JP2843907B2 - Composite particle synthesis method by vibrating fluidized bed method - Google Patents
Composite particle synthesis method by vibrating fluidized bed methodInfo
- Publication number
- JP2843907B2 JP2843907B2 JP13080496A JP13080496A JP2843907B2 JP 2843907 B2 JP2843907 B2 JP 2843907B2 JP 13080496 A JP13080496 A JP 13080496A JP 13080496 A JP13080496 A JP 13080496A JP 2843907 B2 JP2843907 B2 JP 2843907B2
- Authority
- JP
- Japan
- Prior art keywords
- particles
- fluidized bed
- component
- composite
- core
- 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
- 238000000034 method Methods 0.000 title claims description 39
- 239000011246 composite particle Substances 0.000 title claims description 32
- 238000001308 synthesis method Methods 0.000 title description 3
- 239000002245 particle Substances 0.000 claims description 52
- 239000007771 core particle Substances 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 23
- 230000002194 synthesizing effect Effects 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 13
- 239000010419 fine particle Substances 0.000 claims description 9
- 239000013590 bulk material Substances 0.000 claims description 7
- 230000002776 aggregation Effects 0.000 claims description 6
- 238000005054 agglomeration Methods 0.000 claims description 4
- 238000004220 aggregation Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 26
- 239000007789 gas Substances 0.000 description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 15
- 229910052742 iron Inorganic materials 0.000 description 13
- 239000002131 composite material Substances 0.000 description 10
- 239000011164 primary particle Substances 0.000 description 8
- 238000005243 fluidization Methods 0.000 description 7
- 239000010408 film Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000696 magnetic material Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Glanulating (AREA)
Description
【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION
【０００１】[0001]
【発明の属する技術分野】本発明は、核粒子表面が第２
成分で粒子状や膜状にコーティングされた被覆型複合粒
子の新規な合成方法に関するものである。更に詳しく言
えば、本発明は、触媒やセンサー材料など粒子状態で機
能を示す粉体や、あるいは軟磁性バルク体などの焼結体
原料粉体の合成方法として好適な、核粒子が１次粒子の
状態まで均一に第２成分でコーティングされ、しかも、
その被覆状態が粒子状または膜状などとしてその複合構
造が制御された複合粒子の合成方法に関するものであ
る。BACKGROUND OF THE INVENTION The present invention relates to a method for producing a core particle having a second surface.
The present invention relates to a novel method for synthesizing coated composite particles coated with the components in the form of particles or a film. More specifically, the present invention relates to a method for synthesizing a powder exhibiting a function in a particle state such as a catalyst or a sensor material, or a raw material powder for a sintered body such as a soft magnetic bulk material, in which a core particle is a primary particle. Is uniformly coated with the second component up to the state of
The present invention relates to a method for synthesizing composite particles in which the coating state is particulate or film-like and the composite structure is controlled.
【０００２】[0002]
【従来の技術】高特性化や多機能化が要求されているセ
ラミックス材料等の原料粉体として、第２成分が粒子や
膜として核粒子表面を被覆した複合構造を有する複合粒
子が合成され、粒子としての機能を向上させたり、それ
を焼結体原料粉体としてセラミックコンポジットを製造
することが検討されている。このような複合粒子合成方
法の１つとして流動層法が考えられる。しかしセラミッ
クス分野で主に対象となるミクロンオーダー以下の微粒
子の流動化及び第２成分による複合粒子合成では、核粒
子の難流動化性と凝集体形成という問題点がある（「化
学工学の進歩２６・流動層」、化学工学会編、横書店
（１９９２））。2. Description of the Related Art Composite particles having a composite structure in which a second component is coated as a particle or film on a core particle surface are synthesized as a raw material powder of a ceramic material or the like which is required to have high performance and multifunctionality. It has been studied to improve the function as particles or to manufacture a ceramic composite using the powder as a sintered material raw material powder. A fluidized bed method is considered as one of such composite particle synthesis methods. However, fluidization of fine particles on the order of microns or less and synthesis of composite particles using the second component, which are mainly targets in the field of ceramics, have problems such as poor fluidity of core particles and formation of aggregates (see “Progress in Chemical Engineering 26”). Fluidized bed, edited by the Society of Chemical Engineers, Horizontal Bookstore (1992)).
