameter of 55 mm, an outer diameter of 70 mm, and a length of 220 mm, and a high-frequency oscillation coil is mounted on the outside thereof. A gas inlet is provided above the plasma torch. Reaction chamber B has an inner diameter of 110 mm,
The base material particles supplied from F are introduced by being carried by a carrier gas from a powder supply port provided at a central portion of the stainless steel double tube having a length of 200 mm. The cooling section C is composed of a water-cooled stainless steel double tube, and has an inner diameter of 440 mm and a length of 800 mm. A product recovery section E is provided below the cooling section C and is connected to a suction pump.
At the locations C and D, the base material particles coated with the ultrafine particles in a fluidized state are sucked and collected and collected on a filter provided in the collection section E.
【００２５】プラズマ焔の直上に設置される原料粉末放
出装置は、銅製の三重管で内管の直径２mm、中間管の直
径４mm、外側管の直径２０mmを有し、外側管には冷却水
の入口および出口が設けられている。The raw material powder discharging device installed immediately above the plasma flame is a copper triple tube having a diameter of an inner tube of 2 mm, a diameter of an intermediate tube of 4 mm, and a diameter of an outer tube of 20 mm. An inlet and an outlet are provided.
【００２６】この装置の、高周波発振コイルに４MHz、
８０KVAの高周波電流を印加し、プラズマトーチの上部
のガス導入口からアルゴンガス４０リットル／分、酸素
ガス５０リットル／分を噴出させてアルゴン−酸素プラ
ズマを発生させた。そして被覆すべき酸化アルミニウム
の原料粉末（平均粒径２μｍ）を１０ｇ／分の割合でア
ルゴンガス１０リットル／分と共に原料粉末放出装置Ｄ
の内管より供給するとともに、旋回流発生のためにアル
ゴンガス１０リットル／分を同装置の中間管より供給し
た。In this device, the high-frequency oscillation coil has a frequency of 4 MHz,
A high-frequency current of 80 KVA was applied, and argon-oxygen plasma was generated by ejecting 40 l / min of argon gas and 50 l / min of oxygen gas from a gas inlet above the plasma torch. Then, the raw material powder discharging device D is supplied with the raw material powder of aluminum oxide to be coated (average particle size 2 μm) at a rate of 10 g / min together with 10 liter / min of argon gas.
And an argon gas of 10 liter / min. Was supplied from an intermediate tube of the apparatus to generate a swirling flow.
【００２７】一方、被覆されるべき母材粒子の窒化ケイ
素（平均粒径１μｍ）は、供給装置Ｆにより３０ｇ／分
の割合で供給されたキャリアガスのアルゴンガス１５リ
ットル／分に担持させて供給した。On the other hand, the silicon nitride (average particle size: 1 μm) of the base material particles to be coated is supplied while being supported by 15 liter / minute of an argon gas of a carrier gas supplied at a rate of 30 g / minute by the supply device F. did.
【００２８】このようにして酸化アルミニウムの超微粒
子で表面が被覆された窒化ケイ素粒子を製造し、これを
Ｅから取り出した。In this way, silicon nitride particles whose surface was coated with ultrafine particles of aluminum oxide were produced, and were taken out of E.
【００２９】この酸化アルミニウムの超微粒子で表面が
被覆された窒化ケイ素粒子について、電子顕微鏡で観察
したところ、窒化ケイ素の表面は酸化アルミニウムの超
微粒子（０.０５〜０.０１μｍ、主として０.０３μ
ｍ）で被覆されていた。また、酸化アルミニウムの超微
粒子で表面が被覆された窒化ケイ素粒子からなる粉末中
には、未蒸発の被覆すべき酸化アルミニウム原料粒子は
認められなかった。When the silicon nitride particles whose surfaces were coated with the ultrafine aluminum oxide particles were observed with an electron microscope, the surface of the silicon nitride was found to be ultrafine aluminum oxide particles (0.05 to 0.01 μm, mainly 0.03 μm).
m). Also, in the powder composed of silicon nitride particles whose surface was coated with ultrafine particles of aluminum oxide, no unvaporized aluminum oxide raw material particles to be coated were found.
【００３０】比較例２ 上記実施例２と同様の操作を行なったが、旋回流発生の
ためのアルゴンガスは供給せず、その代りにキャリアガ
スとしてアルゴンガスを２０リットル／分の量で用い
た。Comparative Example 2 The same operation as in Example 2 was performed, except that argon gas for generating a swirling flow was not supplied, and instead, argon gas was used as a carrier gas at a rate of 20 l / min. .
【００３１】この条件によって製造した酸化アルミニウ
ムの超微粒子で表面が被覆された窒化ケイ素粒子につい
て、電子顕微鏡で観察したところ、窒化ケイ素の表面は
酸化アルミニウムの超微粒子（０.１〜０.０３μｍ、主
として０.０５μｍ）で被覆されていた。また、酸化ア
ルミニウムの超微粒子で表面が被覆された窒化ケイ素粒
子からなる粉末中には、多数の未蒸発の被覆すべき酸化
アルミニウム原料粒子が認められた。When the surface of the silicon nitride particles coated with the ultrafine particles of aluminum oxide produced under these conditions was observed with an electron microscope, the surface of the silicon nitride was found to be ultrafine particles of aluminum oxide (0.1 to 0.03 μm, (Mainly 0.05 μm). In addition, a large number of unevaporated aluminum oxide raw material particles to be coated were found in the powder composed of silicon nitride particles whose surface was coated with ultrafine aluminum oxide particles.
