JPH0644990B2 - Manufacturing method of composite fine powder material - Google Patents
Manufacturing method of composite fine powder materialInfo
- Publication number
- JPH0644990B2 JPH0644990B2 JP63258071A JP25807188A JPH0644990B2 JP H0644990 B2 JPH0644990 B2 JP H0644990B2 JP 63258071 A JP63258071 A JP 63258071A JP 25807188 A JP25807188 A JP 25807188A JP H0644990 B2 JPH0644990 B2 JP H0644990B2
- Authority
- JP
- Japan
- Prior art keywords
- fine powder
- fluidized bed
- fluidized
- substance
- powder
- 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
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Chemical Vapour Deposition (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、微粉体を流動化し、完全ドライプロセスで、
第二成分を気相反応法(Chemical Vapor Deposition, CV
D)によって当該微粉体上に析出させ、極めて均質な複合
超微粉体を連続的に作製する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention fluidizes a fine powder, and uses a complete dry process.
The second component is a gas phase reaction method (Chemical Vapor Deposition, CV
The method D) relates to a method for continuously producing extremely homogeneous composite ultrafine powder by depositing on the fine powder.
従来、複数の超微粉体を均一に混合して、複合微粉体材
料を作製しようとする場合は、予め別々に作製した微粉
体を、振動ボールミルなどによって強力なエネルギーを
加えて混合するのが通常である。乳鉢で混ぜ合わせたく
らいでは、超微粉体は全く混合しない。振動ボールミル
のような高エネルギー混合器は、混合器自身も粉砕され
て行くので、微粉体の汚染を避けることができない。Conventionally, when it is attempted to uniformly mix a plurality of ultrafine powders to produce a composite fine powder material, the fine powders produced separately in advance are mixed by applying strong energy with a vibrating ball mill or the like. It is normal. Even if mixed in a mortar, the ultrafine powder does not mix at all. In a high-energy mixer such as a vibrating ball mill, the mixer itself is also crushed, so that contamination of fine powder cannot be avoided.
また、微粉体を焼結成型する場合は、微粉体単味で焼結
することはほとんどなく、焼結助剤を添加することが多
い。通常は、微粉体を助剤を溶解した溶液中に浸せきし
た後に乾燥する。しかし、超微粉体を乾燥する際には、
溶液の偏在が生じ、均一に助剤が混合することは困難で
ある。Further, when the fine powder is sintered and molded, the fine powder is rarely sintered alone, and a sintering aid is often added. Usually, the fine powder is dipped in a solution in which the auxiliary agent is dissolved and then dried. However, when drying the ultrafine powder,
Uneven distribution of the solution occurs, and it is difficult to mix the auxiliary agent uniformly.
特開昭63-55112号公報には、超短波によって加熱される
流動床反応器にて、高純度シリコン粒子状にシラン、2
塩化シラン、3塩化シラン、3臭化シランのシリコン含有
ガスの熱分解又は水素還元反応による化学蒸着によって
シリコンを析出する高純度多結晶シリコンの製造方法及
びその装置が記載されている。上記公報は、流動層CVD
(気相反応法)によるシリコン製造方法に関するものであ
り、複合微粉体材料に関するものではない。Japanese Patent Laid-Open No. 63-55112 discloses that in a fluidized bed reactor heated by ultrashort waves, silane, 2
A method and an apparatus for producing high-purity polycrystalline silicon in which silicon is deposited by chemical vapor deposition by thermal decomposition or hydrogen reduction reaction of silicon-containing gas of silane chloride, silane trichloride, and silane tribromide are described. The above publication is a fluidized bed CVD
The present invention relates to a method for producing silicon by (gas phase reaction method), not to a composite fine powder material.