【０００３】難流動化性については、これまで主に、流
動化ガス流速を大きくする方法や、流動層に振動を組み
合わせた振動流動層法などが検討されてきた。しかし、
前者の方法では流動層からの核粒子の飛び出しの多さが
問題視されていた（Ｓ．Ｍｏｒｏｏｋａ、Ｔ．Ｏｋｕｂ
ｏ、Ｋ．Ｋｕｓａｋａｂｅ：Ｐｏｗｄｅｒ Ｔｅｃｈｎ
ｏｌ．、６３、１０５（１９９０））。また振動流動層
法は、低ガス流速で微粒子の飛び出し量を抑制しつつ流
動化させることができるが、凝集体形成の問題はこれま
で検討されていなかった（森滋勝、春田武男、山本晃
稔、山田幾穂、水谷栄一：化学工学論文誌、１５、９９
２（１９８９））。[0003] As to the difficulty of fluidization, a method of increasing a fluidized gas flow rate, a vibrating fluidized bed method in which vibration is combined with a fluidized bed, and the like have been mainly studied. But,
In the former method, a large amount of nuclear particles jumping out of the fluidized bed was regarded as a problem (S. Morooka, T. Okub).
o, K. Kusakabe: Powder Techn
ol. , 63, 105 (1990)). In addition, the oscillating fluidized bed method enables fluidization while suppressing the amount of ejected fine particles at a low gas flow rate, but the problem of agglomerate formation has not been studied so far (Shigeru Mori, Takeo Haruta, Akinori Yamamoto, Ikuho Yamada, Eiichi Mizutani: Journal of Chemical Engineering, 15, 99
2 (1989)).
【０００４】ＧｅｌｄａｒｔのＣ粉体と呼ばれる上記の
大きさの微粒子は、数１０〜数１００ミクロンの凝集体
が形成されることによって流動化されるため、流動層法
によって複合粒子を合成する場合、核粒子の分散性や第
２成分の拡散及び反応の均一性に問題がある。これまで
は、第２成分が凝集体内部に拡散するように厳密な条件
設定を行う方法などが用いられていたが、その場合にも
良好な固気接触条件の実現が困難となっていた（Ｓ．Ｍ
ｏｒｏｏｋａ、Ｔ．Ｏｋｕｂｏ、Ｋ．Ｋｕｓａｋａｂ
ｅ：Ｐｏｗｄｅｒ Ｔｅｃｈｎｏｌ．、６３、１０５
（１９９０））。[0004] Since fine particles of the above-mentioned size called Geldart C powder are fluidized by forming aggregates of several tens to several hundreds of microns, when synthesizing composite particles by a fluidized bed method, There is a problem in the dispersibility of the core particles, the diffusion of the second component, and the uniformity of the reaction. Until now, a method of setting strict conditions so that the second component diffuses inside the aggregate has been used, but in such a case, it has been difficult to realize good solid-gas contact conditions ( SM
oroka, T .; Okubo, K .; Kusakab
e: Powder Technology. , 63, 105
(1990)).
【０００５】[0005]
【発明が解決しようとする課題】本発明は、このような
従来技術が持つ欠点を克服し、微粒子の安定な流動化
と、第２成分の拡散や反応の均一化を同時に実現した、
すなわち核粒子が１次粒子の状態まで均一に第２成分で
コーティングされ、しかも、その被覆状態が粒子状また
は膜状などとしてその複合構造が制御された複合粒子の
合成方法を提供することを目的として開発されたもので
ある。すなわち、本発明は、核粒子表面が第２成分で粒
子状や膜状などにコーティングされた被覆型複合粒子の
新規な合成方法を提供することを目的とするものであ
る。また、本発明は、触媒やセンサー材料など粒子状態
で機能を示す粉体や、あるいは軟磁性バルク体などの焼
結体原料粉体の高機能化を可能とする合成方法として好
適な被覆型複合粒子の合成方法を提供することを目的と
するものである。DISCLOSURE OF THE INVENTION The present invention overcomes the drawbacks of the prior art, and achieves stable fluidization of fine particles and uniform diffusion and reaction of the second component at the same time.
