JP2545716B2 - Method for producing Fe-Si-C ultrafine particles - Google Patents
Method for producing Fe-Si-C ultrafine particlesInfo
- Publication number
- JP2545716B2 JP2545716B2 JP1052295A JP5229589A JP2545716B2 JP 2545716 B2 JP2545716 B2 JP 2545716B2 JP 1052295 A JP1052295 A JP 1052295A JP 5229589 A JP5229589 A JP 5229589A JP 2545716 B2 JP2545716 B2 JP 2545716B2
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- JP
- Japan
- Prior art keywords
- ultrafine particles
- torch
- reaction
- wall
- thermal 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.)
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Description
【発明の詳細な説明】 （産業上の利用分野） この発明はFe−Si−Ｃ系超微粒子の製造法に関し、更
に詳細には、高周波熱プラズマ法によるFe−Si−Ｃ系超
微粒子の製造法に関するものである。Description: TECHNICAL FIELD The present invention relates to a method for producing Fe—Si—C ultrafine particles, and more specifically to the production of Fe—Si—C ultrafine particles by a high frequency thermal plasma method. It is about law.
（従来の技術） 高周波熱プラズマは4000〜10000℃に亘る広範な超高
温領域を創出できるのみならず、超急冷によって通常の
方法では困難な非平衡物質や超微粒子を高純度に合成す
ることが可能であることから、新素材合成の反応場を提
供するものとして利用が大いに期待されている。(Prior Art) High-frequency thermal plasma can not only create a wide range of ultra-high temperature range from 4000 to 10000 ℃, but also can synthesize highly equilibrium non-equilibrium substances and ultra-fine particles, which is difficult by ordinary methods, by ultra-quenching. Since it is possible, it is highly expected to be used as a reaction field for synthesizing new materials.
（発明が解決しようとする課題） 従って、この発明は、高い触媒活性を示す新しい触媒
の合成を可能にするFe−Si−Ｃ系超微粒子を容易に製造
することができるFe−Si−Ｃ系超微粒子の製造法を提供
することをその課題としている。(Problems to be Solved by the Invention) Therefore, the present invention is capable of easily producing Fe—Si—C ultrafine particles which enable the synthesis of a new catalyst exhibiting high catalytic activity. It is an object to provide a method for producing ultrafine particles.
（課題を解決するための手段） 上記課題を解決するために、この発明は、約4000〜10
000℃の超高温領域を創出させた高周波熱プラズマに、F
e−Si−Ｃ系超微粒子の原料となる反応用原料ガスであ
るシラン、メタンおよび鉄カルボニルを単独でもしくは
混合ガスとして送り込んだ後、急冷し、生成したFe−Si
−Ｃ系超微粒子を捕集することから構成されている。(Means for Solving the Problems) In order to solve the above problems, the present invention provides about
For high-frequency thermal plasma that created an ultra-high temperature region of 000 ℃, F
Fe-Si produced by feeding silane, methane, and iron carbonyl, which are raw material gases for reaction, which are raw materials for e-Si-C ultrafine particles, individually or as a mixed gas, and then rapidly cooling.
-C-based ultrafine particles are collected.
なお、本発明でいう、Fe−Si−Ｃ系超微粒子とは、F
e、Si及びＣの少なくとも１種を含有する超微粒子を意
味し、β−FeSi2、β−SiC、α−Fe、FeSi、Si及びα−
FeSi2を典型例とするものである。In the present invention, the Fe-Si-C based ultrafine particles are F
e means ultrafine particles containing at least one of Si and C, β-FeSi 2 , β-SiC, α-Fe, FeSi, Si and α-
FeSi 2 is a typical example.
（実施例） 以下、この発明を実施例により説明する。(Examples) Hereinafter, the present invention will be described with reference to Examples.
（実施例） 以下の実施例に使用する超微粒子合成用高周波熱プラ
ズマ装置を第１図に示す。第１図において、高周波熱プ
ラズマ装置は、点火用トーチおよび反応用トーチを上下
二段に組み合わせて配置したトーチシステムを用いてア
ルゴンの熱プラズマを発生することができるような構成
になっている。つまり、高周波熱プラズマ装置１は、基
本的には、上段に配置された点火用トーチ２および下段
に配置された反応用トーチ３からなるトーチシステム
と、このトーチシステムの下部には、そこで反応生成さ
れた超微粒子を急冷ガスにより急冷する急冷システムと
から構成されている（T.Kamiyama etal.;Proceedings o
f the ISPC−8,p−2065,1987）。(Example) FIG. 1 shows a high frequency thermal plasma device for synthesizing ultrafine particles used in the following examples. In FIG. 1, the high frequency thermal plasma device is configured to generate a thermal plasma of argon by using a torch system in which an ignition torch and a reaction torch are arranged in a combination of upper and lower two stages. That is, the high-frequency thermal plasma device 1 basically has a torch system including an ignition torch 2 arranged in an upper stage and a reaction torch 3 arranged in a lower stage, and a reaction generation portion in the lower part of the torch system. It consists of a quenching system that quenches the produced ultrafine particles with a quenching gas (T. Kamiyama et al .; Proceedings o
f the ISPC-8, p-2065, 1987).
