CN104259469B - The manufacture method of micron and the spherical powder of nano metal - Google Patents
The manufacture method of micron and the spherical powder of nano metal Download PDFInfo
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Abstract
The present invention provides the manufacture method of a kind of micron and the spherical powder of nano metal, and step is as follows：(1) metal dust is prepared；(2) metal dust and carbon material powder or the uniform mixed-powder with ceramic powder are prepared；(3) high annealing makes metal melting and is frozen into metal ball；The temperature of high annealing is the temperature for reaching the metal melting, especially more than metal melting point temperature in the range of 40 to 100 DEG C；(4) remove carbon material powder or ceramic powder obtains micron, the spherical powder of nano metal.The metal of spherical metal powder includes the alloy formed between all elemental metals of gold, silver, copper, aluminium, gallium, tin, zinc, lead, iron, cobalt, nickel, rare earth etc., elemental metals and compound with including the alloy and compound of the metalloids such as boron, silicon, carbon, phosphorus, germanium, nitrogen and nonmetallic formation.
Description
Technical field
The present invention relates to suitable for powder metallurgy, metal 3D printing, spray (pricker) weldering metal dust, lubriation material, solar energy
The manufacture method of the microns such as battery, solid fuel propellant, Electronic Packaging, accurate preparation field and the spherical powder of nano metal.
Background technology
Globular metallic powder can be used for powder metallurgy, 3D metallic prints, spray (pricker) weldering metal dust, lubriation material, the sun
Energy battery, Electronic Packaging, accurate preparation field etc..The preparation method of current existing metal ball shaped particle is in terms of balling-up mechanism
To divide, it can substantially be divided into three classes：Gas atomization and centrifugal atomization are had based on drop injection solidification balling-up；Based on machinery
That shears balling-up has chopping or punching remelting process；Uniform droplet spray and pulse small hole gunite[1]。
Atomization is the industrial method for preparing metallic particles mainly used, can prepare spherical metallic particles, such as
Gas atomization, centrifugal atomization, plasma atomization, water atomization and vacuum atomization etc., wherein using more for aerosol
Change method and the class of centrifugal atomization two.Cardinal principle is by liquid material high-speed gas atomization, crushing, forms fine droplets,
By surface tension in cooling procedure, spherical micro-particle is formed.The production efficiency of atomization is high, and cost is relatively low, but it is produced
Particulate particle size distribution range it is very big, it is necessary to by repeatedly screening can just obtain needed for particle diameter particle, finished product rate is not
Height, and be difficult to prepare the metal dust that size is less than less than 10 μm；In addition, particulate sphericity prepared by atomization is not high
, there is the particle of thermal induction hole in (being often spherical or drop shape particle).In addition, the consumption of inert gas is big, cost compared with
Height, gas reclaiming clean technical difficulty is big.
Chopping or punching remelting process are the material for needing to prepare by the machining such as wire drawing shearing or paillon foil punching press mode
Material is processed into the minute cells of homogeneous quality, then liquid medium of the minute cells input with certain temperature gradient processed
Middle remelting turns into spherical into drop in drop dropping process in the presence of interfacial tension.Chopping or punching remelting process technique can
Control property is good, but its process operation process is various, and is limited to cut line width, and minute cells can not be decreased further, particle diameter without
There is bottleneck with can avoiding.The technique is also subject to processing the limitation of material physical property simultaneously, and such as hard brittle material is difficult to be processed
Into silk or foil, materials with high melting point is difficult to be melted.In addition, the particle that this kind of method is prepared also needs to carry out at degreasing
Reason, this causes the cost of this method to greatly increase.
Liquid droplet ejection method includes uniform droplet spray and pulse small hole gunite.Uniform droplet spray is by liquid
Flowed out from capillary nozzle, periodic disturbance applied to liquid stream by mechanical oscillation, liquid stream is broken and is separated into homogeneous drop,
Drop forms spheric granules under surface tension effects.Pulse small hole gunite is to allow metal to be kept molten by crucible,
Displacement of the same size is produced by piezoelectric ceramics, the displacement acts on liquid, make metal liquid from the aperture of crucible bottom
Spray, form homogeneous drop.Drop forms spheric granules under surface tension effects.The metal spherolite prepared with liquid droplet ejection method
Footpath is consistent, good sphericity.But liquid droplet ejection method low production efficiency, it is high to prepare cost, and be difficult to prepare size be less than 100 μm with
Under metal ball.Therefore, the globular metallic powder that prepared by liquid droplet ejection method, which is difficult to use in, needs a large amount of powder using metal dust
The fields such as last metallurgy, 3D printing, spray (pricker) weldering metal dust, lubriation material.
