CN104942300B - Preparation method of hollow or solid spherical metal powder - Google Patents
Preparation method of hollow or solid spherical metal powder Download PDFInfo
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Abstract
A preparation method of hollow or solid spherical metal powder includes the steps that metal powder or alloy powder or pre-mixed powder is mixed or subjected to grain size gradation according to the component proportion; the particle size distribution of the mixed powder or the powder subjected to grain size gradation meets the requirements that D50 is 0.3-3.5 microns, and D90 is smaller than or equal to 5.0 microns; then, the powder, a water-based solvent, adhesion agents, dispersing agents and defoaming agents are mixed in proportion, grinding and dispersing are performed, slurry which is dispersed and evenly mixed is obtained, and the viscosity of the slurry is not larger than 1.5 Pa*s; the slurry is pumped into a spraying dryer to be dried; next, the slurry is transferred to a thermal treatment device and subjected to thermal treatment, and the product is obtained when temperature is lowered to be room temperature through cooling. The preparation method has the advantages that the technological steps are simple, and waste is little.
Description
Technical field
The invention belongs to field of material technology, is related to a kind of method for preparing micron-size spherical metal-powder, more particularly to
A kind of preparation method of hollow or solid spherical metal-powder.
Technical background
Metal-powder is almost applied to all industries of national economy as main industrial raw materials, widely applies
In the field such as machinery, metallurgy, chemical industry, Aero-Space.With modern science development in science and technology, micron and submicron spherical metal-powder
Become transformation and promote paint, thermal spraying, electronic technology, functional material, powder metallurgy, 3D printing and biotechnology etc. new
The basis of emerging industry development；Meanwhile, the also more and more higher of the requirement to metal-powder itself quality, the preparation of metal-powder is towards height
Pure, fine, composition and granularity is controllable and direction of functionalization is developed.At present, the preparation method of solid spherical metal powder is main
There are water, gas atomization, ultrasonic atomizatio and centrifugal atomization.Due to self-technique feature, the metal powder that gas atomization is prepared
Last particle size distribution is wide (20-200um), to realize that less than 50 μm even more thin powder (≤20um) difficulty are very big, fine powder yield
Low, quality is unstable and cost increases.
Spherical hollow metal powder has unique structure, typically exhibits some special light, electricity, magnetic and catalytic performances,
Also begin to show up prominently in fields such as electromagnetism, optics, chemistry, materia medica, biologys.Hollow metal powder has special cavity
Microenvironment, can be used as the carrier of catalyst, it can also be used to chemical microreactor or electrode material；With reference to hollow metal powder
Metal material self-characteristic, can be used as the filtration under harsh ring change border, separation and absorbing material.Such as Rare Metals Materials and work
Journey, 2013,42:2179-2182 reports Ni-Al-Co magnetic metal composite hollow microballons and there is magnetic absorbing and DIELECTRIC ABSORPTION and answers
Cooperation is used, and has preferable absorbing property in low-frequency range；Journal of Inorganic Materials, 2009,27:732-736 have studied cenosphere ferrum
The preparation of oxysome powder body and absorbing property.In addition also studies have reported that, the powder sintered material of hollow metal is used as one
Engineering material is planted, with relatively low heat conductivity and extremely light weight；Ultra-fine hollow magnetic metal dust makes microwave stealth painting
Layer, in the case of equal assimilation effect, density is less, meets the development trend that aircraft industry material lightweight and functionalization are laid equal stress on.
At present, the method for preparing fine hollow metal powder is mainly wet chemistry method, such as sol-gel process, microemulsion method,
Self catalyzed reduction method, solvent-thermal method and template etc., wherein template are main stream approach.Template first prepares template, then
Clad structure is formed on template surface, finally again removes template therein, be just obtained similar with shape of template hollow
Structure.Wet chemistry method general technology link is more, and the granularity and pattern of powder body are difficult to control to, and some metal-powders are not suitable for
Prepare in wet chemistry method, therefore range of application is narrow, and powder body profile is irregular；Additionally, wet method preparation process produces substantial amounts of giving up
Gas, waste water, waste residue etc., are faced with severe environments problem, therefore are unfavorable for industrialized production.