In other words, an object of the present invention is to provide a method for synthesizing composite particles in which the core particles are uniformly coated with the second component up to the state of the primary particles, and the state of the coating is particulate or film-like and the composite structure is controlled. It was developed as That is, an object of the present invention is to provide a novel method for synthesizing a coated composite particle in which the core particle surface is coated with the second component in the form of particles or a film. Further, the present invention provides a coating type composite suitable as a synthesizing method capable of enhancing the functionality of a powder that functions in a particle state such as a catalyst or a sensor material, or a raw material powder of a sintered body such as a soft magnetic bulk body. It is an object of the present invention to provide a method for synthesizing particles.
【０００６】[0006]
【課題を解決するための手段】上記課題を解決するため
の本発明は、振動流動層法を利用して、核粒子表面が第
２成分でコーティングされた被覆型複合粒子を合成する
方法であって、微粒子（核粒子）に、その凝集を解砕す
るための粗粒子（媒体粒子）を添加するとともに、流動
化ガスを供給して核粒子を凝集を制御しつつ流動化させ
て核粒子の流動層を形成させ、流動化状態にある核粒子
に第２成分形成用の原料を供給して、その化学反応によ
り核粒子表面に第２成分のコーティングを行うことを特
徴とする、被覆型複合粒子の合成方法、に係るものであ
る。また、本発明は、複合粒子が軟磁性バルク体の原料
粉体である前記の被覆型複合粒子の合成方法、及び流動
層を加熱する前記の被覆型複合粒子の合成方法、を好ま
しい実施態様とするものである。次に、本発明について
更に詳述する。本発明者らは、微粒子の安定流動化と、
第２成分の拡散や反応の均一化を同時達成した複合粒子
合成方法を開発するため鋭意研究を重ね、ミクロンオー
ダー以下の微粒子であっても低ガス流速で核粒子を流動
化できる振動流動層法を用い、その時同時に、核粒子の
凝集を解砕することを目的とした数１００ミクロンの粗
粒子から成る媒体粒子を加え、流動化状態にある核粒子
に第２成分形成用の原料を供給した。その結果、媒体粒
子の働きにより核粒子が１次粒子の状態まで均一に第２
成分でコーティングされ、また第２成分形成条件を制御
することで、被覆状態が粒子状または膜状など、構造が
制御された複合粒子が合成できることを見いだした。本
発明はかかる知見に基づいて完成したものである。According to the present invention, there is provided a method of synthesizing coated composite particles having a core particle surface coated with a second component by utilizing a vibrating fluidized bed method. Then, coarse particles (medium particles) for disintegrating the agglomeration are added to the fine particles (core particles), and a fluidizing gas is supplied to fluidize the core particles while controlling the agglomeration. A coating type composite comprising forming a fluidized bed, supplying a raw material for forming a second component to core particles in a fluidized state, and coating the surface of the core particles with a second component by a chemical reaction. A method for synthesizing particles. In addition, the present invention preferably includes a method for synthesizing the coated composite particles, wherein the composite particles are the raw material powder of the soft magnetic bulk material, and a method for synthesizing the coated composite particles, wherein the fluidized bed is heated. Is what you do. Next, the present invention will be described in more detail. The present inventors have found that stable fluidization of fine particles,
A vibrating fluidized bed method that enables the nuclear particles to be fluidized at a low gas flow rate even for fine particles of the order of microns or less, in order to develop a method for synthesizing composite particles that simultaneously achieves diffusion of the second component and uniformization of the reaction. At the same time, medium particles composed of coarse particles of several hundred microns for the purpose of breaking up agglomeration of the core particles were added, and the raw material for forming the second component was supplied to the core particles in a fluidized state. . As a result, the core particles are uniformly converted to the primary particles by the action of the medium particles.