特開昭63-216904号公報には、磁性を有する芯部と、こ
の芯部を被覆する被覆層とを有し、被覆層がTi並びにN
及び/もしくはCを含有するか、またはAl及びNを含有す
る磁性粒子及びその製造方法が記載されている。上記公
報では、芯部に振動を与えながら、プラズマCVD法によ
り被覆層を設層する方法で磁性粒子を製造している。Japanese Unexamined Patent Publication No. 63-216904 has a core having magnetism and a coating layer for coating the core, and the coating layer includes Ti and N.
Magnetic particles containing C and / or C or containing Al and N and methods of making the same are described. In the above publication, magnetic particles are manufactured by a method of forming a coating layer by a plasma CVD method while applying vibration to the core.
この特開昭63-216904号公報は、複合微粉体材料とし
て、粒子表面にCVDによって他の物質を析出させ改質す
るものである。すなわち、第2図に示すように、物質Aの
表面にCVDにより物質Bを被覆するものである。したがっ
て、作製された物質は、力学的にはAであっても、化学
的にはBの性状になるといった表面の改質方法である。This Japanese Patent Application Laid-Open No. 63-216904 discloses a composite fine powder material in which another substance is deposited on the surface of a particle by CVD to modify it. That is, as shown in FIG. 2, the surface of the substance A is coated with the substance B by CVD. Therefore, the produced substance is a method of modifying the surface such that it is mechanically A but chemically B.
一般に、30〜40μmよりも小さな粒子径を持つ粉体は、
流動化がきわめて困難であるとされている。Generally, powders with particle sizes smaller than 30-40 μm are
Liquidation is said to be extremely difficult.
本発明者は、微粉体の流動化について種々の研究・実験
を重ねた結果、粒径10μm以下の粒子が、特別の振動、
撹拌を加えなくとも、ガス流速を数cm/s以上にすれば、
十分に流動化できることを知見した。The present inventor has conducted various researches and experiments on fluidization of fine powder, and as a result, particles with a particle diameter of 10 μm or less have a special vibration,
Even without stirring, if the gas flow rate is set to several cm / s or more,
We have found that they can be sufficiently fluidized.
本発明は上記の諸点に鑑みなされたもので、複合微粉体
材料に使用する超微粉を流動化し、この流動層内に混合
しようとする第二成分を気体で投入して、気相反応法(C
hemical Vapor Deposition)によって、流動媒体である
超微粉粒子上に析出させて極めて均質な複合体を製造す
る方法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 points, fluidizes the ultrafine powder used for the composite fine powder material, and introduces the second component to be mixed in the fluidized bed by gas, and the gas phase reaction method ( C
It is an object of the present invention to provide a method for producing an extremely homogeneous composite by precipitating it on ultrafine powder particles which is a fluid medium by means of chemical vapor deposition.
上記の目的を達成するために、本発明の複合微粉体材料
の製造方法は、第一の微粉体を流動化させて流動層を形
成し、この流動層内に第二の微粉体を気体状で吹き込ん
で、第一の微粉体上の一部に第二の微粉体を析出させ、
均質な複合微粉体を作製するようにしたものである。In order to achieve the above object, a method for producing a composite fine powder material according to the present invention comprises fluidizing a first fine powder to form a fluidized bed, and forming a second fine powder in a gaseous state in the fluidized bed. Blow in to deposit the second fine powder on a part of the first fine powder,
It is intended to produce a homogeneous composite fine powder.
第一の微粉体は、常圧近傍で流動化するのが望ましい。It is desirable that the first fine powder be fluidized near atmospheric pressure.
また、第一の微粉体より大きい粗大粒子を流動層に加え
て流動層中で流動化させる場合がある。Further, coarse particles larger than the first fine powder may be added to the fluidized bed and fluidized in the fluidized bed.
さらに、流動層に振動または撹拌を加える場合がある。Furthermore, vibration or agitation may be added to the fluidized bed.
流動層中の微粉体は、複数個が会合してアグロメレート
を形成している。反応条件を調整すれば、アグロメレー
トの表面のみでなく、アグロメレート内部、すなわち個
々の第一の粒子の表面に均一に析出させることができ
る。直径1〜20mmの粗大粒子を流動層中で流動化し、こ
れによって超微粉体の流動化を維持する場合、または流
動層に振動あるいは撹拌を加える場合には、アグロメレ
ートが生成せずに、微粉体が分散して流動化することが
あるが、当然、この場合にも、第二成分の均一な析出が
得られる。A plurality of fine powders in the fluidized bed are associated with each other to form agglomerates. By adjusting the reaction conditions, not only the surface of the agglomerates but also the inside of the agglomerates, that is, the surfaces of the individual first particles can be uniformly deposited. When fluidizing coarse particles with a diameter of 1 to 20 mm in a fluidized bed to maintain the fluidization of ultrafine powder, or when vibrating or agitating the fluidized bed, agglomerates are not formed and fine powder is generated. Although the body may be dispersed and fluidized, naturally, in this case as well, uniform precipitation of the second component is obtained.
以下、本発明の方法を第1図に基づいて詳細に説明す
る。希釈用窒素は窒素ボンベ1の止弁2を通り、圧力制
御装置3で圧力が制御され、マノメーター4で流量が測
定される。酸素吸収装置5で酸素が取り除かれ、脱水装
置6、7で水分が除かれる。この窒素ラインは二系列あ
り、一方の窒素は、アンモニアボンベ8からのアンモニ
アと混合されて、圧力制御装置10で圧力が制御され、
止弁11を通り、マノメーター12で流量を計測し、脱
水装置13で脱水した後、ノズル14から流動層15内
に投入される。Hereinafter, the method of the present invention will be described in detail with reference to FIG. The diluting nitrogen passes through the stop valve 2 of the nitrogen cylinder 1, the pressure is controlled by the pressure control device 3, and the flow rate is measured by the manometer 4. Oxygen is removed by the oxygen absorbing device 5, and water is removed by the dehydrating devices 6 and 7. This nitrogen line has two series, and one of the nitrogen lines is mixed with ammonia from the ammonia cylinder 8 and the pressure is controlled by the pressure control device 10,
After passing through the stop valve 11, the flow rate is measured by the manometer 12, the water is dehydrated by the dehydrator 13, and then the liquid is fed from the nozzle 14 into the fluidized bed 15.
別の系列の窒素は、塩化チタン(TiCl4)蒸発装置16に
送られ、塩化チタンガスを希釈した後、流動層15内に
吹き込まれる。Another series of nitrogen is sent to a titanium chloride (TiCl 4 ) evaporator 16 to dilute the titanium chloride gas and then blown into the fluidized bed 15.
流動層15は、たとえば微粉の窒化珪素で形成されてお
り、流動層内に析出した窒化チタンと混合され、飛び出
し、フィルター17にて捕集されて製品とされる。1
8、20は温度計、21は充填床(ガス分散器)、22は
ヒーター、23はアンモニアおよび塩化チタンの吸収装
置である。The fluidized bed 15 is made of, for example, fine powder silicon nitride, is mixed with titanium nitride deposited in the fluidized bed, jumps out, and is collected by the filter 17 to be a product. 1
8 and 20 are thermometers, 21 is a packed bed (gas disperser), 22 is a heater, and 23 is an absorber of ammonia and titanium chloride.
本発明は、物質Aと物質Bとの単なる混合方法を示してい
るものであり、物質表面へのCVD析出を目的としている
わけではない。The present invention shows a mere mixing method of the substance A and the substance B, and is not intended for CVD deposition on the surface of the substance.
物質Aと物質Bの微粉を機械的に混合すると、粒度が小さ
いので、第3図に示すように均一にはならない。When the fine powders of the substance A and the substance B are mechanically mixed, they are not uniform as shown in FIG. 3 because of the small particle size.
そこで、物質A又は物質Bを流動化させて他の物質B又はA
をCVDで析出させると、第4図のようになる。すなわち、
1つの粒子毎に物質Aと物質Bとが存在し、全体としては
物質Aと物質Bとを均一に混合したものとなる。CVDによ
る析出は、なにも粒子表面を均一にコーチングする必要
はなく、したがって改質する必要もなく、ただ、Aとい
う物質とBという物質とが均一に混合すればよいだけで
ある。本発明では、上記のことが可能である。Therefore, the substance A or B is fluidized and the other substance B or A is
Fig. 4 shows the result of CVD deposition. That is,
The substance A and the substance B exist for each particle, and the substance A and the substance B are uniformly mixed as a whole. Precipitation by CVD does not require any uniform coating of the particle surface and therefore no modification, only that the substance A and the substance B are uniformly mixed. The present invention is capable of the above.
つぎに実施例を挙げて説明する。 Next, examples will be described.
実施例1 本実施例は、窒化珪素微粉体上へ窒化チタンを析出させ
る場合の方法に関するものである。窒化珪素は優れた高
温材料であるが、電気伝導度がないために、放電加工が
できない。そこで、窒化珪素に、電気伝導性を有する窒
化チタンを混合して焼結すれば、放電加工が可能な窒化
珪素が得られる。従来は、窒化珪素微粉体と窒化チタン
微粉体とを混合していたので、放電加工可能な電気伝導
度を得るためには20wt%程度の窒化チタン混合する必要
があった。Example 1 This example relates to a method for depositing titanium nitride on silicon nitride fine powder. Although silicon nitride is an excellent high temperature material, it cannot be electric discharge machined because it has no electrical conductivity. Therefore, by mixing titanium nitride having electrical conductivity with silicon nitride and sintering the mixture, silicon nitride capable of electric discharge machining can be obtained. In the past, since the silicon nitride fine powder and the titanium nitride fine powder were mixed, it was necessary to mix titanium nitride in an amount of about 20 wt% in order to obtain electric conductivity capable of electric discharge machining.
第1図における酸素吸収装置5として、活性化銅を充填
した槽を用いて脱酸素し、脱水装置6(シリカゲルを充
填した槽)および脱水装置7(ドライアイストラップ)を
用いて脱水した窒素でアンモニアを希釈し、ノズル14
から内径35mmの流動層15内に吹き込んだ。塩化チタン
容器を恒温槽内に保った塩化チタン蒸発装置16に、前
記の脱酸素、脱水した窒素を通過させて一定量の塩化チ
タンを蒸発させ、アンモニアとは別の入口から流動層1
5内に吹き込んだ。流動層15内には、1100℃の温度
で、サブミクロンの窒化珪素微粉体を脱酸素、脱水した
常圧窒素で流動化しておいた。飛び出した粒子はろ紙を
用いたフイルター17へ捕集した。塩化チタンの流量
は、流動層出口でガスを分析し、アンモニアの流量(測
定してある)を基に算出した。As the oxygen absorber 5 in FIG. 1, nitrogen was deoxidized using a tank filled with activated copper, and dehydrated using a dehydrator 6 (tank filled with silica gel) and a dehydrator 7 (dry ice trap). Dilute ammonia, nozzle 14
Was blown into the fluidized bed 15 having an inner diameter of 35 mm. The deoxygenated and dehydrated nitrogen is passed through a titanium chloride vaporizer 16 in which a titanium chloride container is kept in a constant temperature bath to vaporize a fixed amount of titanium chloride, and a fluidized bed 1 is introduced from an inlet different from ammonia.
I blew in 5. In the fluidized bed 15, the submicron silicon nitride fine powder was fluidized with deoxidized and dehydrated atmospheric pressure nitrogen at a temperature of 1100 ° C. The particles that jumped out were collected in the filter 17 using filter paper. The flow rate of titanium chloride was calculated based on the flow rate (measured) of ammonia by analyzing the gas at the fluidized bed outlet.
