JPH0821475B2 - High frequency plasma equipment - Google Patents
High frequency plasma equipmentInfo
- Publication number
- JPH0821475B2 JPH0821475B2 JP4356059A JP35605992A JPH0821475B2 JP H0821475 B2 JPH0821475 B2 JP H0821475B2 JP 4356059 A JP4356059 A JP 4356059A JP 35605992 A JP35605992 A JP 35605992A JP H0821475 B2 JPH0821475 B2 JP H0821475B2
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- purity
- high frequency
- plasma
- frequency plasma
- 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
- 239000002994 raw material Substances 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 30
- 239000000523 sample Substances 0.000 claims description 22
- 238000002347 injection Methods 0.000 claims description 19
- 239000007924 injection Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 239000000470 constituent Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000011109 contamination Methods 0.000 description 5
- 239000012159 carrier gas Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000013626 chemical specie Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000007751 thermal spraying Methods 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Landscapes
- Coating By Spraying Or Casting (AREA)
- Plasma Technology (AREA)
Description
【０００１】[0001]
【産業上の利用分野】この発明は、高周波プラズマ装置
に関するものである。さらに詳しくは、この発明は、素
材への汚染を防止し、均質で超高純度の素材を得ること
のできる高周波プラズマ装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high frequency plasma device. More specifically, the present invention relates to a high-frequency plasma device capable of preventing contamination of a material and obtaining a homogeneous and ultra-high purity material.
【０００２】[0002]
【従来の技術とその課題】高周波プラズマは、数千度〜
１万５千度の超高温を有する。このプラズマ中に原料を
注入すると、原料は分解・電離して、原子、イオン、ラ
ジカル、電子等の極めて反応性に富む化学種が生成され
る。また、プラズマの尾炎部では、プラズマは１０６〜
１０７Ｋ／ｓｅｃで超急冷される。この超高温、高反応
性の化学種、及び超急冷を利用して、酸化物或いは非酸
化物を問わずに非平衡相物質の合成、超微粒子の合成、
分解反応、金属精錬、溶射等を行うことができる。2. Description of the Related Art High-frequency plasma is several thousand degrees
It has an extremely high temperature of 15,000 degrees. When the raw material is injected into this plasma, the raw material is decomposed and ionized, and extremely reactive chemical species such as atoms, ions, radicals and electrons are generated. Further, in the tail flame portion of the plasma, the plasma is 10 6 to
It is rapidly cooled at 10 7 K / sec. Utilizing this ultra-high temperature, highly reactive chemical species, and ultra-quenching, synthesis of non-equilibrium phase substance, synthesis of ultra-fine particles, regardless of oxide or non-oxide,
Decomposition reaction, metal refining, thermal spraying, etc. can be performed.
【０００３】高周波誘導プラズマは、無電極型の放電発
生法であり、プラズマガスの制限がなく、酸化・還元
性、腐食性のあらゆるガスの使用が可能であるという利
点を有している。The high-frequency induction plasma is an electrodeless discharge generation method, and has the advantage that there is no limitation on the plasma gas and that any oxidizing / reducing or corrosive gas can be used.
【０００４】その一方で、この高周波プラズマ合成法に
ついては、プラズマ中への原料の注入に問題があるのが
否めない。On the other hand, it cannot be denied that this high-frequency plasma synthesis method has a problem in injecting the raw material into the plasma.
【０００５】すなわち、プラズマが発生すると、高周波
コイル上部には渦流（図１中、符号８参照）ができ、こ
の渦流は逆流成分を持つため、プラズマ中への原料供給
が難しくなる。無理に原料供給を図ると、プラズマ壁方
向への飛散が起こり、場合によってはプラズマが乱れて
消えてしまう。That is, when plasma is generated, a vortex (see reference numeral 8 in FIG. 1) is formed in the upper part of the high frequency coil, and this vortex has a backflow component, so that it becomes difficult to supply the raw material into the plasma. If the raw material is forcibly supplied, scattering will occur in the direction of the plasma wall, and the plasma may be disturbed and disappear in some cases.
【０００６】そこで、従来においては、高周波プラズマ
の直上からプラズマの中心軸に沿って細い原料注入プロ
ーブを挿入し、その先端を高周波コイルの中心付近に位
置させた装置が提案されている。このプローブを通して
原料を注入すると、原料の飛散もなく、プラズマの乱れ
もないので、プラズマ中での履歴が揃った均質材料を得
ることが期待される。Therefore, conventionally, there has been proposed an apparatus in which a thin raw material injection probe is inserted from directly above the high frequency plasma along the central axis of the plasma and the tip thereof is positioned near the center of the high frequency coil. When the raw material is injected through this probe, the raw material is not scattered and the plasma is not disturbed. Therefore, it is expected to obtain a homogeneous material having a uniform history in the plasma.