【図１】本発明の装置の概要を示す図面である。FIG. 1 is a drawing showing an outline of an apparatus of the present invention.
【図２】本発明の装置における原料粉末放出装置部分を
示す図面である。FIG. 2 is a drawing showing a raw material powder discharging device part in the device of the present invention.
【図３】図２のＡ−Ａで切断した断面図面である。FIG. 3 is a sectional view taken along the line AA of FIG. 2;
【図４】図２のＢ−Ｂで切断した断面図面である。FIG. 4 is a sectional view taken along line BB of FIG. 2;
【図５】本発明の他の一つの装置の概要を示す図面であ
る。FIG. 5 is a drawing showing an outline of another apparatus of the present invention.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 秋山 聡 埼玉県川越市稲荷町17−22 沢田コーポ 202 (72)発明者 濱田 美明 埼玉県川越市末広町３−４−８ (72)発明者 黒田 英輔 埼玉県川越市西小仙波町２−16−４ (72)発明者 梅屋 薫 宮城県仙台市太白区八木山本町１−30− 13 (56)参考文献 特開 平４−45845（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) B01J 19/00 - 19/32 B22F 1/00 C23C 14/00 - 14/58 C04B 41/87 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Satoshi Akiyama 17-22 Inaricho, Kawagoe-shi, Saitama 202 Sawada Corp. 202 (72) Inventor Miaki Hamada 3-4-8, Suehiro-cho, Kawagoe-shi, Saitama (72) Inventor Eisuke Kuroda 2-16-4, Nishikosenba-cho, Kawagoe-shi, Saitama (72) Inventor Kaoru 1-30-13, Yagiyama-honmachi, Taihaku-ku, Sendai, Miyagi Prefecture (56) References JP-A-4-45845 (JP, A) (58) Field surveyed (Int. Cl. 7 , DB name) B01J 19/00-19/32 B22F 1/00 C23C 14/00-14/58 C04B 41/87
Claims (2)
ズマ焔の直上に、無機材料または金属材料の粉末原料の
放出装置の放出口が設置され、供給される粉末原料はキ
ャリヤガスにより旋回運動が与えられてプラズマ焔中に
供給されるようにされた、該粉末原料から無機材料また
は金属材料の超微粒子を製造する装置。A discharge port of a discharge device for a powder material of an inorganic material or a metal material is provided directly above a plasma flame formed by an RF plasma method, and the supplied powder material is swirled by a carrier gas. An apparatus for producing ultrafine particles of an inorganic material or a metal material from the powdery raw material supplied in a plasma flame.
ズマ焔の直上に、無機材料または金属材料の粉末原料の
放出装置の放出口が設置され、供給される粉末原料はキ
ャリヤガスにより旋回運動が与えられてプラズマ焔中に
供給されるようにされ、そしてプラズマ焔の下流に超微
粒子によって表面を被覆しようとする無機材料または金
属材料母材の粉末を導入する装置を備え、生成した超微
粒子と導入された母材の粉末とが互に流動状態で接触せ
しめられるようにされた、母材の粒子の表面を超微粒子
で被覆する装置。2. A discharge port of a discharge device for a powder material of an inorganic material or a metal material is provided immediately above a plasma flame formed by an RF plasma method, and the supplied powder material is swirled by a carrier gas. A device for introducing a powder of an inorganic material or a metal material base material which is to be coated with ultrafine particles downstream of the plasma flame, and which is introduced with the generated ultrafine particles. An apparatus for coating the surfaces of particles of a base material with ultrafine particles so that the powders of the base material can be brought into contact with each other in a flowing state.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03308174A JP3100084B2 (en) | 1991-11-25 | 1991-11-25 | Ultrafine particle manufacturing equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03308174A JP3100084B2 (en) | 1991-11-25 | 1991-11-25 | Ultrafine particle manufacturing equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0691162A JPH0691162A (en) | 1994-04-05 |
| JP3100084B2 true JP3100084B2 (en) | 2000-10-16 |
Family
ID=17977799
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP03308174A Expired - Fee Related JP3100084B2 (en) | 1991-11-25 | 1991-11-25 | Ultrafine particle manufacturing equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3100084B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2845078A1 (en) * | 2002-09-26 | 2004-04-02 | Alstom | Production of aluminum nitride substrates, e.g. useful as supports for power electronics, comprises spraying a support with a powder comprising aluminum nitride particles coated with an oxide precursor |
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| JP5661446B2 (en) * | 2010-12-14 | 2015-01-28 | 株式会社クリーンベンチャー２１ | Method for producing crystalline semiconductor particles |
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-
1991
- 1991-11-25 JP JP03308174A patent/JP3100084B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2845078A1 (en) * | 2002-09-26 | 2004-04-02 | Alstom | Production of aluminum nitride substrates, e.g. useful as supports for power electronics, comprises spraying a support with a powder comprising aluminum nitride particles coated with an oxide precursor |
| EP1418161A3 (en) * | 2002-09-26 | 2006-03-01 | Alstom | Method for the production of an aluminium nitride substrate |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0691162A (en) | 1994-04-05 |
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