得られた微粉体は、窒化珪素微粉体に窒化チタン微粉体
が混合したものであった。得られた窒化チタンの結晶子
径は、窒化チタンの析出量とともに増加し、反応温度の
増加とともに減少し、20〜100nmの範囲であった。X線
マイクロアナライザー、電子線回折、および透過電子顕
微鏡による測定の結果、窒化珪素と窒化チタンとの混合
は極めて均一であることが示された。この微粉体を1700
℃以上で窒素雰囲気で焼結して、電気伝導度を測定した
ところ、放電加工に十分適した焼結体が得られた。窒化
珪素と窒化チタン微粉体をおのおの製造した後に混合し
た場合は、実用的な電気伝導度となるためには、窒化チ
タンの量が約20wt%必要であるが、本例の方法では、そ
の半分以下に低下した。The obtained fine powder was a mixture of silicon nitride fine powder and titanium nitride fine powder. The crystallite size of the obtained titanium nitride increased with the precipitation amount of titanium nitride and decreased with the increase of the reaction temperature, and was in the range of 20 to 100 nm. As a result of measurement by an X-ray microanalyzer, electron diffraction, and a transmission electron microscope, it was shown that the mixture of silicon nitride and titanium nitride was extremely uniform. 1700 this fine powder
When the electrical conductivity was measured by sintering in a nitrogen atmosphere at ℃ or higher, a sintered body sufficiently suitable for electrical discharge machining was obtained. When silicon nitride and titanium nitride fine powder are manufactured and then mixed, the amount of titanium nitride is required to be about 20 wt% in order to obtain practical electric conductivity. Fell below.
なお、本実施例では、流動層の温度を500〜1200℃に保
つのが望ましい。In this example, it is desirable to keep the temperature of the fluidized bed at 500 to 1200 ° C.
実施例2 本実施例は、アルミナとチタニアとの複合微粉体を製造
する方法に関するものである。サブミクロンのアルミナ
微粉体を、流動層15内で乾燥した常圧空気で流動化
し、1200℃に保ち、塩化チタン蒸気を送入したところ、
アルミナとチタニアの混合超微粒子が得られた。X線回
折、X線マイクロアナライザー、電子顕微鏡などによる
測定結果、アルミナとチタニアとが均一に混合している
ことがわかった。反応後も流動状態は良好で、層の閉塞
などは起こらなかった。Example 2 This example relates to a method for producing a composite fine powder of alumina and titania. When the submicron alumina fine powder was fluidized with atmospheric air dried in the fluidized bed 15 and kept at 1200 ° C. and titanium chloride vapor was fed,
Mixed ultrafine particles of alumina and titania were obtained. As a result of measurement by X-ray diffraction, an X-ray microanalyzer, an electron microscope, etc., it was found that alumina and titania were uniformly mixed. After the reaction, the fluid state was good, and the layer did not clog.
なお、本実施例では、流動層の温度を800〜1300℃に保
つのが望ましい。In this example, it is desirable to keep the temperature of the fluidized bed at 800 to 1300 ° C.
実施例3 本実施例は、媒体粒子を流動化した流動層でアルミナと
チタニアとの複合微粉体を製造する方法に関するもので
ある。Example 3 This example relates to a method for producing a composite fine powder of alumina and titania in a fluidized bed in which medium particles are fluidized.