【０００７】しかしながら、そのような高周波プラズマ
装置においては、原料注入プローブは、製作の容易なス
テンレス或いは銅などの金属を用いて作製されているた
め、原料注入プローブが蒸発しやすいという問題があっ
た。反応ガス雰囲気によっては、プローブの蒸発が促進
され、合成等により得られる素材がそれによって汚染さ
れ、素材の高純度化に重大な支障を来す。However, in such a high-frequency plasma apparatus, since the raw material injection probe is made of a metal such as stainless steel or copper which is easy to manufacture, there is a problem that the raw material injection probe is easily evaporated. . Depending on the reaction gas atmosphere, the evaporation of the probe is promoted, and the material obtained by synthesis or the like is contaminated, which seriously hinders the purification of the material.
【０００８】この発明は、以上の事情に鑑みてなされた
ものであり、従来の高周波プラズマ装置の欠点を解消
し、素材の合成等において原料注入プローブからの汚染
を防止することのできる、改善された高周波プラズマ装
置を提供することを目的とするものである。The present invention has been made in view of the above circumstances, and is improved in that the drawbacks of the conventional high-frequency plasma device can be solved and contamination from the raw material injection probe can be prevented in the synthesis of raw materials. Another object of the present invention is to provide a high frequency plasma device.
【０００９】[0009]
【課題を解決するための手段】この発明の発明者らは、
上記の解決するために鋭意検討した結果、高周波プラズ
マの中心に原料粉末、原料液体、原料ガス、若しくはそ
れらの混合物等を注入する原料注入プローブの材質とし
て、合成素材と同じ化学組成、或いはその構成元素を含
んだ高純度物質を使用することによって、均質の超高純
度材料の合成等が可能であることを見出した。この発明
は、その知見に基づいて完成されたものである。SUMMARY OF THE INVENTION The inventors of the present invention have
As a result of extensive studies to solve the above, as a material of the raw material injection probe for injecting the raw material powder, the raw material liquid, the raw material gas, or a mixture thereof into the center of the high-frequency plasma, the same chemical composition as the synthetic material, or its configuration It was found that it is possible to synthesize homogeneous ultra-high purity materials by using high-purity substances containing elements. The present invention has been completed based on that finding.
【００１０】すなわち、この発明は、高周波プラズマト
ーチの直上からプラズマトーチの中心軸に沿って原料注
入プローブが挿入され、その先端が高周波コイルの中心
付近に配置された高周波プラズマ装置において、原料注
入プローブが、製造しようとする素材と同一の成分組成
の材料又はその構成元素を含んだ高純度物質から形成さ
れたことを特徴とする高周波プラズマ装置を提供する。That is, according to the present invention, a raw material injection probe is inserted from directly above the high frequency plasma torch along the central axis of the plasma torch, and the tip thereof is arranged near the center of the high frequency coil. The present invention provides a high-frequency plasma device characterized by being formed from a material having the same composition as the material to be manufactured or a high-purity substance containing the constituent elements thereof.
【００１１】また、この発明は、製造しようとする素材
と同一の成分組成の材料又はその構成元素を含んだ高純
度物質を材質とする原料注入プローブを通して、高周波
プラズマトーチの中心に原料粉末、原料液体、原料ガス
又はこれらの混合物を供給し、超高純度で均質な素材を
製造する超高純度・均質素材の製造方法を提供するもの
でもある。Further, according to the present invention, the raw material powder and the raw material are fed to the center of the high frequency plasma torch through a raw material injection probe made of a material having the same composition as the raw material to be manufactured or a high purity substance containing the constituent elements. The present invention also provides a method for producing an ultra-high-purity / homogeneous material by supplying a liquid, a raw material gas or a mixture thereof to produce an ultra-high-purity and homogeneous material.
【００１２】原料注入プローブは、製造しようとする素
材の組成に応じて、高純度の石英ガラス、グラファイ
ト、窒化ホウ素等のチューブ、或いは高純度の酸化物、
炭化物、窒化物、硼化物、珪化物等をチューブ表面にコ
ーティングしたものを用いる。これによって、原料注入
プローブは蒸発しにくくなり、素材への汚染の心配がな
くなる。The raw material injection probe is a tube of high purity quartz glass, graphite, boron nitride or the like, or a high purity oxide, depending on the composition of the material to be manufactured.