Present inventor discovery, the high gold of currently acquired sphericity after the manufacture method of current metal ball is furtherd investigate
Belong to the method for ball, two classes can be attributed to；1) by molten drop/gas interface (i.e.：Liquid/gas interface) surface tension make
With obtaining metal ball, such as：Atomization and liquid droplet ejection method；2) by molten drop/oil interface (i.e.：Liquid/liquid interface) interface
Tension force effect, obtains metal ball, such as chopping or punching remelting process.The present invention is proposed by molten drop/carbon material or ceramic material
Expect interface (i.e.：Liquid/solid interface) method prepare micron, nano metal ball.Its principle is by metallic particles carbon material powder
Or separated with ceramic powder, using molten drop carbon material or ceramic material solid interface is nonwetting, indiffusion or
The property spread less, forms spherical in the case where the interfacial tension and liquid gas interface Surface Tension of Liquid Drops of liquid-solid boundary drop are acted on simultaneously
Molten drop, obtains micron and nano metal ball after cooling.
Bibliography：
[1] " progress of homogeneous spherical micro-size particles technology of preparing ", Dong Wei, Li Ying, Fu Yifan, Tan Yi, material
Engineering, 9 (2012) 92-98.
The content of the invention
It is an object of the present invention to provide a kind of manufacture method of spherical metal powder, by by metal and carbon materials feed powder
End is mixed with ceramic powder, metallic particles is separated by carbon material powder or by ceramic powder.Reaching or high
In a certain temperature of melting point metal, molten drop/carbon material or ceramic material interface are formed (i.e.：Liquid/solid interface), utilize gold
Belong to drop carbon material or ceramic material solid interface is nonwetting, indiffusion or the property spread less, in solid liquid interface drop
Interfacial tension and liquid surface tension simultaneously act under, formed spherical metal drop, in cooling procedure obtain micron and
Nano metal ball.
The technical scheme is that：A kind of manufacture method of the spherical powder of micron and nano metal, comprises the following steps：
(1) metal dust is prepared；
(2) metal dust and carbon material powder or the uniform mixed-powder with ceramic powder are prepared；
(3) high annealing makes metal melting and is frozen into metal ball；The temperature of high annealing is to reach the metal melting
Temperature, especially more than metal melting point temperature in the range of 40 to 100 DEG C；
(4) remove carbon material powder or ceramic powder obtains micron, the spherical powder of nano metal.
The metal of spherical metal powder includes all elemental metals (such as：Gold, silver, copper, aluminium, gallium, tin, zinc, lead, iron, cobalt,
Nickel, rare earth etc.), the alloy and compound and elemental metals formed between elemental metals and metalloid and it is nonmetallic (such as：Boron, silicon,
Carbon, phosphorus, germanium, nitrogen etc.) formed alloy and compound.
The step of preparing the raw metal powder includes obtaining elemental metals, alloy and compound by melting, crushes
Into metal dust, or fast quenching is into being broken into metal dust after band；Or gold is obtained by metal oxide or metal salt back
Belong to powder；Or the metal dust obtained by other method.
The raw metal powder size is less than 10mm, and size range preferably is in 50nm~1mm.
Carbon material powder is graphite, graphene, diamond, carbon dust or coal dust and their two or more mixing
Thing, ceramic powder be carbide ceramics, boride ceramics, oxide ceramics or nitride ceramics and they two kinds or two
Plant the mixture of the above.