なお、以下の実施例においては、点火用トーチ２で
は、27MHz、1KWのアルゴンの熱プラズマを、また反応用
トーチ３では3MHz、10KWのアルゴンの熱プラズマを発生
させている。また、シラン（SiH4）、メタン（CH4）お
よび鉄カルボニル（Fe（CO）５）からなる原料ガスは単
独でもしくは混合ガスとして、第１図に示す高周波熱プ
ラズマ装置１の反応用トーチ３の上部もしくは下部また
は点火用トーチの横部からトーチシステム内に送り込む
ようになっている。In the following embodiments, the ignition torch 2 generates a 27 MHz, 1 KW argon thermal plasma, and the reaction torch 3 generates a 3 MHz, 10 KW argon thermal plasma. Further, the raw material gas consisting of silane (SiH 4 ), methane (CH 4 ) and iron carbonyl (Fe (CO) 5 ) is used alone or as a mixed gas, and the reaction torch 3 of the high frequency thermal plasma apparatus 1 shown in FIG. 1 is used. It feeds into the torch system from the top or bottom of the car or the side of the ignition torch.
実施例１ 原料ガスであるSiH4、CH4およびFe（CO）５をそれぞ
れ50ml/分の割合で反応用トーチ３の上部から高周波熱
プラズマ装置１のトーチシステム内に送り込み、最適温
度約8000℃のアルゴンプラズマ中で反応させた。反応生
成したFe−Si−Ｃ系超微粒子は、石英管で作られた急冷
システム内で急冷用ガスで急冷した。得られた超微粒子
は、反応用トーチ３の内壁（第１図のＡ）および急冷シ
ステムの石英管内壁（第１図のＢ）で捕集した。Example 1 SiH 4 , CH 4 and Fe (CO) 5, which are raw material gases, were fed into the torch system of the high frequency thermal plasma apparatus 1 from the upper part of the reaction torch 3 at a rate of 50 ml / min, and the optimum temperature was about 8000 ° C. Reaction was performed in Argon plasma. The Fe-Si-C-based ultrafine particles produced by the reaction were quenched with a quenching gas in a quenching system made of a quartz tube. The obtained ultrafine particles were collected on the inner wall of the reaction torch 3 (A in FIG. 1) and the inner wall of the quartz tube of the quenching system (B in FIG. 1).
このようにして捕集した生成物の種類、その生成相と
捕集場所を調べたところ、反応用トーチの内壁に析出し
た生成物は、非晶質相と結晶質のβ−FeSi2の超微粒子
であり、石英管内壁に析出した生成物は結晶質のβ−Si
Cおよびα−Feの超微粒子であることが判明した。ま
た、得られた超微粒子の粒径は数十nmであった。When the kind of the product thus collected, the production phase and the collection place were examined, the product deposited on the inner wall of the reaction torch was found to be an amorphous phase and a crystalline β-FeSi 2 The product, which is fine particles and deposited on the inner wall of the quartz tube, is crystalline β-Si.
It was found to be ultrafine particles of C and α-Fe. The particle size of the obtained ultrafine particles was several tens of nm.
このようにして得られた超微粒子の触媒活性を、H2/C
O＝２、温度280℃、圧力１気圧の条件で、フィッシャー
・トロプシュ反応におけるオレフィン選択活性から調べ
た。その結果、反応性トーチの内壁で捕集した超微粒子
および石英管内壁に析出した超微粒子ではそれぞれCO転
化率が0.3％および6.3％（エチレン＋プロピレン）／
（エタン＋プロパン）が15.2および1.8であることが判
明した。Thus the catalytic activity of ultrafine particles obtained, H 2 / C
It was investigated from the olefin selective activity in the Fischer-Tropsch reaction under the conditions of O = 2, temperature 280 ° C. and pressure 1 atm. As a result, CO conversion was 0.3% and 6.3% (ethylene + propylene) / in the ultrafine particles collected on the inner wall of the reactive torch and the ultrafine particles deposited on the inner wall of the quartz tube, respectively.
The (ethane + propane) was found to be 15.2 and 1.8.
実施例２ 原料ガスであるSiH4、CH4およびFe（CO）５をいずれ
も50ml/分の割合で、前者２つについては反応用トーチ
３の上部から、また後者については反応用トーチ３の下
部分から導入し、実施例１と同様に処理したところ、反
応用トーチの内壁では、非晶質相と結晶質のSiおよびβ
−SiCの超微粒子が析出し、石英管内壁では、結晶質の
α−Fe、β−SiCの超微粒子が析出した。Example 2 The source gases SiH 4 , CH 4 and Fe (CO) 5 were all at a rate of 50 ml / min, the former two from above the reaction torch 3 and the latter from the reaction torch 3. When introduced from the lower part and treated in the same manner as in Example 1, the amorphous phase and crystalline Si and β were formed on the inner wall of the reaction torch.
-SiC ultrafine particles were deposited, and crystalline α-Fe and β-SiC ultrafine particles were deposited on the inner wall of the quartz tube.
石英管内壁で得られた金属超微粒子の触媒特性を実施
例１と同様に調べたところ、CO転化率が4.0％であり、
（エチレン＋プロピレン）／（エタン＋プロパン）が1.
9であることが判明した。When the catalytic characteristics of the ultrafine metal particles obtained on the inner wall of the quartz tube were examined in the same manner as in Example 1, the CO conversion was 4.0%,
(Ethylene + propylene) / (ethane + propane) is 1.
It turned out to be 9.
実施例３ 原料ガスであるSiH4、CH4およびFe（CO）５をそれぞ
れ50ml/分、50ml/分および10ml/分を、実施例３と同様
にして導入して処理したところ、反応用トーチの内壁で
は、非晶質相と結晶質のSiおよびβ−SiCの超微粒子
が、また石英管内壁では、結晶質のFeSi、Si、α−FeSi
2およびβ−SiCの超微粒子が得られた。Example 3 SiH 4 , CH 4 and Fe (CO) 5 as source gases were introduced at 50 ml / min, 50 ml / min and 10 ml / min, respectively, in the same manner as in Example 3 and treated. Amorphous phase and crystalline ultrafine particles of Si and β-SiC are formed on the inner wall of the quartz tube, and crystalline FeSi, Si, α-FeSi on the inner wall of the quartz tube.
Ultrafine particles of 2 and β-SiC were obtained.
実施例４ 原料ガスSiH4、CH4およびFe（CO）５を、いずれも50m
l/分の割合で、点火用トーチ２の横部から導入し、実施
例１と同様にして処理したところ、反応用トーチの内壁
では非晶質相と結晶質のβ−FeSi2の超微粒子が、石英
管の内壁では非晶質相と結晶質のFeSiおよびβ−SiCの
超微粒子が得られた。Example 4 Source gas SiH 4 , CH 4 and Fe (CO) 5 were each 50
It was introduced from the lateral part of the ignition torch 2 at a rate of 1 / min and treated in the same manner as in Example 1. As a result, on the inner wall of the reaction torch, ultrafine particles of amorphous phase and crystalline β-FeSi 2 were obtained. However, amorphous phase and crystalline ultrafine particles of FeSi and β-SiC were obtained on the inner wall of the quartz tube.
このようにして得られた超微粒子について触媒特性を
調べたところ、反応用トーチ壁で捕集された超微粒子に
よるCO転化率は0.4％、（エチレン＋プロピレン）／
（エタン＋プロパン）が15.1であり、また石英管の内壁
で捕集された超微粒子によるCO転化率は5.7％、（エチ
レン＋プロピレン）／（エタン＋プロパン）が1.6であ
ることが判明した。When the catalyst characteristics of the ultrafine particles thus obtained were examined, the CO conversion rate due to the ultrafine particles collected on the reaction torch wall was 0.4%, (ethylene + propylene) /
It was found that (ethane + propane) was 15.1, the CO conversion rate due to the ultrafine particles collected on the inner wall of the quartz tube was 5.7%, and (ethylene + propylene) / (ethane + propane) was 1.6.
実施例５ 原料ガスであるSiH4、CH4およびFe（CO）５をそれぞ
れ50ml/分、11ml/分および7.5ml/分の割合で実施例１と
同様に導入し処理したところ、反応用トーチの内壁
（Ａ）では非晶質相と結晶質のα−FeSi2、Siの超微粒
子が捕集され、また石英管の内壁では結晶質のα−FeSi
O2、Siおよびβ−SiCの超微粒子が捕集された。Example 5 SiH 4 , CH 4 and Fe (CO) 5 as source gases were introduced and treated in the same manner as in Example 1 at a rate of 50 ml / min, 11 ml / min and 7.5 ml / min, respectively, and a reaction torch was obtained. Amorphous phase and crystalline ultrafine particles of α-FeSi 2 , Si are collected on the inner wall (A) of the quartz tube, and crystalline α-FeSi 2 is collected on the inner wall of the quartz tube.