The content of the invention
Above-mentioned deficiency of the present invention for prior art, there is provided a kind of without the need for preparing template in advance, processing step is simple, and
The preparation method of the few hollow or solid spherical metal-powder of Litter.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is：A kind of hollow or solid spherical metal powder
The preparation method of body, step includes：
(1) metal powder or alloyed powder or premixing flour carry out mixture or grain composition by component ratio；Mixture or grain composition
The particle diameter distribution of powder body afterwards meets D50 (meso-position radius or median particle diameter) 0.3-3.5um, D90 and (represents in particle diameter distribution and account for 90%
Corresponding particle diameter)≤5.0um；
(2) it is molten with water base in proportion using step (1) mixture or metal powder or alloy powder after grain composition as raw material
Agent, binding agent, dispersant and defoamer are mixed, and the metal powder or alloy powder after mixture or grain composition is molten with water base
The mass ratio of agent, binding agent, dispersant and defoamer is 1:0.25～1: 0.002～0.08: 0.001～0.005: 0.0001～
0.0003, dispersion is ground with basket type sand mill, planetary mills or wet method Ball-stirring mill, the uniform slurry of dispersion mixing is obtained, starch
Material viscosity is not more than 1.5Pa.s；
(3) the metal-powder slurry after step (2) grinding distribution is pumped in spray dryer by wriggling and is done
Dry, the inlet temperature for adjusting spray dryer is 220～350 DEG C, outlet temperature is 80～130 DEG C, charging rate is 10-
40kg/h, carrier gas is air or noble gases, and gas flow is 180-350Nm3/ h (refers to the volume flow under the status of criterion), i.e.,
Dry mist projection granulating powder can be prepared；
(4) spherical metal powder body obtained in step (3) is transferred in Equipment for Heating Processing, carry out vacuum or inert atmosphere or
Vacuum, inert atmosphere and reducing atmosphere combine the heat treatment of condition；The heating rate of heat treatment is 3-50 DEG C/min, is heated up
It is 300～2000 DEG C to heat treatment temperature, heat treatment time (temperature retention time) 0.5-5h；Then cooled down, cooldown rate is
1-100 DEG C/min, it is cooled to room temperature and obtains product.
Metal powder in above-mentioned steps (1) of the present invention is fine or ultra-fine simple metal powder or alloyed powder or premixed powder, puts down
Particle diameter is not more than 3.5um (micron).
Water-based solvent in above-mentioned steps (2) of the present invention is made up of deionized water with the Organic Alcohol of short carbon chain, short carbon chain
Organic Alcohol can be the mixed alcohol of ethanol or propanol or the two any ratio, deionized water and the mass ratio of Organic Alcohol be 1: 0.3～
1。
Binding agent in above-mentioned steps (2) of the present invention is hybrid adhesive, is made up of polyvinyl alcohol and phenolic resin, poly- second
Enol is 1: 0.2～4 with the mass ratio of phenolic resin.
Dispersant in above-mentioned steps (2) of the present invention is carboxylic acidss and amide analog anion surfactants, or polyalcohols
Neutral surface active agent.
Defoamer in above-mentioned steps (2) of the present invention is n-butyl alcohol.
The solid content that the present invention passes through binder content and metal-powder in set-up procedure (2), optimization spraying in step (3)
Dry technological parameter can prepare hollow or solid spherical metal powder body.
The restriction of D50 and D90 in step (1) of the present invention, is the grain for mixed powder after mixture or granule second wife
Footpath requires；Above-mentioned restriction can reach two effects：One can be to guarantee later stage slurry in the range of certain viscosity, and slurry contains admittedly
Amount is higher to be conducive to solid or hollow-core construction pelletize to control；Two can be to be conducive to controlling pelletizing formation hollow-core construction ---
Just think 50 microns of particle diameter bulky grain can not possibly mist projection granulating into the microns hollow-core construction of particle diameter 50 powder body.
The restriction of step (2) viscosity of the present invention is because exceeding this viscosity, and slurry is difficult to be pumped into atomizing disk；Even if pump
It is sent to atomizing disk and is also unfavorable for mist projection granulating.
Being disposed to of step (3) peristaltic pump of the present invention adapts to the special operation principle of the present invention, will not pollute slurry,
The abrasion of pump is also reduced simultaneously.
Spray dryer in step (3) of the present invention, 12000～22000rpm of atomizing disk rotating speed therein or atomizing pressure
5-50kg/cm2。
The present invention can keep the hollow or solid state of spherical metal powder in step (3), and impurity by heat treatment
Content can be substantially reduced.
Less than 13.3Pa, the noble gases of inert atmosphere are nitrogen, argon to its vacuum of the vacuum of step (4) of the present invention
Gas, helium or the wherein gaseous mixture of both or three；The reducibility gas of reducing atmosphere be hydrogen, methane, carbon monoxide or
The gaseous mixture of acetylene gas and above-mentioned inert atmosphere.