The tube surface is coated with carbide, nitride, boride, silicide or the like. As a result, the raw material injection probe is less likely to evaporate, and there is no fear of contamination of the raw material.
【００１３】プローブの冷却は、高周波電力は比較的低
出力の場合、原料とキャリアーガスで行い、高出力の場
合、必要に応じて水冷により行う。The probe is cooled with the raw material and the carrier gas when the high frequency power has a relatively low output, and with water cooling as needed when the high frequency power has a high output.
【００１４】これを図面に基づいて説明すると、図１
は、この発明の高周波プラズマ装置の一例を模式的に示
した断面図であり、図中１が原料注入プローブである。
２は原料＋キャリアーガス、３はシースガス、４はプラ
ズマガス、５は高周波コイル、６は水冷構造プラズマ反
応管、７はプラズマトーチをそれぞれ示している。This will be described with reference to the drawings.
FIG. 2 is a cross-sectional view schematically showing an example of the high-frequency plasma device of the present invention, in which 1 is a raw material injection probe.
Reference numeral 2 is a raw material + carrier gas, 3 is a sheath gas, 4 is a plasma gas, 5 is a high frequency coil, 6 is a water-cooled structure plasma reaction tube, and 7 is a plasma torch.
【００１５】プラズマトーチ（７）中で加熱され、溶
融、蒸発、電離して生成した化学種は、プラズマトーチ
（７）の下流部で超急冷される。ここに基板を置けば、
超高純度膜材料を得ることができ、或いは基板なしの場
合には、反応管（６）中で超高純度超微粒子を生成させ
ることができる。The chemical species produced by being melted, evaporated and ionized by being heated in the plasma torch (7) are ultra-quenched in the downstream portion of the plasma torch (7). If you put the board here,
Ultra high purity membrane material can be obtained, or ultra high purity ultra fine particles can be produced in the reaction tube (6) without substrate.
【００１６】以下実施例を示し、この発明についてさら
に詳しく説明する。The present invention will be described in more detail with reference to the following examples.
【００１７】[0017]
【実施例】図１に示した高周波プラズマ装置において、
シースガス（３）としてアルゴン２５１／ｍｉｎ及び酸
素１０１／ｍｉｎ、プラズマガス（４）としてアルゴン
６１／ｍｉｎをそれぞれ流し、石英ガラス製三重水冷構
造の原料注入プローブ（１）を通して、キャリアーガス
のアルゴン４１／ｍｉｎとともに四塩化珪素２５ｇ／ｍ
ｉｎを原料＋キャリアーガス（２）として供給し、高周
波コイル（５）に４０ｋＷの高周波電力を供給して熱プ
ラズマ（プラズマトーチ（７））を発生させた。１時間
の反応後、水冷した反応容器（６）の壁面に約５００ｇ
の微粉末が堆積した。これを分析したところ、遷移金属
不純物含有量が１ｐｐｍ以下の高純度な非晶質シリカで
あることが確認された。EXAMPLE In the high frequency plasma device shown in FIG.
Argon 251 / min and oxygen 101 / min as a sheath gas (3) and argon 61 / min as a plasma gas (4) were respectively flowed, and passed through a raw material injection probe (1) having a triple water-cooled structure made of quartz glass, and an argon gas of 41 / Silicon tetrachloride 25g / m with min
In was supplied as a raw material + carrier gas (2), and high frequency power of 40 kW was supplied to the high frequency coil (5) to generate thermal plasma (plasma torch (7)). After the reaction for 1 hour, about 500 g on the wall of the water-cooled reaction vessel (6)
Of fine powder was deposited. When this was analyzed, it was confirmed to be a highly pure amorphous silica having a transition metal impurity content of 1 ppm or less.
【００１８】もちろんこの発明は以上の例によって限定
されるものではない。原料注入プローブの材質、原料の
種類や形態、装置の細部の構造等については様々な態様
が可能であることは言うまでもない。Of course, the present invention is not limited to the above examples. It goes without saying that various aspects are possible with respect to the material of the raw material injection probe, the type and shape of the raw material, the detailed structure of the apparatus, and the like.