It has been found that by controlling the conditions for forming the second component by coating with the components, it is possible to synthesize composite particles having a controlled structure such as a particulate or film-like coating. The present invention has been completed based on such findings.
【０００７】すなわち、本発明は核粒子に媒体粒子を添
加し、振動流動層法で核粒子を凝集を抑制しつつ流動化
させ、そこへ第２成分原料を供給し、適当な反応によっ
て核粒子表面に第２成分を形成することを特徴とする、
複合粒子の合成方法を提供するものである。That is, according to the present invention, the medium particles are added to the core particles, the core particles are fluidized while suppressing aggregation by a vibration fluidized bed method, the second component material is supplied thereto, and the core particles are subjected to an appropriate reaction. Forming a second component on the surface,
The present invention provides a method for synthesizing composite particles.
【０００８】本発明方法においては、予め合成された核
粒子を振動流動層反応装置へ充填する。このとき核粒子
の種類については特に制限はないが、例えば、軟磁性バ
ルク体の焼結体原料粉体である鉄粒子などが例示され
る。サイズについては、ミクロンオーダー以下のＧｅｌ
ｄａｒｔのＣ粉体と呼ばれる難流動化性の粒子を本発明
方法の対象とする。好適には０．１〜１０ミクロンの粒
子が例示される。In the method of the present invention, nuclear particles synthesized in advance are charged into a vibrating fluidized bed reactor. At this time, the type of the core particles is not particularly limited, and examples thereof include iron particles, which are raw material powders of a sintered soft magnetic bulk material. Regarding size, Gel of micron order or less
The hard-flowable particles, called dart C powders, are the subject of the process according to the invention. Preferably, particles of 0.1 to 10 microns are exemplified.
【０００９】また核粒子には予め媒体粒子を添加してお
く。媒体粒子の種類については振動流動化処理中安定
で、核粒子や第２成分と反応しないものであれば特に制
限はないが、例えば、化学的に安定なセラミックス製の
ビーズなどが例示される。サイズについては、流動化し
易く、しかも振動流動化処理後、核粒子との粒径差を利
用して分離し易い数１００ミクロン程度とする。Further, medium particles are added to the core particles in advance. The type of the medium particles is not particularly limited as long as it is stable during the vibration fluidization treatment and does not react with the core particles or the second component. Examples thereof include chemically stable ceramic beads. The size is set to about several hundred microns, which is easy to fluidize and, after the vibration fluidization treatment, is easily separated by utilizing the particle size difference from the core particles.
【００１０】第２成分はＣＶＤ法などの方法により、核
粒子を複合化する目的に応じた最適な反応系を用いて合
成する。例えば軟磁性バルク体では、高周波領域で透磁
率が低下する原因となる渦電流損失を低減する目的でバ
ルク体を高電気抵抗とするため被覆層には誘電体を形成
する反応系を選択する。また、第２成分としては、例え
ば、アルミナやシリカなどの酸化物が例示されるが、特
に制限されるものではない。The second component is synthesized by a method such as a CVD method using an optimum reaction system for the purpose of compounding the core particles. For example, in the case of a soft magnetic bulk material, a reaction system for forming a dielectric material is selected for the coating layer in order to increase the electrical resistance of the bulk material in order to reduce eddy current loss which causes a decrease in magnetic permeability in a high frequency region. Examples of the second component include oxides such as alumina and silica, but are not particularly limited.
【００１１】このようにして核粒子は１次粒子の状態ま
で均一に第２成分でコーティングされ、しかも、その被
覆状態が粒子状または膜状などとしてその複合構造が制
御された複合粒子が合成できる。In this way, the core particles can be uniformly coated with the second component up to the state of the primary particles, and the composite state can be synthesized by controlling the composite structure such that the coating state is a particle state or a film state. .
【００１２】次に、本発明の実施態様の１例を添付図面
に従って説明する。図１は本発明方法によって軟磁性バ
ルク体原料粉体を合成する場合の装置の１例の説明図で
ある。Next, an embodiment of the present invention will be described with reference to the accompanying drawings. FIG. 1 is an explanatory view of one example of an apparatus for synthesizing a soft magnetic bulk material powder by the method of the present invention.
【００１３】核粒子となる軟磁性材料微粒子と媒体粒子
とを混合した出発粉体を、スプリングで支持した石英反
応管へ充填し、反応管に加振装置を用いて振動を与え、
反応管下部よりガス分散器を通じて流動化ガスを供給
し、更に排気量をＰｕｍｐにより調節することにより、
出発粉体の流動層を形成させる。A starting powder obtained by mixing soft magnetic material fine particles serving as core particles and medium particles is charged into a quartz reaction tube supported by a spring, and vibration is applied to the reaction tube using a vibration device,
By supplying the fluidizing gas from the lower part of the reaction tube through a gas disperser and further adjusting the exhaust amount by Pump,
A fluidized bed of the starting powder is formed.
【００１４】第２成分原料を被覆成分気化器に充填し、
その気化温度に加熱して第２成分ガス（被覆成分ガス）
を発生させ、流動層へ供給する。[0014] The second component raw material is charged into a coating component vaporizer,
Heated to the vaporization temperature and the second component gas (coating component gas)
And supply it to the fluidized bed.
【００１５】このとき熱ＣＶＤ法などによって、流動層
を第２成分形成温度に加熱し核粒子表面に第２成分をコ
ーティングする。またこの際に媒体粒子の働きによっ
て、核粒子が１次粒子の状態まで均一に第２成分でコー
ティングされる。At this time, the fluidized bed is heated to a temperature for forming the second component by a thermal CVD method or the like, and the surface of the core particles is coated with the second component. At this time, the core particles are uniformly coated with the second component to the state of the primary particles by the action of the medium particles.
【００１６】更に、第２成分ガスに希釈ガスを混合して
その濃度を調節するなどＣＶＤ条件を制御することによ
り、その被覆状態が粒子状または膜状などとしてその構
造が制御された複合粒子を合成することができる。Further, by controlling the CVD conditions such as adjusting the concentration by mixing a diluent gas with the second component gas, the composite particles whose structure is controlled such that the coating state is particulate or film-like is obtained. Can be synthesized.
【００１７】複合化処理後、反応管から処理粉体を回収
し、核粒子と媒体粒子の粒径差を利用して核粒子（複合
粒子）を取り出し、軟磁性材料バルク体原料粉体として
用いる。After the complexing treatment, the treated powder is recovered from the reaction tube, the core particles (composite particles) are taken out by utilizing the difference in particle diameter between the core particles and the medium particles, and used as the raw material powder of the soft magnetic material bulk body. .
【００１８】[0018]
【実施例】次に、実施例により本発明を更に詳細に説明
するが、本発明はこの例によってなんら限定されるもの
ではない。Next, the present invention will be described in more detail by way of examples, which should not be construed as limiting the present invention.
【００１９】実施例 本実施例においては、鉄粒子について、鉄−アルミナの
複合粒子を合成した例を示す。Example In this example, an example in which iron-alumina composite particles are synthesized for iron particles will be described.
【００２０】核粒子である直径５ミクロンの鉄粒子を、
媒体粒子である直径１００ミクロンのジルコニア粒子と
混合して出発粉体を作製し、加熱帯長さ３００ミリメー
ターの石英反応管へ充填した。反応管には周波数６０ヘ
ルツ、最大振幅３ミリメーターの振動を与え、１リット
ル／分〜２．５リットル／分のアルゴンガス（流動化ガ
ス）を供給し、水封ポンプで排気量を調節することによ
り、出発粉体を流動化状態とした。The iron particles having a diameter of 5 microns, which are core particles, are
A starting powder was prepared by mixing with zirconia particles having a diameter of 100 microns, which were medium particles, and charged into a quartz reaction tube having a heating zone length of 300 mm. Vibration at a frequency of 60 Hz and a maximum amplitude of 3 millimeters is applied to the reaction tube, and argon gas (fluidizing gas) of 1 liter / min to 2.5 liter / min is supplied, and the displacement is adjusted by a water ring pump. This brought the starting powder into a fluidized state.
【００２１】第２成分原料にはアルミニウムイソプロポ
キシド（ＡＩＰ）を用い、約２００℃でＡＩＰ蒸気を発
生させ、流動化状態にある核粒子にアルゴンガスをキャ
リアガスとして０．５リットル／分〜１リットル／分で
ＡＩＰ蒸気を供給した。Aluminum isopropoxide (AIP) is used as the second component material, AIP vapor is generated at about 200 ° C., and 0.5 liter / min. AIP vapor was supplied at 1 liter / min.
【００２２】流動層温度は２５０℃〜５００℃の間で制
御し、ＡＩＰの熱分解反応を反応系として用いて鉄粒子
表面にアルミナをコーティングした。The temperature of the fluidized bed was controlled between 250 ° C. and 500 ° C., and the surface of iron particles was coated with alumina using a thermal decomposition reaction of AIP as a reaction system.
【００２３】アルミナを粒子状にコーティングする場
合、流動層温度５００℃、加振振幅１ミリメーター、流
動化ガス流量２．５リットル／分、キャリアガス流量１
リットル／分、希釈ガス流量０リットル／分とした。In the case where alumina is coated in the form of particles, the fluidized bed temperature is 500 ° C., the vibration amplitude is 1 millimeter, the fluidizing gas flow rate is 2.5 liter / min, and the carrier gas flow rate is 1
Liter / minute, and the dilution gas flow rate was 0 liter / minute.
【００２４】得られた複合粒子の電子顕微鏡観察結果を
図２に示す。数ミクロンの大粒子が鉄粒子、その表面に
付着した数１０〜１００ナノメーター程度の小粒子がア
ルミナ粒子である。FIG. 2 shows the results of electron microscopic observation of the obtained composite particles. Large particles of several microns are iron particles, and small particles of several tens to 100 nanometers attached to the surface are alumina particles.
【００２５】鉄粒子が１次粒子の状態まで均一にアルミ
ナ粒子でコーティングされた複合粒子を合成することが
できた。It was possible to synthesize composite particles in which iron particles were uniformly coated with alumina particles up to the state of primary particles.
【００２６】アルミナを膜状にコーティングする場合、
流動層温度２５０℃、加振振幅１．６ミリメーター、流
動化ガス流量１リットル／分、キャリアガス流量０．５
リットル／分、希釈ガス流量２リットル／分とした。When coating alumina in a film form,
Fluidized bed temperature 250 ° C, vibration amplitude 1.6 millimeters, fluidizing gas flow rate 1 liter / min, carrier gas flow rate 0.5
Liter / minute, and the dilution gas flow rate was 2 liter / minute.
【００２７】得られた複合粒子の電子顕微鏡観察結果を
図３に示す。数ミクロンの大粒子が鉄粒子、その表面に
形成された数１０ナノメーターオーダーの薄膜がアルミ
ナ層である。FIG. 3 shows the results of electron microscopic observation of the obtained composite particles. Large particles of several microns are iron particles, and a thin film of several tens of nanometers formed on the surface is an alumina layer.
【００２８】鉄粒子が１次粒子の状態まで均一にアルミ
ナ薄膜でコーティングされた複合粒子を合成することが
できた。It was possible to synthesize composite particles in which iron particles were uniformly coated with an alumina thin film up to the state of primary particles.