The advantages of the present invention：
1. the present invention passes through adjustment binding agent itself formula and mass ratio in the slurry, by grinding distribution,
Make powder body, binding agent and dispersant uniform, technological parameter is controlled during mist projection granulating can prepare hollow or solid ball-type
Metal powder；
When preparing hollow ball-type metal powder, for the different solid-to-liquid ratio of slurry and binder content, by out temperature
Regulation with atomizing disk rotating speed or atomisation pressure to control spray droplet in solvent evaporation rate so that binding agent can be in liquid
Drop surface forms one layer thin of the organic film for possessing certain elasticity --- both be able to can be allowed again in drop with binding metal powder body
The solvent diffuse in portion to surface speed be slightly larger than or it is in a basic balance in solvent pass through speed of the thin layer from surface evaporation, so as to
Hollow metal-powder is obtained after the completion of whole dry run.Aiding in again can be with other classification techniques such as cyclonic separation, screening
It is prepared on a large scale the hollow metal powder of different size；
When preparing solid ball-type metal powder, the particle diameter distribution of metal-powder can mainly by the rotating speed of regulation centrifugal spray
Or the pressure of press atomization aids in again the spherical gold that can be prepared on a large scale different-grain diameter demand with techniques such as cyclonic separation, screenings
Category powder body.
2. the heat treatment that the present invention passes through the later stage, keeps the architectural characteristic of hollow or solid spherical metal powder, removes bonding
Agent and dispersant, powder purity is improved, and can meet different quality requirements；The preparation method is with super-fine metal powder or alloyed powder
Raw material, can carry out fine regulation to the different component of alloy powder；Hollow or solid metal powder prepared by the invention, both can protect
Hold yardstick from tens to hundreds of micron of powder body characteristic such as good fluidity etc., while can also have the characteristic of superfine powder concurrently, can
To open up the functionalized application of metal-powder.
In sum, what this method can be controllable prepares hollow or solid construction spherical metal powder body, and powder body grain
Degree is suitable, sphericity height, good fluidity, purity are high.Present invention process is practical, and raw material selection extensively, fit by low cost of manufacture
Close batch production and the exploitation of functional metal powder body.
Description of the drawings
The stereoscan photograph of Fig. 1 Ni base hollow metal powder.
The stereoscan photograph of Fig. 2 Ni base solid metal powder.
The stereoscan photograph of Fig. 3 CuMn alloy solid metal powder.
The XRD figure of Fig. 4 CuMn alloy solid metal powder.
Specific embodiment
The present invention is described in further detail below by embodiment, but the present invention is not limited solely to following examples.
Embodiment 1：
(1) the Ni powder with 0.6 micron of mean diameter is as raw material, by Ni powder, water-based solvent, hybrid adhesive and dispersant,
Mix by 1: 0.43: 0.03: 0.002 quality proportioning, be put into basket type sand mill and be ground dispersion 12h, finally add and account for
The n-butyl alcohol of Ni silty amount 0.1 ‰ continues to stir 1h as defoamer, obtains slurry.Wherein, water-based solvent is 1 for mass ratio:
0.5 deionized water and the mixed solution of dehydrated alcohol；It is 1 that binding agent is mass ratio:1 polyvinyl alcohol and phenolic resin it is mixed
Close binding agent.
(2) slurry is spray-dried using drying machine with centrifugal spray, inlet amount 15kg/h, import and export temperature difference
300 DEG C and 129 DEG C are adjusted to, atomizing disk rotating speed 14000rpm is taken away the granule that quality kicks the beam using cyclone separator, is obtained
Hollow ball shape Ni powder.
(3) the hollow dry particle for obtaining is put into into Equipment for Heating Processing, under hydrogen reducing atmosphere, from room temperature 300 is heated to
DEG C, heating rate is 10-15 DEG C/min, and in 300 DEG C of isothermal holding 1h, is subsequently cooled to room temperature, and cooldown rate is 30-40
DEG C/min obtains final hollow Ni powder (Fig. 1), powder body apparent density 1.68g/cm3, C content 380ppm.
Embodiment 2：
(1) the Ni powder with mean diameter 0.6um is as raw material, by Ni powder, water-based solvent, hybrid adhesive and dispersant, by 1
: 0.54: 0.015: 0.002 quality proportioning mixing, it is put into basket type sand mill and is ground dispersion 12h, finally add and account for Ni
The n-butyl alcohol of silty amount 0.1 ‰ continues to stir 1h as defoamer, obtains slurry.Wherein, water-based solvent is that mass ratio is 1: 1
Deionized water and dehydrated alcohol mixed solution；It is 1 that binding agent is mass ratio:1 polyvinyl alcohol and the mixing of phenolic resin
Binding agent.