【００１９】[0019]
【発明の効果】以上詳しく説明した通り、この発明によ
って、原料注入プローブの蒸発を防止することができ、
素材への汚染が防止される。粒径、形態、化学組成の揃
った均質の超高純度物質を合成することができ、酸化
物、非酸化物、非平衡相物質等のあらゆる素材の高速合
成が可能となる。また、合成のみならず、分解反応、金
属精錬、溶射等においても素材への汚染が防止される。
超高純度・均質素材の製造が可能となる。As described in detail above, according to the present invention, it is possible to prevent evaporation of the raw material injection probe,
Contamination of the material is prevented. It is possible to synthesize homogeneous ultra-high purity substances with uniform particle size, morphology and chemical composition, and to perform high-speed synthesis of all materials such as oxides, non-oxides and non-equilibrium phase substances. Further, not only in the synthesis but also in the decomposition reaction, metal refining, thermal spraying, etc., the contamination of the material is prevented.
It enables the production of ultra-high purity and homogeneous materials.
【図１】この発明の高周波プラズマ装置の一例を示した
模式的に示した断面図である。FIG. 1 is a schematic sectional view showing an example of a high-frequency plasma device of the present invention.
１ 原料注入プローブ ２ 原料＋キャリアーガス ３ シースガス ４ プラズマガス ５ 高周波コイル ６ 水冷構造プラズマ反応管 ７ プラズマトーチ ８ 高周波コイル上部に発生する渦流 1 Raw material injection probe 2 Raw material + carrier gas 3 Sheath gas 4 Plasma gas 5 High frequency coil 6 Water cooled structure plasma reaction tube 7 Plasma torch 8 Eddy current generated in the upper part of high frequency coil
Claims (4)
マトーチの中心軸に沿って原料注入プローブが挿入さ
れ、その先端が高周波コイルの中心付近に配置された高
周波プラズマ装置において、原料注入プローブが、製造
しようとする素材と同一の成分組成の材料又はその構成
元素を含んだ高純度物質から形成されたことを特徴とす
る高周波プラズマ装置。1. A raw material injection probe is to be manufactured in a high frequency plasma device in which a raw material injection probe is inserted from directly above the high frequency plasma torch along the central axis of the plasma torch, and the tip thereof is arranged near the center of the high frequency coil. A high-frequency plasma device characterized by being formed from a material having the same composition as the material described above or a high-purity substance containing its constituent elements.
の成分組成の材料又はその構成元素を含んだ高純度物質
から形成された請求項（１）記載の高周波プラズマ装
置。2. The high frequency plasma apparatus according to claim 1, wherein the raw material injection probe is formed of a material having the same composition as the material to be synthesized or a high-purity substance containing its constituent elements.
の材料又はその構成元素を含んだ高純度物質を材質とす
る原料注入プローブを通して、高周波プラズマトーチの
中心に原料粉末、原料液体、原料ガス又はこれらの混合
物を供給し、超高純度で均質な素材を製造する超高純度
・均質素材の製造方法。3. A raw material powder, a raw material liquid, a raw material gas at the center of the high-frequency plasma torch through a raw material injection probe made of a material having the same composition as the material to be manufactured or a high-purity substance containing the constituent elements thereof. Alternatively, a method for producing an ultrahigh-purity / homogeneous material, which comprises supplying a mixture of these and producing an ultrahigh-purity, homogeneous material.
の成分組成の材料又はその構成元素を含んだ高純度物質
から形成された請求項（３）記載の超高純度・均質素材
の製造方法。4. The method for producing an ultra-high-purity / homogeneous material according to claim 3, wherein the material-injection probe is formed of a material having the same composition as the material to be synthesized or a high-purity substance containing the constituent elements thereof. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4356059A JPH0821475B2 (en) | 1992-12-18 | 1992-12-18 | High frequency plasma equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4356059A JPH0821475B2 (en) | 1992-12-18 | 1992-12-18 | High frequency plasma equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06283298A JPH06283298A (en) | 1994-10-07 |
| JPH0821475B2 true JPH0821475B2 (en) | 1996-03-04 |
Family
ID=18447116
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4356059A Expired - Lifetime JPH0821475B2 (en) | 1992-12-18 | 1992-12-18 | High frequency plasma equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0821475B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100348586B1 (en) * | 1999-02-25 | 2002-08-13 | 송병무 | Method and apparatus for treatment of hazardous and toxic gases |
| EP1630849B1 (en) * | 2004-08-27 | 2011-11-02 | Fei Company | Localized plasma processing |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5851378B2 (en) * | 1975-10-29 | 1983-11-16 | 株式会社日立製作所 | Micro Haspattering Ion Gen |
-
1992
- 1992-12-18 JP JP4356059A patent/JPH0821475B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06283298A (en) | 1994-10-07 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |