JPH02243707A - Manufacture of metal super fine particle - Google Patents
Manufacture of metal super fine particleInfo
- Publication number
- JPH02243707A JPH02243707A JP6572489A JP6572489A JPH02243707A JP H02243707 A JPH02243707 A JP H02243707A JP 6572489 A JP6572489 A JP 6572489A JP 6572489 A JP6572489 A JP 6572489A JP H02243707 A JPH02243707 A JP H02243707A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- thermal decomposition
- transition metal
- volume
- compound
- 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.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 title abstract description 19
- 239000002184 metal Substances 0.000 title abstract description 19
- 239000010419 fine particle Substances 0.000 title description 3
- 239000007789 gas Substances 0.000 claims abstract description 55
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 19
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 16
- -1 transition metal carbonyl compound Chemical class 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000003085 diluting agent Substances 0.000 claims description 18
- 239000002923 metal particle Substances 0.000 claims description 18
- 150000001728 carbonyl compounds Chemical class 0.000 claims description 12
- 239000012071 phase Substances 0.000 claims description 12
- 238000000197 pyrolysis Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 150000003624 transition metals Chemical class 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000012808 vapor phase Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 12
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000010790 dilution Methods 0.000 abstract description 4
- 239000012895 dilution Substances 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract 3
- 238000007796 conventional method Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 7
- 239000011882 ultra-fine particle Substances 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 6
- 230000005415 magnetization Effects 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔発明の背景〕
産業上の利用分野
本発明は、金属超微粒子の製法に関する。さらに詳しく
は、本発明は、遷移金属カルボニル化合物を特定の条件
下で気相熱分解することにより、高密度磁気記録媒体等
に適する優れた磁気特性、すなわち高保磁力および高飽
和磁化、を有する金属磁性超微粒子の製法に関する。DETAILED DESCRIPTION OF THE INVENTION [Background of the Invention] Industrial Application Field The present invention relates to a method for producing ultrafine metal particles. More specifically, the present invention produces a metal having excellent magnetic properties suitable for high-density magnetic recording media, such as high coercive force and high saturation magnetization, by subjecting transition metal carbonyl compounds to gas phase thermal decomposition under specific conditions. This article relates to a method for producing magnetic ultrafine particles.
従来の技術
Ｆｅ５Ｎｉ等の遷移金属カルボニル化合物の気相熱分解
により金属微粉末を得る方法は公知であって、例えば特
公昭４３．、−２４，３１６号、同４４１１５２９号、
同５２−３１．８０９号公報等が知られている。2. Description of the Related Art A method for obtaining fine metal powder by gas-phase thermal decomposition of a transition metal carbonyl compound such as Fe5Ni is known, for example, as disclosed in Japanese Patent Publication No. 43, No. , No.-24,316, No. 4411529,
Publication No. 52-31.809 and the like are known.
しかし、本発明者らの知る限りでは、これら公報のいず
れにおいても、得られる粉末の粒子径は数ミクロン程度
と大きく、本発明が目的とするような短軸径の平均粒径
が０．０５ミクロン以下の針状金属超微粒子は得られな
いし、更に高密度磁気記録媒体等に適した高保磁力およ
び高飽和磁化の優れた磁気特性を有する金属超微粒子も
得られていない。However, as far as the present inventors know, in all of these publications, the particle size of the obtained powder is large, on the order of several microns, and the average particle size of the short axis diameter, which is the objective of the present invention, is 0.05. Acicular ultrafine metal particles of micron size or less have not been obtained, and furthermore, ultrafine metal particles having excellent magnetic properties such as high coercive force and high saturation magnetization suitable for high-density magnetic recording media have not been obtained.
また、特公昭３９−１００４号、同４５１６８６８号、
特開昭５８−１３７２０２号公報等に於いては、遷移金
属カルボニル化合物を特殊な溶媒に溶解した液相状態で
熱分解反応を行なうことにより、溶媒中に分散した金属
超微粒子を得ることを提案している。Also, Special Publication No. 39-1004, No. 4516868,
In JP-A-58-137202, etc., it is proposed to obtain ultrafine metal particles dispersed in a solvent by carrying out a thermal decomposition reaction in a liquid phase state in which a transition metal carbonyl compound is dissolved in a special solvent. are doing.
しかし、本発明者らの知る限りでは、金属超微粒子の工
業的製造において、液相法の製法では、金属超微粒子は
見掛は密度が極めて低いことなとから、超微粒子と溶媒
との分離プロセスが困難となったり、溶媒当りの生産量
が低く抑えられるなどして高コストになるなど、気相法
の製法に比較すると量産性、経済性の点で問題を生ずる
。However, as far as the present inventors know, in the industrial production of ultrafine metal particles, in the liquid phase method, the ultrafine metal particles have an extremely low apparent density, so it is difficult to separate the ultrafine particles from the solvent. This poses problems in terms of mass production and economy compared to the gas phase method, such as the process being difficult and the production volume per solvent being kept low, resulting in high costs.
そこで本発明者らは、遷移金属カルボニル化合物を気相
熱分解して該遷移金属の粉末を製造する方法を、先に提
案した（特願昭６３−２８４７６号明細書）
しかしながら、この方法を単に実施した場合には、
（１）反応部に設けられた金属カルボニル化合物供給導
入管に希釈ガスからの熱が直接供給される為に、供給導
入管内で金属カルボニル化合物の熱分解が生じて供給導
入管の閉塞か起こり、長時間運転に耐えないこと、
（２）金属カルボニル化合物の供給導入管先端部分が直
接希釈ガスの高温湯にさらされる為、該先端部分近傍で
滞留した金属カルボニルが分解を起こし、先端部分で成
長し、性能の安定性を阻害すること、
（３）金属カルボニル化合物と希釈ガスとの混合が充分
行われないうちに熱分解反応が進行する為に、反応濃度
、反応温度が不均一のまま粒子成長が起こり、粒子径分
布か広くなること、等実用化の点で大きな問題があるこ
とが判明した。Therefore, the present inventors previously proposed a method for producing transition metal powder by vapor-phase pyrolysis of a transition metal carbonyl compound (Japanese Patent Application No. 63-28476). If carried out, (1) Heat from the diluent gas is directly supplied to the metal carbonyl compound supply introduction pipe installed in the reaction section, so thermal decomposition of the metal carbonyl compound occurs in the supply introduction pipe, causing the supply introduction. (2) Since the tip of the metal carbonyl compound supply introduction tube is directly exposed to the high-temperature water of the diluent gas, the metal carbonyl stagnant near the tip may be decomposed. (3) Since the thermal decomposition reaction proceeds before the metal carbonyl compound and diluent gas are sufficiently mixed, the reaction concentration and reaction temperature may It was found that there were major problems in terms of practical application, such as particle growth occurring while the particles remained non-uniform and the particle size distribution becoming broader.
要旨
本発明者等は、以上の状況に鑑み、気相法金属超微粒子
の製法について鋭意検討の結果、本発明をなし得た。Summary In view of the above circumstances, the present inventors have completed the present invention as a result of intensive studies on the method for producing ultrafine metal particles produced by vapor phase method.
すなわち、本発明による金属超微粒子の製造法は、水素
および／または不活性ガスからなる希釈ガスで希釈され
た遷移金属カルボニル化合物を気相熱分解して該遷移金
属の粉末を製造する方法において、予め０． １〜３０
体積％の濃度に希釈された２００℃以下の遷移金属カル
ボニル化合物の希釈混合気体の１〜３０体積％と、気相
熱分解の供給熱源としての４００℃以上の更なる希釈ガ
ス９６〜５５体積％とを各々反応部に供給し、混合する
ことにより気相熱分解を行うこと、該カルボニル化合物
の希釈混合気体を反応部に導入する際、導入部周囲より
該混合気体の流出に逆らわない方向に２００℃以下の低
温希釈ガス３〜１５体積％を流出させること、および前
記気合熱分解を３００ガウス以上の磁場の存在下に行う
こと、を特徴とするものである。That is, the method for producing ultrafine metal particles according to the present invention is a method for producing powder of a transition metal by gas-phase pyrolysis of a transition metal carbonyl compound diluted with a diluent gas consisting of hydrogen and/or an inert gas. 0 in advance. 1-30
1-30% by volume of a diluted mixture gas of transition metal carbonyl compound below 200°C diluted to a concentration of % by volume and 96-55% by volume of a further diluent gas above 400°C as a feed heat source for gas phase pyrolysis. and gas-phase thermal decomposition by supplying and mixing them to the reaction section, and when introducing the diluted mixed gas of the carbonyl compound into the reaction section, from the periphery of the introduction section in a direction that does not oppose the outflow of the mixed gas. The method is characterized in that 3 to 15% by volume of a low-temperature diluent gas of 200° C. or lower is allowed to flow out, and that the vapor pyrolysis is performed in the presence of a magnetic field of 300 Gauss or higher.
効果
本発明方法によれば、極めて微細な、たとえば平均短軸
径０．０５ミクロン以下の針状の、遷移金属粉末が安定
して得られる。そして、この遷移金属粉末は、磁気特性
が優れている。Effects According to the method of the present invention, extremely fine, acicular transition metal powder having an average minor axis diameter of 0.05 microns or less, for example, can be stably obtained. This transition metal powder has excellent magnetic properties.
本発明の方法で、極めて微細な針状金属粉末が安定して
得られるのは、磁場の印加状態で、低温の金属カルボニ
ル化合物を希釈ガスで所定割合希釈した少量の混合気体
（ど対して、高温で多量の希釈ガスを混合することによ
り、金属カルボニルの分解に要する反応熱と分解熱を外
部熱源から与える場合に比較して、著しく急速に熱を供
給できる為および低温の希釈ガスで金属カルボニル供給
導入管を冷却保護することにより該管出口の閉塞や反応
物の付着を抑制できる為に、粒子形成時の核発生数が多
く、それだけ微細な粒子を安定的に形成できるものと考
えられる。In the method of the present invention, extremely fine acicular metal powder can be stably obtained under the application of a magnetic field using a small amount of a mixed gas (as opposed to By mixing a large amount of diluent gas at high temperature, heat can be supplied significantly more rapidly than when the reaction heat and decomposition heat required for decomposing metal carbonyls is supplied from an external heat source, and metal carbonyls can be decomposed with low-temperature diluent gas. It is thought that by cooling and protecting the supply inlet pipe, it is possible to suppress the clogging of the pipe outlet and the adhesion of reactants, so that a large number of nuclei are generated during particle formation, and it is possible to stably form finer particles.
遷移金属カルボニル化合物
本発明に於いて使用される遷移金属カルボニル化合物は
、Ｆｅ、Ｎｉ、Ｃｏ、Ｗ、Ｍｏ等のカルボニル化合物及
びこれらの混合物であり、好ましくは低沸点のＦ ｅ
（ＣＯ） ５およびＣｏ Ｈ（ＣＯ） ４である。Transition metal carbonyl compound The transition metal carbonyl compound used in the present invention is a carbonyl compound such as Fe, Ni, Co, W, Mo, etc., or a mixture thereof, and is preferably a low boiling point Fe.
(CO) 5 and Co H(CO) 4.
高沸点のＭｏＸＷ等のカルボニル化合物は、それ自身の
熱分解に加えて、これをＦ ｅ （ＣＯ） ５あるいは
ＣｏＨ（Ｃｏ）４に少量溶解させて、反応系に供給する
ことで溶媒金属との合金粒子を得ることもできる。In addition to thermally decomposing high-boiling point carbonyl compounds such as MoXW, carbonyl compounds such as MoXW can be dissolved with a solvent metal by dissolving a small amount in Fe (CO) 5 or CoH (Co) 4 and supplying it to the reaction system. Alloy particles can also be obtained.
希釈ガス
希釈ガスとしては、窒素、アルゴン等の不活性ガスまた
は水素若しくはそれらの混合気体が使用される。Diluting gas As the diluting gas, an inert gas such as nitrogen or argon, hydrogen, or a mixture thereof is used.
熱分解
本発明による熱分解は、原料遷移金属カルボニル化合物
の希釈ないし内部熱源の導入ならびに気相熱分解を磁場
の印加下で行なうことを除けば、従来公知のそれと本質
的には変らない。Thermal decomposition The thermal decomposition according to the present invention is essentially the same as that known in the art, except that the raw transition metal carbonyl compound is diluted or an internal heat source is introduced, and the gas phase thermal decomposition is carried out under the application of a magnetic field.
第１図は、本発明方法を実施するための装置の一例を示
すものである。FIG. 1 shows an example of an apparatus for carrying out the method of the present invention.
第１図において、導入管１より高温の希釈ガスを、また
、導入管５より低温の金属カルボニルと希釈ガスの混合
気体を導入し、両者を磁場の印加されているノズル出口
６の位置で接触させることにより、金属カルボニルの分
解に必要な３００℃以上、好ましくは４００〜８００℃
の範囲、の熱を高温側希釈ガスより瞬時に供給すること
ができる。In Fig. 1, a high-temperature diluent gas is introduced through the introduction tube 1, and a mixed gas of metal carbonyl and dilution gas at a low temperature is introduced through the introduction tube 5, and the two are brought into contact at the nozzle outlet 6 where a magnetic field is applied. By heating, the temperature is 300°C or higher, preferably 400 to 800°C, which is necessary for the decomposition of metal carbonyl.