【００２９】この複合粒子を用いて軟磁性材料バルク体
を作製した結果、１０-2アンペア・センチメーター〜１
０-1アンペア・センチメーターの高い電気抵抗値を有す
るバルク体が得られた。鉄単体では１０-5アンペア・セ
ンチメーターであり、これは複合粒子表面のアルミナ薄
膜が、バルク体の粒界にアルミナ層を形成した結果と考
えられる。すなわち複合粒子を用いることで、高周波領
域で透磁率が低下する原因となる渦電流損失を低減する
ため、軟磁性材料バルク体を高電気抵抗化することがで
きた。As a result of producing a soft magnetic material bulk body using the composite particles, 10 −2 amperes / cm to 1 cm
A bulk body having a high electrical resistance of 0 -1 amp-cm was obtained. It is 10 −5 amper centimeters for iron alone, which is considered to be the result of the alumina thin film on the surface of the composite particles forming an alumina layer at the grain boundary of the bulk body. That is, by using the composite particles, the eddy current loss which causes a decrease in the magnetic permeability in a high frequency region is reduced, so that the electrical resistance of the soft magnetic material bulk body can be increased.
【００３０】[0030]
【発明の効果】本発明によると、簡便な方法で、核粒子
表面にその１次粒子の状態まで均一に第２成分でコーテ
ィングでき、しかもその被覆状態が粒子状または膜状な
どとして構造が制御された複合粒子を容易に合成するこ
とができ、本発明方法は、触媒やセンサー材料など粒子
状態で機能を示す粉体や、あるいは軟磁性バルク体など
の焼結体原料粉体の高機能化を可能とする合成方法とし
て好適である。According to the present invention, it is possible to coat the surface of the core particles with the second component uniformly to the state of the primary particles by a simple method, and the structure is controlled such that the coating state is a particle or a film. Can be easily synthesized, the method of the present invention can be used to enhance the functionality of powders that exhibit functions in the form of particles such as catalysts and sensor materials, or raw material powders of sintered compacts such as soft magnetic bulk bodies. It is suitable as a synthesis method that enables
【図１】本発明方法を実施するための装置の１例の説明
図である。FIG. 1 is an explanatory diagram of an example of an apparatus for carrying out the method of the present invention.
【図２】本発明方法により得られた鉄粒子とアルミナ粒
子との複合粒子の微細構造（金属材料とセラミックス材
料の複合体の組織）を示す電子顕微鏡写真図である（Ｆ
ｅは鉄粒子、Ａｌ2 Ｏ3 はアルミナ粒子を示す）。FIG. 2 is an electron micrograph showing the microstructure (structure of a composite of a metal material and a ceramic material) of a composite particle of iron particles and alumina particles obtained by the method of the present invention (F
e indicates iron particles, and Al 2 O 3 indicates alumina particles).
【図３】本発明方法により得られた鉄粒子とアルミナ薄
膜との複合粒子の微細構造（金属材料とセラミックス材
料の複合体の組織）を示す電子顕微鏡写真図である（Ｆ
ｅは鉄粒子、Ａｌ2 Ｏ3 はアルミナ薄膜を示す）。FIG. 3 is an electron micrograph showing the microstructure (structure of a composite of a metal material and a ceramic material) of a composite particle of iron particles and an alumina thin film obtained by the method of the present invention (F
e indicates iron particles, and Al 2 O 3 indicates an alumina thin film).
Claims (3)
第２成分でコーティングされた被覆型複合粒子を合成す
る方法であって、微粒子（核粒子）に、その凝集を解砕
するための粗粒子（媒体粒子）を添加するとともに、流
動化ガスを供給して核粒子を凝集を制御しつつ流動化さ
せて核粒子の流動層を形成させ、流動化状態にある核粒
子に第２成分形成用の原料を供給して、その化学反応に
より核粒子表面に第２成分のコーティングを行うことを
特徴とする、被覆型複合粒子の合成方法。1. A method for synthesizing coated composite particles having a core particle surface coated with a second component using a vibrating fluidized bed method, wherein the aggregation is broken into fine particles (nuclear particles). And a fluidizing gas to supply the fluidized particles while controlling the agglomeration to form a fluidized bed of the nuclear particles. A method for synthesizing coated composite particles, comprising supplying a raw material for forming two components and coating the surface of the core particles with a second component by a chemical reaction.
