CN100413618C - Apparatus for gas-phase synthesis of super-fine metal powder - Google Patents
Apparatus for gas-phase synthesis of super-fine metal powder Download PDFInfo
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- CN100413618C CN100413618C CNB2006100354887A CN200610035488A CN100413618C CN 100413618 C CN100413618 C CN 100413618C CN B2006100354887 A CNB2006100354887 A CN B2006100354887A CN 200610035488 A CN200610035488 A CN 200610035488A CN 100413618 C CN100413618 C CN 100413618C
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- metal powder
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- fine metal
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Abstract
The present invention discloses a gas phase synthesizing device for ultrafine metal powder, which comprises a reactant precursor supply system, a chemical gas phase reaction region, a heating device and a powder collecting and tail gas treating system, wherein spatial domain limiters which divide the reaction region into a plurality of reaction intervals are fixed in the chemical gas phase reaction region. The device is capable of limiting the four stages of chemical reaction, nucleation, primary particle growth and collosion and coagulation among particles generated in the process of chemical gas phase particle preparation in a large number of tiny intervals in the spatial domain limiters, has a regional limiting function to the flow directions of air streams, avoids the disadvantages of large possibility of mutual collision in the process of forming the particles, the particulate agglomeration of final products, wide size distribution, etc. due to the flow disturbance of the air streams, and is favorable for forming high performance ultrafine particles with narrow and dispersive particle size distribution.
Description
Technical field
The present invention relates to a kind of device for preparing super-fine metal powder, be specifically related to a kind of apparatus for gas-phase synthesis of super-fine metal powder.
Background technology
New material is one of the most active field of world today's development in science and technology, and little, nano material is occupied extremely important status in current field of new, and important component part little, that nano-powder is super-fine material.Little, nano material has special performances because its particle is small, in fields such as powder metallurgy, fine chemistry industry, electronic material and devices wide application prospect is arranged.The method little, nano-powder of preparation mainly contains liquid phase method and vapor phase method at present.And the chemical gaseous phase reducing process is one of preparation method who wherein is fit to industrialized production, be applicable to the various materials of preparation, the purity requirement of raw material is not high, do not need vacuum condition, and have chemical characteristic, obtain high-purity product easily, and collect easily, average grain diameter and granule-morphology are regulated by formation condition easily, thereby can produce in a large number with lower cost.
Chemical gaseous phase prepares particle and mainly comprises four steps: chemical reaction, nucleation, primary granule grow up (surface reaction and epitaxial growth) and particle coalescence, coalescent.In whole process, first three step is finished at short notice, and during the late stages of developmet, and particle coalescence, coalescent ability play a decisive role to the size of particle, structure and morphology etc.And the mobility status of air-flow all played an important role to each stage in the particle building-up process in the reaction zone.
The extra-fine nickel powder (U.S.PatentNO.5,853,451) that the multi-layer ceramic capacitance electrode that people such as Hiroyuki Ishikawa use the hydrogen reducing nickel chloride to prepare 0.2-3um in 1004 ℃ of-1453 ℃ of scopes is used.Kenichi Otsuka and Henry L also use similar method to prepare spherical super fine copper powder and superfine iron powder (U.S.Patent NO.4,810,285, U.S.Patent NO.2,663,633).
Use chemical vapor process to prepare in the equipment of particle at present, the restriction that reaction zone in the equipment does not play local to the flow direction and the scope of air-flow, the air current flow disorder of reaction zone, intergranular collision probability strengthens, thereby the particle size of end product becomes big, reunite easily, Size Distribution is wide, is unfavorable for preparing the granule that particle size is average, disperse.
Summary of the invention
The apparatus for gas-phase synthesis that the purpose of this invention is to provide a kind of super-fine metal powder, this device can play the local restriction to the air current flow of reaction zone, reduces the particle collision, helps forming particle size distribution high-performance ultra-fine grain narrow, that comparatively disperse.
Purpose of the present invention is achieved through the following technical solutions:
The apparatus for gas-phase synthesis of super-fine metal powder of the present invention, comprise reactant presoma supply system, chemical gas phase reaction district, firing equipment and powder collection and exhaust treatment system, in the chemical gas phase reaction district, be fixed with the space confinement device that this reaction zone is separated into a plurality of reaction intervals.
Described space confinement device can be by a plurality of tube banks of axially forming with the axial equidirectional or acutangulate pipeline of reaction zone.The internal diameter of described arbitrary pipeline is 0.05mm～3.0mm, and interior cross sectional shape is circle or regular polygon; The length of tube bank can be shorter than, is longer than or equals burner hearth heating region length.
Described space confinement device also can be a plurality of axial and axial equidirectional or acutangulate laminates that are fixed in parallel to each other in the reaction zone of reaction zone.Distance between adjacent laminate is 0.05mm～3.0mm.
Described space confinement device can be made by quartz glass, aluminium, copper, molybdenum, tungsten, high temperature alloy or ceramic material.
As a kind of improvement, described space confinement device adopts resistant to elevated temperatures material, is fixed in the reaction zone as support as molybdenum, tungsten, fire-resistant cotton etc.
The heating of described reaction zone can with but be not limited to resistance heated, light heating, high-frequency induction heating or plasma heating etc.
Described reactant presoma supply system comprises carrier gas device that transports metal chloride steam and the device that transports reducing gas, stream oriented device crosses in the front, porch of space confinement device, and enter in the space confinement reaction zone and carry out metal reduction reaction, the metal-powder that back formation is finished in reaction enters powder collector.
Synthesizer of the present invention is like this work: the reactant presoma is a metal chloride, as nickel chloride, iron chloride, cobalt chloride etc., metal chloride evaporation back by carrier gas (as Ar gas, N
2Gas, Ar gas and Cl
2Oxygen mixture or N
2Gas and Cl
2Oxygen mixture) send space confinement device inlet front side to by carrier gas device, reducing gas is (as H simultaneously
2, NH
3Or its both mist etc.) device through transporting reducing gas enters space confinement device inlet front side, and above-mentioned metal chloride steam is prepared super-fine metal powder with after reducing gas fully mixes thereby add thermal response in space confinement device.
Device of the present invention can allow chemical gaseous phase prepare the chemical reaction that takes place in the particle process, nucleation, primary granule is grown up between (surface reaction and epitaxial growth) and the particle in collision and coalescent four-stage be limited between Microcells a large amount of in the space confinement device, the flow direction of air-flow is played the restriction of local, collision probability is big mutually in the particle forming process owing to the air current flow disorder causes to have avoided traditional chemical gas-phase reaction district, the particle agglomeration of end product, shortcomings such as Size Distribution is wide, it is narrow to help forming particle size distribution, the high-performance ultra-fine grain of Fen Saning comparatively.
Description of drawings
Fig. 1 is the structural representation of a kind of embodiment of apparatus for gas-phase synthesis of the present invention.
Fig. 2 is the structural representation of the another kind of embodiment of apparatus for gas-phase synthesis of the present invention.
Fig. 3 is the cross sectional representation of a kind of embodiment of space confinement device.
Fig. 4 is the cross sectional representation of the another kind of embodiment of space confinement device.
The specific embodiment
Embodiment one:
As Fig. 1, shown in Figure 3, the device that this chemical gas-phase method prepares superfine powder comprises reactant presoma supply system 1, chemical gas phase reaction district 2, firing equipment 3 and exhaust treatment system 4, in chemical gas phase reaction district 2, place a space confinement device 5 that constitutes by bundle of capillary tubes, this bundle of capillary tubes use exotic material such as molybdenum, tungsten, fire-resistant cotton etc. are positioned in the reaction zone 2 as support casing 8, and this bundle of capillary tubes is coaxial with reaction zone, and bundle of capillary tubes is formed by the tight binding of many capillaries.Material capillaceous can select for use quartz ampoule, aluminum pipe, copper pipe, steel pipe, high temperature alloy pipes and other ceramic materials (as Al
2O
3, ZrO
2Deng).The internal diameter of arbitrary capillary is 0.05mm～3.0mm, and its length can be shorter than, is longer than or equals burner hearth heating region length.
Reactant presoma nickel chloride is evaporated the back and is sent to the front side of conversion zone space confinement device 5 by carrier gas Ar by a carrier gas device 6, simultaneously reducing gas H
2Through the front side that another device 7 enters conversion zone space confinement device 5, both fully mix herein.When temperature in 950 ℃～1200 ℃ scope, the velocity ratio of nickel chloride steam and argon gas is 1.43%～2.95%, hydrogen flowing quantity is 0.2～1m
3During/h, after fully reacting, nickel chloride steam and reducing gas prepare the class spherical super fine nickel powder of average grain diameter at 50nm～1um.
Embodiment two:
Use the used device of embodiment one, after presoma iron chloride is evaporated, sent to conversion zone space confinement device front side by a device, simultaneously reducing gas H by carrier gas Ar
2Enter conversion zone space confinement device front side through another device.When temperature in 600 ℃～900 ℃ scope, H
2Throughput and Ar throughput ratio are in 1～2.6 scope time, prepare the class spherical super fine iron powder of average grain diameter at 100nm～1.6um after iron chloride steam and reducing gas fully react.
Embodiment three:
Use the used device of embodiment one, reactant presoma nickel chloride is evaporated the back by Ar gas and Cl
2The mist of gas is sent conversion zone space confinement device front side to by a device, simultaneously reducing gas H
2Enter conversion zone space confinement device front side through another device.When temperature in 900 ℃～1100 ℃ scope, H
2Throughput and Cl
2Throughput ratio is 3.6～7.4 o'clock, nickel chloride steam and Cl
2After fully reacting, gas, reducing gas prepare the class spherical super fine nickel powder of average grain diameter at 130nm～560nm.