Heat in the range of 100 to 100% can be instantly supplied from the high-temperature side diluent gas.
この際、導入管５内での低温の金属カルボニルの分解反
応による閉塞を防止する為に、導入管１１より低温の希
釈ガスを導入し保護する。At this time, in order to prevent blockage due to the decomposition reaction of low-temperature metal carbonyl in the introduction pipe 5, low-temperature diluent gas is introduced from the introduction pipe 11 for protection.
導入管５より導入される混合気体は、金属カルボニル化
合物（導入管２より導入）と希釈ガス（導入管３より導
入）とを混合室４において混合して、所定の濃度の金属
カルボニル化合物混合気体として得られる。この導入管
５より導入される混合気体中の遷移金属カルボニル化合
物の濃度は、０．１〜３０体積％、好ましくは０．５〜
２５体積％、の範囲である。この濃度が高過ぎると得ら
れる金属粒子の粒径が大きく成長するので、本発明が目
的とする高保磁力を有する磁性超微粉は得られず、一方
、濃度が低過ぎると生産性が劣る。The mixed gas introduced through the introduction pipe 5 is produced by mixing a metal carbonyl compound (introduced through the introduction pipe 2) and a diluent gas (introduced through the introduction pipe 3) in the mixing chamber 4 to produce a metal carbonyl compound mixed gas having a predetermined concentration. obtained as. The concentration of the transition metal carbonyl compound in the gas mixture introduced through the introduction pipe 5 is 0.1 to 30% by volume, preferably 0.5 to 30% by volume.
The range is 25% by volume. If this concentration is too high, the particle size of the metal particles obtained will grow large, making it impossible to obtain the magnetic ultrafine powder having a high coercive force, which is the object of the present invention.On the other hand, if the concentration is too low, productivity will be poor.
この導入管５より導入される混合気体は、２００℃以下
、好ましくは１８０〜３０℃、の温度範囲であって、そ
の導入量は導入管１と導入管５および導入管１１との総
供給量に対して１〜３０体積％、好ましくは３〜２０体
積％、である。The mixed gas introduced through the introduction pipe 5 has a temperature range of 200°C or less, preferably 180 to 30°C, and the amount introduced is the total amount supplied from the introduction pipe 1, the introduction pipe 5, and the introduction pipe 11. 1 to 30% by volume, preferably 3 to 20% by volume.
導入量が少な過ぎると生産性が劣り、一方、多過ぎると
十分な反応熱が得られないので反応速度が低下し、生成
金属粒子が大きく成長して超微粒子が得られない。また
、この混合ガスの温度が高すぎると、導入管５内での金
属カルボニルの分解反応が生じ、所望の超微粒子は得ら
れない。If the amount introduced is too small, the productivity will be poor, while if it is too large, sufficient reaction heat will not be obtained, so the reaction rate will be reduced, and the produced metal particles will grow large, making it impossible to obtain ultrafine particles. Furthermore, if the temperature of this mixed gas is too high, a decomposition reaction of the metal carbonyl occurs within the introduction pipe 5, making it impossible to obtain the desired ultrafine particles.
また、導入管１より導入される高温の希釈ガスは、４０
０℃以上、好ましくは４５０℃以上（上限は１０００℃
程度）、であって、その導入量は導入管１と導入管５お
よび導入管１１との総供給量に対して９６〜５５体積％
、好ましくは９２〜７０体積％、である。このガスの温
度が低すぎたり、導入量が少ないと、十分な反応熱が得
られないので反応速度が著しく低下し、金属粒子形成時
の核発生量も減少するので粒径が大きく成長して本発明
が目的とする超微粒子は得られない。In addition, the high temperature diluent gas introduced from the introduction pipe 1 is
0°C or higher, preferably 450°C or higher (upper limit is 1000°C)
degree), and the amount introduced is 96 to 55% by volume based on the total supply amount of introduction tube 1, introduction tube 5, and introduction tube 11.