実施例2の系で、流動状態を向上させるために、直径1〜
5mmの範囲にある分級したアルミナ粒子を空気で流動化
し、その中にアルミナ微粉体を送入し、アルミナ粗粒子
とともに流動化した。流動状態は、アルミナ微粉体単味
の流動層よりも、さらに向上した。そこに塩化チタンを
送入してチタニア微粉体を析出させた。本実施例では、
アルミナとチタニア微粉体の混合度は、実施例2よりも
さらに向上したが、微粉体の飛び出しが多くなった。し
かし、気相反応法(Chemical Vapor Deposition)で析出
させるべき第二成分の量が少なくてもよい場合には、反
応は十分速やかに起こるので、飛び出しがあっても操作
の阻害にはならなかった。さらに、連続的にアルミナ超
微粉体を流動層内に供給し、連続的に飛び出せることに
より、アルミナ・チタニア混合微粉体を連続して生産で
きた。In the system of Example 2, in order to improve the flow state, the diameter of 1 ~
Classified alumina particles in the range of 5 mm were fluidized with air, and fine alumina powder was fed into the fluidized particles, and fluidized with coarse alumina particles. The fluidized state was further improved as compared with the fluidized bed of the fine alumina powder alone. Titanium chloride was fed thereinto to deposit fine titania powder. In this embodiment,
The degree of mixing of the alumina and the titania fine powder was further improved as compared with Example 2, but the amount of the fine powder jumped out increased. However, when the amount of the second component to be precipitated by the vapor phase reaction method (Chemical Vapor Deposition) may be small, the reaction occurs sufficiently quickly, and even if there is a jump out, it did not hinder the operation. . Further, by continuously supplying the ultrafine alumina powder into the fluidized bed and continuously ejecting it, the alumina / titania mixed fine powder could be continuously produced.
本発明の実施例では、振動あるいは撹拌を加えない流動
層を用いているが、振動、撹拌などの機械的エネルギー
を加えた流動層を用いてもよい。いずれにしても、微粉
体が運動した状態で常圧近傍の気体と接触し、気相反応
法によって、第二成分をドライプロセスで添加すること
を特徴とするものである。粉体は連続的に供給あるいは
排出することができるが、仕込んだ粉体を回分式あるい
は半回分式に処理してもよい。In the embodiments of the present invention, a fluidized bed that is not subjected to vibration or stirring is used, but a fluidized bed to which mechanical energy such as vibration or stirring is added may be used. In any case, it is characterized in that the fine powder is brought into contact with a gas in the vicinity of normal pressure in a moving state, and the second component is added by a dry process by a gas phase reaction method. The powder can be continuously supplied or discharged, but the charged powder may be processed in a batch system or a semi-batch system.
上記の実施例は一例であって、これがすべてではない。
本発明は、粉体を何等かの方法により常圧またはそれに
近い圧力下で流動化し、気相反応法により、ドライプロ
セスで複合粉体を製造し、あるいは粉体の表面を修飾す
る方法を包含するものである。The above embodiments are examples and not all.
The present invention includes a method of fluidizing a powder by some method under normal pressure or a pressure close thereto and producing a composite powder by a dry process by a gas phase reaction method, or modifying the surface of the powder. To do.
本発明は上記のように構成されているので、従来、不可
能であった超微粉同士の混合を気相内で行うことがで
き、しかも混合の均一性は極めて高く、第一の微粉体上
の一部に第二の微粉体が析出した、品質の優れた複合微
粉体材料を製造することができる。また溶剤の使用は不
必要になり、かつ乾燥過程も不必要になるなどの効果を
有している。Since the present invention is configured as described above, it is possible to mix ultrafine powders in the gas phase, which was not possible conventionally, and the uniformity of mixing is extremely high. It is possible to produce a composite fine powder material of excellent quality in which the second fine powder is deposited on a part of the above. In addition, the use of a solvent is unnecessary and the drying process is also unnecessary.