ある請求項１記載の被覆型複合粒子の合成方法。2. The method for synthesizing coated composite particles according to claim 1, wherein the composite particles are a raw material powder of a soft magnetic bulk material.
複合粒子の合成方法。3. The method according to claim 1, wherein the fluidized bed is heated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13080496A JP2843907B2 (en) | 1996-04-26 | 1996-04-26 | Composite particle synthesis method by vibrating fluidized bed method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13080496A JP2843907B2 (en) | 1996-04-26 | 1996-04-26 | Composite particle synthesis method by vibrating fluidized bed method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09290143A JPH09290143A (en) | 1997-11-11 |
| JP2843907B2 true JP2843907B2 (en) | 1999-01-06 |
Family
ID=15043107
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13080496A Expired - Lifetime JP2843907B2 (en) | 1996-04-26 | 1996-04-26 | Composite particle synthesis method by vibrating fluidized bed method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2843907B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6963222B2 (en) | 2020-04-12 | 2021-11-05 | 由城 紫垣 | A method that enables uniform contact between gas and powder by providing a rocking mechanism, and an air-solid contact device for a packed bed, a moving bed, and a multi-stage fluidized bed using the method. |
-
1996
- 1996-04-26 JP JP13080496A patent/JP2843907B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH09290143A (en) | 1997-11-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR960002416B1 (en) | Spray conversion process for the production of nanophase composite powders | |
| JP2751136B2 (en) | Method for producing self-grading composite particles | |
| JP2017528591A (en) | Parts manufacturing method | |
| JP2002507055A (en) | Ferromagnetic particles | |
| US3475158A (en) | Production of particulate,non-pyrophoric metals and product | |
| JP2843907B2 (en) | Composite particle synthesis method by vibrating fluidized bed method | |
| JPS6257568B2 (en) | ||
| US5298296A (en) | Process for the elaboration of powders uniformly coated with ultrafine silicon-base particles using chemical vapor decomposition in the presence of core powders | |
| Shin et al. | Deposition of diamond coatings on particles in a microwave plasma-enhanced fluidized bed reactor | |
| US5527747A (en) | Rapid process for the preparation of diamond articles | |
| TW502307B (en) | Method for preparation of diamond film | |
| JP2004107096A (en) | Oriented silicon carbide sintered body and method for producing the same | |
| JPS5884107A (en) | Plasma nitriding method | |
| RU2629416C2 (en) | Method for producing composite powder material by cladding | |
| JPH02102730A (en) | Production of multiple fine powdery material | |
| Barinova et al. | Effect of iron oxalate additions on the phase composition of combustion products of silicon–carbon mixtures in nitrogen | |
| US3592627A (en) | Production of particulate,non-pyrophoric metals | |
| JPH01283305A (en) | Production of metallic iron powder from ferrous dust | |
| Shishido et al. | Synthesis of porous γ-gallium oxide films using refrigerator aging oxidation from gallium nanoparticles | |
| JPS62121643A (en) | Preparation of powder using laser | |
| Kim et al. | Preparation of Mechanically Robust, Macroscopic Low-Density Gold Foams by Highly Efficient Electroless Gold Plating | |
| JPH0648709A (en) | Production of silicon nitride powder | |
| JPH03245835A (en) | Coating method for surface of particle with ultrafine particle | |
| JPH03122094A (en) | Method for vapor synthesis of fine diamond grain | |
| JPS62121642A (en) | Apparatus for preparing powder using laser |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| EXPY | Cancellation because of completion of term |