, preferably 92 to 70% by volume. If the temperature of this gas is too low or the amount introduced is too small, sufficient reaction heat will not be obtained and the reaction rate will drop significantly, and the amount of nuclei generated during metal particle formation will also decrease, causing the particle size to grow larger. The ultrafine particles targeted by the present invention cannot be obtained.
また導入管１１より導入される低温の希釈ガスは、２０
０℃以下、好ましくは１００℃以下であって、その導入
量は総供給量の３〜１５体積％、好ましくは５〜１０体
積％である。このガス導入量が少ないと、原料金属カル
ボニル化合物導入管５内での分解反応による閉塞、ある
いは導入管５先端での付着を防止する事ができず、長時
間の安定運転が継続できない。一方、多すぎると反応温
度が充分保てず、目的とする超微粒子が得られない。In addition, the low temperature diluent gas introduced from the introduction pipe 11 is
The temperature is 0°C or lower, preferably 100°C or lower, and the amount introduced is 3 to 15% by volume, preferably 5 to 10% by volume of the total amount supplied. If the amount of gas introduced is small, it will not be possible to prevent blockage due to decomposition reaction within the raw material metal carbonyl compound introduction tube 5 or adhesion at the tip of the introduction tube 5, making it impossible to continue stable operation for a long time. On the other hand, if the amount is too large, the reaction temperature cannot be maintained sufficiently and the desired ultrafine particles cannot be obtained.
ノズル出口６の位置で接触混合されたガスは、７の反応
管内で５秒以下、好ましくは２秒以下、滞留して気相分
解反応を行う。The gases catalytically mixed at the nozzle outlet 6 remain in the reaction tube 7 for 5 seconds or less, preferably 2 seconds or less, to perform a gas phase decomposition reaction.
反応系への磁場の印加は、永久磁石、電磁石、ソレノイ
ドコイル等の装置８のいずれも使用可能である。印加す
る磁場は、３００ガウス以上、好ましくは４００〜１５
００ガウスの範囲、である。Any device 8 such as a permanent magnet, an electromagnet, or a solenoid coil can be used to apply the magnetic field to the reaction system. The applied magnetic field is 300 Gauss or more, preferably 400 to 15
00 Gauss range.
磁場を印加することで、生成する金属超微粒子の針状性
を制御して、保磁力を大きくすることができる。By applying a magnetic field, the acicularity of the produced ultrafine metal particles can be controlled and the coercive force can be increased.
熱分解によって生成した金属超微粒子は、管路９を経て
捕集室１０へ送って回収する。Ultrafine metal particles generated by thermal decomposition are sent to a collection chamber 10 via a pipe 9 and collected.
上記の条件により、金属超微粒子を生成させることで、
たとえば、保磁力８００〜２５００エルステツド、飽和
磁化１２０〜２００ｅｍｕ／ｇの磁気特性を有する金属
超微粒子が安定的に得られる。By generating ultrafine metal particles under the above conditions,
For example, ultrafine metal particles having magnetic properties of a coercive force of 800 to 2,500 oersted and a saturation magnetization of 120 to 200 emu/g can be stably obtained.
本発明で得られる金属超微粒子は、高密度記録媒体とし
て好ましいものであるが、金属超微粒子を要する分野は
、これに限るものではないし、本発明による超微粒子の
用途もそれに限られるものではない。The ultrafine metal particles obtained by the present invention are preferable as high-density recording media, but the fields that require ultrafine metal particles are not limited to this, nor are the uses of the ultrafine particles according to the present invention limited thereto. .
実験例１
第１図に示すような反応装置において、内径２７＋ｎｍ
、長さ１ｍの反応管に６００ガウスの磁場を印加し、下
記の反応条件でＦ ｅ （ＣＯ） ５の気相熱分解反応
を行なって、鉄用微粒子を形成させた。Experimental Example 1 In a reaction apparatus as shown in Fig. 1, an inner diameter of 27+nm was used.
A magnetic field of 600 Gauss was applied to a reaction tube having a length of 1 m, and a gas phase pyrolysis reaction of Fe (CO) 5 was carried out under the following reaction conditions to form fine particles for iron.