第1図は本発明の複合微粉体材料の製造方法を実施する
装置の一例を示すフローシート、第2図は従来方法を示
し、複合微粉体材料として粒子表面にCVDにより他の物
質を析出させ改質する場合の概念図、第3図は従来方法
を示し、AとBの微粉を機械的に混合した場合の概念図、
第4図は本発明の方法を示し、物質A又は物質Bを流動化
させて他の物質B又はAをCVDで析出させた場合の概念図
である。 1……窒素ボンベ、2、11……止弁、3、10……圧
力制御装置、4、12……マノメーター、5……酸素吸
収装置、6、7、13……脱水装置、8……アンモニア
ボンベ、14……ノズル、15……流動層、16……塩
化チタン蒸発装置、17……フィルター、18、20…
…温度計、21……充填床、22……ヒーター、23…
…アンモニアおよび塩化チタンの吸収装置FIG. 1 is a flow sheet showing an example of an apparatus for carrying out the method for producing a composite fine powder material of the present invention, and FIG. 2 shows a conventional method, in which another substance is deposited on the particle surface by CVD as a composite fine powder material. Conceptual diagram when reforming, FIG. 3 shows a conventional method, a conceptual diagram when mechanically mixing fine powders of A and B,
FIG. 4 shows the method of the present invention, and is a conceptual diagram when the substance A or the substance B is fluidized and another substance B or the A is deposited by CVD. 1 ... Nitrogen cylinder, 2, 11 ... Stop valve, 3, 10 ... Pressure control device, 4, 12 ... Manometer, 5 ... Oxygen absorption device, 6, 7, 13 ... Dehydration device, 8 ... Ammonia cylinder, 14 ... Nozzle, 15 ... Fluidized bed, 16 ... Titanium chloride vaporizer, 17 ... Filter, 18, 20 ...
… Thermometer, 21… Packed bed, 22… Heater, 23…
... Ammonia and titanium chloride absorber
Claims (3)
し、この流動層内に第二の微粉体を気体状で吹き込ん
で、第一の微粉体上の一部に第二の微粉体を析出させ、
均質な複合微粉体を作製することを特徴とする複合微粉
体材料の製造方法。1. A fluidized bed is formed by fluidizing a first fine powder, and a second fine powder is blown into the fluidized bed in a gaseous state to form a second layer on a part of the first fine powder. Of fine powder of
A method for producing a composite fine powder material, which comprises producing a uniform composite fine powder.
に加えて流動層中で流動化させる請求項1記載の複合微
粉体材料の製造方法。2. The method for producing a composite fine powder material according to claim 1, wherein coarse particles larger than the first fine powder are added to the fluidized bed and fluidized in the fluidized bed.
記載の複合微粉体材料の製造方法。3. The vibration or stirring is applied to the fluidized bed.
A method for producing the composite fine powder material as described.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP63258071A JPH0644990B2 (en) | 1988-10-13 | 1988-10-13 | Manufacturing method of composite fine powder material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP63258071A JPH0644990B2 (en) | 1988-10-13 | 1988-10-13 | Manufacturing method of composite fine powder material |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH02102730A JPH02102730A (en) | 1990-04-16 |
JPH0644990B2 true JPH0644990B2 (en) | 1994-06-15 |
Family
ID=17315122
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP63258071A Expired - Lifetime JPH0644990B2 (en) | 1988-10-13 | 1988-10-13 | Manufacturing method of composite fine powder material |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0644990B2 (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7878430B2 (en) | 2006-11-20 | 2011-02-01 | The University Of Western Ontario | Method and apparatus for uniformly dispersing additive particles in fine powders |
HU230862B1 (en) * | 2008-04-28 | 2018-10-29 | DARHOLDING Vagyonkezelő Kft | Device and method for continuous production of nanoparticles |
CN110158051B (en) * | 2018-11-22 | 2020-07-17 | 中国科学院过程工程研究所 | Low-temperature medium-steady flow process for preparing TiOxCyNzSystem and method for coating and composite coating thereof |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR880000618B1 (en) * | 1985-12-28 | 1988-04-18 | 재단법인 한국화학연구소 | Preparation for silicon multy crystal |
JPS63216904A (en) * | 1987-03-04 | 1988-09-09 | Tdk Corp | Magnetic particle and production thereof |
JPS6487771A (en) * | 1987-09-30 | 1989-03-31 | Ishikawajima Harima Heavy Ind | Production of thin si3n4 film by cvd to raw material having large specific surface area |
-
1988
- 1988-10-13 JP JP63258071A patent/JPH0644990B2/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
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JPH02102730A (en) | 1990-04-16 |
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