Prepare metal dust and carbon material powder or the method with the uniform mixed-powder of ceramic powder：1) by metal
The method that powder is mixed with carbon material powder or with ceramic powder, i) takes mechanical means uniformly to mix；Ii) in liquid
Stir mixing in (water, ethanol etc.)；Iii) after by dispersant aid dispersion, with carbon material powder or ceramic powder
Mixing, the uniform mixed-powder of metallic particles for being dried to obtain with carbon material or being coated with ceramic material after mixing；2) it is used to
Upper type mixes metal oxide or metal salt with carbon material powder or with ceramic powder, (such as hydrogen in reducing atmosphere
Gas, ammonia, carbon monoxide etc.) annealing, obtain metal dust and carbon material powder or the uniform mixed powder with ceramic powder
End.
The metal dust and carbon material powder should meet weighed metal powder with the mass ratio of ceramic powder
The total surface area at end is less than the total surface area of matched carbon material powder or ceramic powder；The metal dust and carbon materials
Feed powder end or with the mixed-powder of ceramic powder, the quality of metal dust is in metal/carbon material powder or ceramic material
Shared mass ratio is between 10% to 99.9% in mixture of powders.The carbon material powder or ceramic powder can be appointed
The size for size of anticipating, the scope of 10 nanometer of -100 micron grain size is more preferable.The pattern of carbon material powder or ceramic powder can be with
It is sheet, spherical, wire, tubulose or other shapes.
By well mixed metal/carbon material or ceramic material mixed-powder vacuum or atmosphere (including hydrogen, nitrogen,
Argon gas and ammonia etc.) middle annealing, temperature：The fusing point of metal is reached at or above, temperature preferably is higher than melting point metal 40~100
℃；Soaking time：Ensure that metal is completely melt, the preferably time is 1min~6min, and isothermal treatment for short time overcomes molten drop and carbon materials
Phase counterdiffusion between material or ceramic material, it is ensured that molten drop is in carbon material or the nonwetting property of ceramic material interface；Cooling
Mode：1) rapid cooling, allows metal solid particle to keep the shape of liquid metal ball, meanwhile, alloy material composition macroscopic view can be overcome
Segregation and reduce the diffusion of carbon material or ceramic material under high temperature to metallic particles；2) or rapid cooling combination Slow cooling, it is as cold as soon
Fusing point is once after temperature, then Slow cooling, receives the micron and nano metal ball of better crystallinity degree, even monocrystalline state.
By the carbon material powder or ceramic powder in the metal/carbon material or ceramic material mixed-powder of annealing
Remove, obtain micron and the spherical powder of nano metal.Cleaning method includes：1) in liquid (such as：Water or organic solvent etc.) middle leaching
After bubble, using metal and carbon material or the density contrast big with ceramic material, it is cleaned by ultrasonic, removes carbon material powder or ceramic material
Powder, obtains spherical metal powder；2) after soaking in a liquid, metal is obtained using the method for centrifugation, filtering or externally-applied magnetic field
Spherical powder；3) using shape of the metallic particles with carbon material or with ceramic material, of different sizes, using suitable sieve by two
Person separates.
The diameter of the spherical metal powder is less than 10mm.It is preferred that spherical metal powder diameter 50nm~1mm's
Scope.Beneficial effects of the present invention, metallic particles is separated with carbon material powder or with ceramic powder, molten drop is utilized
Carbon material or ceramic material solid interface is nonwetting, indiffusion or the property spread less, at the interface of liquid-solid boundary drop
Tension force and liquid gas interface Surface Tension of Liquid Drops form spherical metal drop act on simultaneously under, and micron and nano metal are obtained after cooling
Ball.According to the present invention, the clear principle of metal ball is prepared, the process for manufacturing spherical metal powder is simple, and manufacturing cost is low,
Production efficiency is high, is a kind of manufacturer simple and easy to apply, environment-friendly, be produced on a large scale micron and the spherical powder of nano metal
Method.The metal bulb diameter of manufacture is less than 10mm, and preferably metal bulb diameter is in 50nm~1mm (especially models of 2-200 micron grain sizes
Enclose more preferably) scope.The sphericity of metal ball is high, and surface quality is good, and no gross segregation, microscopic structure uniformity is good, Ke Yiman
Foot powder metallurgy, metal 3D printing, spray (pricker) weldering metal dust, lubriation material, solar cell, solid fuel propellant,
The extensive use in the field such as Electronic Packaging, precision system be standby.
Brief description of the drawings
The electron scanning micrograph for the micron ping-pong ball that Fig. 1 is obtained by the manufacture method of the present invention；
The electron scanning micrograph for the micron copper ball that Fig. 2 is obtained by the manufacture method of the present invention；
The electron scanning micrograph for the micron aluminium ball that Fig. 3 is obtained by the manufacture method of the present invention；
The electron scanning micrograph for the micron signal bronze ball that Fig. 4 is obtained by the manufacture method of the present invention；
The SEM for the micron iron silicon boron glassy metal ball that Fig. 5 is obtained by the manufacture method of the present invention is shone
Piece.
Embodiment
As described above, the application is separated by metallic particles with carbon material powder or with ceramic powder, molten metal is utilized
Drop in carbon material or ceramic material solid interface is nonwetting, indiffusion or the property spread less, on the boundary of liquid-solid boundary drop
Face tension force and liquid gas interface Surface Tension of Liquid Drops form spherical metal drop act on simultaneously under, and micron is obtained after cooling and nanometer is solid
Body metal ball.Hereinafter, to the present invention micron and the manufacture method of the spherical powder of nano metal is described in detail.
The present invention is first by the metal dust for the required size for preparing or buying.Prepare metal dust：1) to brittle metal
It can be obtained by the method for melting, Mechanical Crushing；2) to there is the metal of excellent toughness to obtain early stage strip by fast quenching,
Again by subsequently grinding broken acquisition metal dust；3) metal powder is prepared by the method for metal oxide or metal salt back
End.In addition to preparing metal dust, the metal dust of size needed for can also obtaining by other means.
Metal dust is uniformly mixed with the carbon material powder or ceramic powder of appropriate size and quantity, to reach use
Carbon material powder or the purpose that metallic particles is separated with ceramic powder.Prepare metal dust and carbon material powder or with ceramics
The method of the uniform mixed-powder of material powder has：1) mixed by metal dust with carbon material powder or with ceramic powder
Method, i) takes mechanical means uniformly to mix；Ii) stir mixing in liquid (water, ethanol etc.)；Iii dispersant) is passed through
After aid dispersion, mixed with carbon material powder or ceramic powder, be dried to obtain after mixing with carbon material or use ceramic material
The uniform mixed-powder of the metallic particles of cladding；2) to upper type by metal oxide or metal salt and carbon material powder or
Mixed with ceramic powder, (such as hydrogen, ammonia, carbon monoxide) anneals in reducing atmosphere, obtains metal dust and carbon
Material powder or the uniform mixed-powder with ceramic powder.
By well mixed metal/carbon material or ceramic material mixed-powder vacuum or atmosphere (including hydrogen, nitrogen,
Argon gas and ammonia etc.) middle annealing, temperature：The fusing point of metal is reached at or above, temperature preferably is higher than melting point metal 40~100
℃；Soaking time：Ensure that metal is completely melt, the preferably time is 1min~6min.Isothermal treatment for short time can overcome molten drop with
Phase counterdiffusion between carbon material or ceramic material, it is ensured that molten drop is in carbon material or the nonwetting property of ceramic material interface；
The type of cooling：1) rapid cooling, allows metal solid particle to keep the shape of liquid metal ball, meanwhile, alloy material composition can be overcome
Gross segregation and reduce the diffusion of carbon material or ceramic material under high temperature to metallic particles.2) rapid cooling combination Slow cooling, rapid cooling
To after fusing point once temperature, then Slow cooling, the micron and nano metal ball of better crystallinity degree, even monocrystalline state can be received.
By the carbon material powder or ceramic powder in the metal/carbon material or ceramic material mixed-powder of annealing
Remove, obtain micron and the spherical powder of nano metal.Cleaning method includes：1) in liquid (such as：Water or organic solvent etc.) middle leaching
After bubble, using metal and carbon material or the density contrast big with ceramic material, carbon material powder or ceramics are removed in repeated ultrasonic cleaning
Material powder, obtains spherical metal powder；2) after soaking in a liquid, obtained using the method for centrifugation, filtering or externally-applied magnetic field
Spherical metal powder；3) using shape of the metallic particles with carbon material or with ceramic material, of different sizes, suitable sieve is used
The two is separated.
In addition, the manufacture method of the spherical metal powder of the present invention is best suited for the metal ball shaped of a diameter of 50nm~1mm
Powder.In the case where diameter is more than 1mm, after being melted, the drop of spheroidizing is due to the Action of Gravity Field of itself, sphericity
It can be deteriorated, be difficult to obtain the high metal ball of sphericity in cooling procedure, therefore, the diameter of spherical metal powder is preferably in 1mm
Below.On the other hand, although particle size is smaller, it is easier to obtain the high particle of sphericity, but tiny metal dust and carbon materials
When feed powder end or ceramic powder mixing, it is not easy uniformly to be divided by carbon material powder or ceramic powder due to reuniting
Open, and after annealing, remove metal ball and carbon material or with carbon material powder in ceramic material mixed-powder or ceramic material powder
The difficulty at end becomes big, thus spherical metal powder diameter preferably in more than 50nm.
Embodiment 1
The preparation of silver micron ball, first, a variety of average-sizes of purchase are 10 μm or so of the argent powder (shape of particle
Shape is the shape of laminar or other corner angle) as raw material.1 gram of silver powder and the flaky graphite powder that size is 1 μm or so are taken, is pressed
Weight ratio is 1:1 proportioning, mechanical agitation methods (including using the method such as ball milling or rod milling mix also can) uniform mixing.
The silver/graphite powder mixed is put into alumina crucible, crucible puts the unheated zone of annealing furnace into, is evacuated down to
6×10-3Pa, 1050 DEG C are heated to by annealing furnace heating zone, are pushed into the crucible equipped with silver/graphite powder to 1050 DEG C of heating zone,
After insulation 5 minutes, the crucible that will be equipped with silver/graphite powder pulls out heating zone rapid cooling.
Be soaked in water silver/graphite mixed powder, and silver micron ball is obtained by being cleaned by ultrasonic.Fig. 1 is outside obtained silver micron ball
The electron scanning micrograph of sight, spherical particle size is at 5 μm -20 μm.According to the manufacturer of spherical metal powder of the present invention
Method, as shown in figure 1, confirming that silver micron metal ball can be obtained.Weight ratio is 3:1 proportioning obtains equifinality.
Embodiment 2
The preparation of copper micron ball, first, purchase size are used as raw material for 3 μm -10 μm or so of metallic copper powder.Take 1 gram
Copper powder and the Graphene powder that size is 10nm-1 μm or so, are 5 by weight:1 proportioning, mechanical agitation methods are uniformly mixed.
The copper mixed/graphene mixed-powder is put into alumina crucible, crucible puts the unheated zone of annealing furnace into,
It is evacuated down to 6 × 10-3Pa, is heated to 1150 DEG C, crucible of the push-in equipped with copper/graphene mixed-powder is arrived by annealing furnace heating zone
1150 DEG C of heating zone, after being incubated 5 minutes, the crucible that will be equipped with copper/graphene mixed-powder pulls out heating zone cooling.
Be soaked in water copper/graphene mixed powder, and copper micron ball is obtained by being cleaned by ultrasonic.Fig. 3 is obtained copper micron ball
The electron scanning micrograph of outward appearance, spherical particle size is at 3 μm -12 μm.According to the system of the spherical metal powder of the present invention
Method is made, as shown in Fig. 2 confirming that copper micron metal ball can be obtained.
Embodiment 3
The preparation of aluminium micron ball, first, purchase average-size are used as raw material for 5 μm or so of metallic aluminium powder.Take 1 gram of aluminium
Powder and the flaky graphite powder that size is 400nm or so, are 1 by weight:2 proportionings, the uniform mixing of ultrasound in alcoholic solution.
Metallic aluminium/graphite mixed-powder is obtained after drying.
The aluminium mixed/graphite mixed-powder is put into quartz ampoule, quartz ampoule is evacuated down to 6 × 10-3Pa, leads to argon gas
Tube sealing after to 0.06MPa, will be equipped with the quartz ampoule of aluminium/graphite mixed-powder protected with argon gas, puts into and is heated to 740 DEG C and moves back
In stove, 6 minutes are incubated, takes out in the outer air of stove and cools down.
With alcohol-pickled aluminium/graphite mixed-powder, aluminium micron spherical powder is obtained by being cleaned by ultrasonic.Fig. 3 is obtained
The electron scanning micrograph of aluminium ball outward appearance, spherical particle size is at 5 μm -30 μm.According to the spherical metal powder of the present invention
Manufacture method, as shown in figure 3, confirm can obtain aluminium micron metal ball.
Embodiment 4
The preparation of signal bronze micron ball, first, signal bronze (Cu is obtained by method of smelting60Sn40, subscript is weight
Percentage), it is 10 μm or so of powder as raw material that Mechanical Crushing signal bronze, which obtains average-size,.Take 1 gram of signal bronze powder
It is 5 by weight with the Graphene powder that size is 10nm-1 μm or so:After 1 proportioning, mechanical agitation, uniform mixing.
The signal bronze mixed/graphene mixed powder is put into alumina crucible, crucible is put the non-of annealing furnace into and added
Hot-zone, is evacuated down to 6 × 10-3Pa, 800 DEG C, earthenware of the push-in equipped with signal bronze/Graphene powder are heated to by annealing furnace heating zone
Crucible is to 800 DEG C of heating zone, and after being incubated 5 minutes, the crucible that will be equipped with signal bronze/Graphene powder pulls out heating zone cooling.
Be soaked in water signal bronze/graphene mixed powder, and signal bronze micron ball shape powder is obtained by being cleaned by ultrasonic.Figure
4 be the electron scanning micrograph of obtained signal bronze ball outward appearance, and spherical particle size is at 5 μm -20 μm.According to the present invention
Spherical metal powder manufacture method, as shown in figure 4, confirm can obtain signal bronze micron ball.
Embodiment 5
The preparation of iron silicon boron glassy metal micron ball, first, melting obtain iron silicon boron alloy (Fe78Si9B13), then, machine
It is 20 μm or so of powder as raw material that tool, which crushes iron silicon boron alloy and obtains average-size,.Take 1 gram of iron silicon boron alloy powder and size
It is 1 by weight for 1 μm or so of flaky graphite powder:1 proportioning, mechanical agitation is uniformly mixed.
The iron silicon boron alloy/graphite mixed powder mixed is put into in quartz ampoule, quartz ampoule is evacuated down to 6 × 10-3Pa,
Logical argon gas will be equipped with the quartz ampoule of iron silicon boron alloy/graphite mixed powder protected with argon gas to tube sealing after 0.06MPa, puts into and adds
Heat is incubated 5 minutes, will be equipped with the quartz of iron silicon boron alloy/graphite mixed powder protected with argon gas into 1220 DEG C of annealing furnace
Pipe is quenched into water, realizes quick cooling.
With alcohol-pickled iron silicon boron alloy/graphite powder, iron silicon boron metal is obtained with reference to magnetism separate method by being cleaned by ultrasonic
Glass micron ball.Fig. 5 is the electron scanning micrograph of obtained iron silicon boron glassy metal ball outward appearance, and spherical particle size exists
10μm-60μm.According to the manufacture method of the spherical metal powder of the present invention, as shown in figure 5, confirming that iron silicon boron metal can be obtained
Glass micron ball.
Above example can also use pulverized coal preparation, can obtain same result.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for those skilled in the art
For member, within the spirit and principles of the invention, any modification, improvement for being made etc. all should be included in the guarantor of the present invention
Within the scope of shield.
Claims (5)
1. the manufacture method of a kind of micron and the spherical powder of nano metal, it is characterised in that comprise the following steps：
（1）Prepare metal dust；
（2）Metal dust and carbon material powder directly mix or added the uniform batch mixing of partially liq with ceramic powder；
（3）High annealing makes metal melting and is frozen into metal ball；The temperature of high annealing is to reach the metal melting point temperature
More than degree in the range of 40 DEG C；
（4）Remove carbon material powder or ceramic powder obtains micron, the spherical powder of nano metal；
The metal of spherical metal powder includes gold, silver, copper, aluminium, gallium, tin, zinc, lead, iron, cobalt, nickel, all elemental golds of rare earth
Category, the alloy formed between elemental metals and compound and elemental metals with including boron, silicon, carbon, phosphorus, germanium, the metalloid of nitrogen and
The alloy and compound of nonmetallic formation；
Preparing the metal dust includes：1）Elemental metals, alloy and compound are obtained by melting, metal dust is broken into,
2）Fast quenching is into being broken into metal dust after band；3）Metal dust is obtained by metal oxide reduction；
Carbon material powder is graphite, graphene, diamond, carbon dust or coal dust and their more than two kinds mixtures, ceramic material
Feed powder end is carbide ceramics, boride ceramics, oxide ceramics or nitride ceramics and their more than two kinds mixtures；
Metal dust and carbon material powder or the mixed method of ceramic powder：1）Mechanical means is taken uniformly to mix；2）
Stir mixing in the liquid of water or ethanol；3）After dispersant aid dispersion, with carbon material powder or ceramic material powder
End mixing, is dried to obtain after mixing with carbon material or the uniform mixed-powder with ceramic material coating metal particles；With the above
Mode is by the mixing of metal dust and carbon material powder or ceramic powder；Moved back in hydrogen, ammonia or CO reducing atmosphere
Fire, obtains metal dust and carbon material powder or the uniform mixed-powder with ceramic powder.
2. the manufacture method of spherical metal powder according to claim 1, it is characterised in that：The metal dust size model
It is trapped among the mm of 50 nm~1.
3. the manufacture method of the spherical metal powder according to any one of claim 1-2, it is characterised in that：
The metal dust should be met with carbon material powder or with the mass ratio of ceramic powder：Weighed metal dust
Total surface area is less than the total surface area of matched carbon material powder or ceramic powder；The metal dust and carbon materials feed powder
End or with the mixed-powder of ceramic powder, the carbon material powder or ceramic powder are 10nm-100 microns, carbon
Material powder or be piece shape with the pattern of ceramic powder, it is spherical, linear or tubular.
4. the manufacture method of the spherical metal powder according to any one of claim 1-2, it is characterised in that：It will mix equal
Even metal and carbon material or ceramic material mixed-powder vacuum or hydrogen, nitrogen, argon, ammonia ambient anneal, temperature：Higher than metal
Fusing point with up to 40oIn the range of C；Soaking time：Ensure that metal is completely melt, take the min of 1 min- 6；Isothermal treatment for short time overcomes
Phase counterdiffusion between molten drop and carbon material or ceramic material, it is ensured that molten drop is in carbon material or ceramic material interface
Nonwetting property；
The type of cooling：1）Rapid cooling, allows metal solid particle to keep the shape of liquid metal ball, meanwhile, overcome alloy material composition
Gross segregation and reduce the diffusion of carbon material or ceramic material under high temperature to metallic particles；2）Or rapid cooling combination Slow cooling, soon
It is as cold as after fusing point temperature below, then Slow cooling, receives the micron and nano metal ball of better crystallinity degree, even monocrystalline state.
5. the manufacture method of the spherical metal powder according to any one of claim 1-2, it is characterised in that：
Carbon material powder in the metal/carbon material or ceramic material mixed-powder of annealing or ceramic powder are cleaned
Remove, obtain micron and the spherical powder of nano metal；Cleaning method includes：1）After being soaked in the liquid of water or organic solvent,
Using metal and carbon material or the density contrast big with ceramic material, carbon material powder or ceramic material are removed in repeated ultrasonic cleaning
Powder, obtains spherical metal powder；2）After soaking in a liquid, metal is obtained using the method for centrifugation, filtering or externally-applied magnetic field
Spherical powder；3）It is shape using metallic particles with carbon material or with ceramic material, of different sizes, using suitable sieve by two
Person separates.
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| CN1243124C (en) * | 2004-06-10 | 2006-02-22 | 复旦大学 | Preparing method for medium hole noble metal hollow microscapsule |
| CN101559938B (en) * | 2008-04-18 | 2011-05-11 | 中国科学院大连化学物理研究所 | Preparation method of high-graphitized nanometer carbon material |
| CN103447542B (en) * | 2013-05-27 | 2015-10-07 | 上海大学 | A kind of preparation method of micron order iron-based hollow ball material and device thereof |
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