Embodiment four:
Embodiment five:
As shown in Figure 2, adopt vertical apparatus for gas-phase synthesis among this embodiment.In the reaction zone, the confinement reactor 5 that constitutes by bundle of capillary tubes on end.All the other are with embodiment one.
Certainly, cross section capillaceous can also be other shapes such as square, regular hexagon.
Claims (9)
1. the apparatus for gas-phase synthesis of a super-fine metal powder, comprise reactant presoma supply system, chemical gas phase reaction district, firing equipment and powder collection and exhaust treatment system, it is characterized in that: in described chemical gas phase reaction district, be fixed with the space confinement device that this reaction zone is separated into a plurality of reaction intervals.
2. the apparatus for gas-phase synthesis of super-fine metal powder according to claim 1 is characterized in that: described space confinement device is by a plurality of tube banks of axially forming with the axial equidirectional or acutangulate pipeline of reaction zone.
3. the apparatus for gas-phase synthesis of super-fine metal powder according to claim 2, it is characterized in that: the internal diameter of described arbitrary pipeline is 0.05mm～3.0mm, interior cross sectional shape is circle or regular polygon.
4. the apparatus for gas-phase synthesis of super-fine metal powder according to claim 1 is characterized in that: described space confinement device axially is made up of with the axial equidirectional or acutangulate laminate that is fixed in parallel to each other in the reaction zone of reaction zone a plurality of.
5. the apparatus for gas-phase synthesis of super-fine metal powder according to claim 4, it is characterized in that: the distance in the described space confinement device between adjacent laminate is 0.05mm～3.0mm.
6. the apparatus for gas-phase synthesis of super-fine metal powder according to claim 1, it is characterized in that: described space confinement device is made by quartz glass, aluminium, copper, molybdenum, tungsten, high temperature alloy or ceramic material.
7. the apparatus for gas-phase synthesis of super-fine metal powder according to claim 1 is characterized in that: the mode of heating of described reaction zone is resistance heated, light heating, high-frequency induction heating or plasma heating.
8. the apparatus for gas-phase synthesis of super-fine metal powder according to claim 1, it is characterized in that: described reactant presoma supply system comprises carrier gas device that transports metal chloride steam and the device that transports reducing gas, stream oriented device crosses in the front, porch of space confinement device, and enter in the space confinement reaction zone and carry out metal reduction reaction, the metal-powder that back formation is finished in reaction enters powder collector.
9. the apparatus for gas-phase synthesis of super-fine metal powder according to claim 1 is used for Ni, Fe, the preparation of Co or Cu metallic particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100354887A CN100413618C (en) | 2006-05-16 | 2006-05-16 | Apparatus for gas-phase synthesis of super-fine metal powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100354887A CN100413618C (en) | 2006-05-16 | 2006-05-16 | Apparatus for gas-phase synthesis of super-fine metal powder |
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| Publication Number | Publication Date |
|---|---|
| CN1843669A CN1843669A (en) | 2006-10-11 |
| CN100413618C true CN100413618C (en) | 2008-08-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100354887A Expired - Fee Related CN100413618C (en) | 2006-05-16 | 2006-05-16 | Apparatus for gas-phase synthesis of super-fine metal powder |
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| CN107362757A (en) * | 2017-08-25 | 2017-11-21 | 江西艾德纳米科技有限公司 | It is a kind of prepare metal salt continuously generate reaction unit and preparation method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5853451A (en) * | 1990-06-12 | 1998-12-29 | Kawasaki Steel Corporation | Ultrafine spherical nickel powder for use as an electrode of laminated ceramic capacitors |
| CN1275103A (en) * | 1998-06-12 | 2000-11-29 | 东邦钛株式会社 | Method for producing metal powder |
| JP2001089804A (en) * | 1999-09-20 | 2001-04-03 | Toho Titanium Co Ltd | Method of fabricating metal powder |
| CN1537029A (en) * | 2001-05-07 | 2004-10-13 | 环球油品公司 | Apparatus for mixing and reacting at least tow fluids |
| WO2004096420A1 (en) * | 2003-04-28 | 2004-11-11 | Indigo Technologies Group Pty Ltd | Method and apparatus for mixing fluids for particle agglomeration |
-
2006
- 2006-05-16 CN CNB2006100354887A patent/CN100413618C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5853451A (en) * | 1990-06-12 | 1998-12-29 | Kawasaki Steel Corporation | Ultrafine spherical nickel powder for use as an electrode of laminated ceramic capacitors |
| CN1275103A (en) * | 1998-06-12 | 2000-11-29 | 东邦钛株式会社 | Method for producing metal powder |
| JP2001089804A (en) * | 1999-09-20 | 2001-04-03 | Toho Titanium Co Ltd | Method of fabricating metal powder |
| CN1537029A (en) * | 2001-05-07 | 2004-10-13 | 环球油品公司 | Apparatus for mixing and reacting at least tow fluids |
| WO2004096420A1 (en) * | 2003-04-28 | 2004-11-11 | Indigo Technologies Group Pty Ltd | Method and apparatus for mixing fluids for particle agglomeration |
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