（イ）管路１からの窒素導入量
窒素：５００℃、総供給量の８５体積％（ロ）管路５か
らの混合気体導入量
窒素＝６０℃、総供給量の８．５体積％Ｆｅ （Ｃｏ）
５： ６０℃、総供給量の１．５体積％
（ハ）管路１１からの希釈ガス導入量
窒素＝６０℃、総供給量の５体積％
（ニ）滞留時間 ０，１秒
（ホ）反応管内平均温度 ４９５℃
得られた鉄用微粒子は、透過電子顕微鏡写真の観察によ
り、短軸径０．０２ミクロン、長軸径０．２０ミクロン
の針状形を呈し、磁気特性は、飽和磁化１３０ （ｅｍ
ｕ／ｇ ） 、保磁力１５２０（Ｏｅ）であった。(a) Amount of nitrogen introduced from pipe 1 Nitrogen: 500°C, 85% by volume of the total supply (b) Amount of mixed gas introduced from pipe 5 Nitrogen = 60°C, 8.5% by volume of the total supply Fe (Co)
5: 60°C, 1.5% by volume of the total supply (c) Amount of diluent gas introduced from pipe 11 Nitrogen = 60°C, 5% by volume of the total supply (d) Residence time 0.1 seconds (e) Average temperature inside the reaction tube: 495°C. Observation of transmission electron micrographs shows that the obtained fine particles for iron exhibit an acicular shape with a minor axis diameter of 0.02 microns and a major axis diameter of 0.20 microns, and the magnetic properties are saturation magnetization. 130 (em
u/g) and coercive force of 1520 (Oe).
実施例２
実施例１の条件において長時間安定性の確認を行なった
結果、
経過時間
［時間］
次の通りであった。Example 2 The long-term stability was confirmed under the conditions of Example 1. As a result, the elapsed time [hours] was as follows.
保磁力 飽和磁化
［Ｏｅ］ ［ｅｍｕ ／ ｇ］
印加装置、９・・・管路、１０・・・捕集室、１１・・
・低温の希釈ガス導入管、１２・・・冷却水管。Coercive force Saturation magnetization [Oe] [emu/g] Application device, 9... Conduit, 10... Collection chamber, 11...
・Low temperature dilution gas introduction pipe, 12...cooling water pipe.
Claims (1)
された遷移金属カルボニル化合物を気相熱分解して該遷
移金属の粉末を製造する方法において、予め０．１〜３
０体積％の濃度に希釈された２００℃以下の遷移金属カ
ルボニル化合物の希釈混合気体の１〜３０体積％と、気
相熱分解の供給熱源としての４００℃以上の更なる希釈
ガス９６〜５５体積％とを各々反応部に供給し、混合す
ることにより気相熱分解を行うこと、該カルボニル化合
物の希釈混合気体を反応部に導入する際、導入部周囲よ
り該混合気体の流出に逆らわない方向に２００℃以下の
低温希釈ガス３〜１５体積％を流出させること、および
前記気相熱分解を３００ガウス以上の磁場の存在下に行
うこと、を特徴とする金属超微粒子の製造法。In a method for producing a transition metal powder by vapor-phase pyrolysis of a transition metal carbonyl compound diluted with a diluent gas consisting of hydrogen and/or an inert gas,
1-30% by volume of a diluted gas mixture of transition metal carbonyl compounds below 200°C diluted to a concentration of 0% by volume and 96-55% by volume of a further diluent gas above 400°C as a feed heat source for gas phase pyrolysis. % respectively to the reaction section and mix them to perform gas phase thermal decomposition, and when introducing the diluted mixed gas of the carbonyl compound into the reaction section, a direction that does not oppose the outflow of the mixed gas from around the introduction section. 1. A method for producing ultrafine metal particles, comprising: flowing out 3 to 15% by volume of a low-temperature diluent gas of 200° C. or lower; and performing the gas phase pyrolysis in the presence of a magnetic field of 300 Gauss or higher.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6572489A JPH02243707A (en) | 1989-03-17 | 1989-03-17 | Manufacture of metal super fine particle |
| US07/433,376 US5064464A (en) | 1988-11-10 | 1989-11-09 | Process for producing ultrafine metal particles |
| EP89311682A EP0368676A3 (en) | 1988-11-10 | 1989-11-10 | Process for producing ultrafine metal particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6572489A JPH02243707A (en) | 1989-03-17 | 1989-03-17 | Manufacture of metal super fine particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02243707A true JPH02243707A (en) | 1990-09-27 |
Family
ID=13295253
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6572489A Pending JPH02243707A (en) | 1988-11-10 | 1989-03-17 | Manufacture of metal super fine particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02243707A (en) |
-
1989
- 1989-03-17 JP JP6572489A patent/JPH02243707A/en active Pending
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