Ultrafine particles of O 2 , Si and β-SiC were collected.
（発明の効果） 前記の記載から明らかなように、この発明は、従来方
法では合成が困難であった超微粒子を高純度で合成でき
るという極めて有用な方法である。このようにして得ら
れた超微粒子は、オレフィン活性が高いかまたCO転化率
が高いことから、高い触媒活性を示す新しい触媒を合成
するために極めて有用である。(Effects of the Invention) As is clear from the above description, the present invention is an extremely useful method in which ultrafine particles, which were difficult to synthesize by conventional methods, can be synthesized with high purity. The ultrafine particles thus obtained have a high olefin activity and a high CO conversion rate, and are therefore extremely useful for synthesizing a new catalyst exhibiting a high catalytic activity.
第１図は、本発明に使用される超微粒子合成用高周波熱
プラズマ装置を示す断面図である。 １……高周波熱プラズマ装置 ２……点火用トーチ ３……反応用トーチFIG. 1 is a cross-sectional view showing a high frequency thermal plasma apparatus for synthesizing ultrafine particles used in the present invention. 1 ... High-frequency thermal plasma device 2 ... Ignition torch 3 ... Reaction torch
───────────────────────────────────────────────────── フロントページの続き (72)発明者 本江 秋弘 茨城県つくば市東１丁目１番地 工業技 術院化学技術研究所内 (72)発明者 荒川 裕則 茨城県つくば市東１丁目１番地 工業技 術院化学技術研究所内 (72)発明者 福田 健三 茨城県つくば市東１丁目１番地 工業技 術院化学技術研究所内 (56)参考文献 特開 昭57−175718（ＪＰ，Ａ) 特開 昭60−239316（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Akihiro Motoe 1-1 Higashi, Tsukuba-shi, Ibaraki Institute of Chemical Technology, Industrial Technology Institute (72) Hironori Arakawa 1-1-chome, East Tsukuba, Ibaraki Industrial Technology Inside Institute for Chemical Research (72) Kenzo Fukuda 1-1-1 Higashi, Tsukuba, Ibaraki Inside Institute for Chemical Research, Industrial Technology (56) Reference JP-A-57-175718 (JP, A) JP-A-60-239316 (JP, A)
Claims (1)
4000℃〜10000℃の超高温領域にある高周波熱プラズマ
中で反応させた後、急冷することを特徴とするFe−Si−
Ｃ系超微粒子の製造法。1. Silane, methane and iron carbonyl
Fe-Si- characterized by rapid reaction after reacting in high frequency thermal plasma in the ultrahigh temperature range of 4000 ℃ ~ 10000 ℃
Method for producing C-based ultrafine particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1052295A JP2545716B2 (en) | 1989-03-04 | 1989-03-04 | Method for producing Fe-Si-C ultrafine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1052295A JP2545716B2 (en) | 1989-03-04 | 1989-03-04 | Method for producing Fe-Si-C ultrafine particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02232309A JPH02232309A (en) | 1990-09-14 |
| JP2545716B2 true JP2545716B2 (en) | 1996-10-23 |
Family
ID=12910809
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1052295A Expired - Lifetime JP2545716B2 (en) | 1989-03-04 | 1989-03-04 | Method for producing Fe-Si-C ultrafine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2545716B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2823494B2 (en) * | 1993-09-29 | 1998-11-11 | 健 増本 | Ultrafine amorphous metal particles and method for producing the same |
| DE19834236A1 (en) * | 1998-07-29 | 2000-02-03 | Basf Ag | Carbonyl iron silicide powder |
| US6495114B1 (en) | 1999-07-22 | 2002-12-17 | Fina Research, S.A. | Production of silica particles |
| US7967891B2 (en) * | 2006-06-01 | 2011-06-28 | Inco Limited | Method producing metal nanopowders by decompositon of metal carbonyl using an induction plasma torch |
| JP6434351B2 (en) * | 2015-03-26 | 2018-12-05 | 株式会社豊田自動織機 | Amorphous-containing Si powder and method for producing the same |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57175718A (en) * | 1981-04-20 | 1982-10-28 | Hitachi Ltd | Preparation of silicon carbide fine powder |
| JPS60239316A (en) * | 1984-05-11 | 1985-11-28 | Natl Inst For Res In Inorg Mater | Manufacture of hyperfine sic powder |
-
1989
- 1989-03-04 JP JP1052295A patent/JP2545716B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02232309A (en) | 1990-09-14 |
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