(2) slurry is spray-dried using drying machine with centrifugal spray, inlet amount 18kg/h, out temperature is adjusted respectively
Whole is 260 DEG C and 103 DEG C, and atomizing disk rotating speed 18500rpm is taken away the too small granule of particle diameter using cyclone separator, obtains reality
Heart spherical Ni powder.
(3) the solid dry particle for obtaining is put into into Equipment for Heating Processing, under hydrogen reducing atmosphere, from room temperature 500 is heated to
DEG C, heating rate is 25-35 DEG C/min, and processes 1h at 500 DEG C, is cooled to room temperature, and cooldown rate is 35-45 DEG C/min, is obtained
To final solid Ni powder (Fig. 2), powder body apparent density 2.06g/cm3, C content 196ppm.
Embodiment 3：
(1) CuMn alloys (the Mn contents 25% or so) powder with mean diameter 1.0um is as raw material, by CuMn alloyed powders, water
Based solvent, hybrid adhesive and dispersant, are mixed by 1: 0.82: 0.01: 0.002 quality proportioning, are put into basket type sand mill and are entered
Row grinding distribution 12h, finally adds the n-butyl alcohol for accounting for Ni silty amount 0.1 ‰ as defoamer, continues to stir 1h, is starched
Material.Wherein, water-based solvent is deionized water and the mixed solution of dehydrated alcohol of the mass ratio for 1: 0.67；Binding agent is mass ratio
For 1:0.8 polyvinyl alcohol and the hybrid adhesive of phenolic resin.
(2) slurry is spray-dried using drying machine with centrifugal spray, inlet amount 18kg/h, out temperature is adjusted respectively
Whole is 300 DEG C and 116 DEG C, and atomizing disk rotating speed 14000rpm is taken away the too small granule of particle diameter using cyclone separator, obtains reality
Bulbus cordis shape CuMn alloy powder.
(3) the solid dry particle for obtaining is put into into Equipment for Heating Processing, under nitrogen atmosphere, from room temperature 700 DEG C is heated to, risen
Warm speed is 35-45 DEG C/min and processes 1h at 700 DEG C, and be cooled to room temperature, cooldown rate obtains final for 45-55 DEG C/min
Solid Ni powder (Fig. 3), powder body apparent density 1.96g/cm3, C content 275ppm.
Fig. 4 for CuMn alloyed powders XRD figure, the point of theory of the corresponding angle of diffraction of diffraction maximum and CuMn25% alloyed powders is very
Good identical explanation forms CuMn alloyed powder Mn elements and is uniformly distributed, and the degree of crystallinity of CuMn alloyed powders is high.
(1) hollow or solid construction judges, is most directly SEM --- such as patent, and the hollow alloy of lithium ion battery is born
The controllable method for preparing (public announcement of a patent application CN 103199226A) of pole material
(2) another Fig. 1 from the present invention, pelletizing has shell parts to split to be formed where shade, and just explanation defines hollow
Structure (Fig. 2 in similar patent CN 103199226A)；Fig. 2-3 ftractures without powder body shell sections, where forming shade,
But by the apparent density (1.68) of final powder body in example 1,1.96 much smaller than 2.06 and the 3 of example 2, absolutely prove attached
Fig. 2-3 is solid powder body.
Claims (7)
1. the preparation method of a kind of hollow or solid spherical metal-powder, it is characterised in that：Step includes：
（1）Metal powder or alloyed powder or premixing flour carry out mixture or grain composition by component ratio；After mixture or grain composition
The particle diameter distribution of powder body meets D50 for 0.3-3.5um, D90≤5.0um；
（2）By step（1）Metal powder or alloy powder after mixture or grain composition as raw material, in proportion with water-based solvent,
Binding agent, dispersant and defoamer are mixed, the metal powder or alloy powder after mixture or grain composition and water-based solvent, viscous
The mass ratio of knot agent, dispersant and defoamer is 1:0.25～1: 0.002～0.08: 0.001～0.005: 0.0001～
0.0003, dispersion is ground with basket type sand mill, planetary mills or wet method Ball-stirring mill, the uniform slurry of dispersion mixing is obtained, starch
Material viscosity is not more than 1.5Pa.s；
（3）By step（2）Metal-powder slurry after grinding distribution is pumped in spray dryer by wriggling and is dried, and is adjusted
The inlet temperature of whole spray dryer is 220～350 DEG C, outlet temperature is 80～130 DEG C, charging rate is 10-40kg/h, is carried
Gas is air or noble gases, and gas flow is 180-350Nm3/ h, you can prepare dry mist projection granulating powder；
（4）By step（3）Obtained spherical metal powder body is transferred in Equipment for Heating Processing, carries out vacuum or inert atmosphere or reduction
Property atmosphere or vacuum, inert atmosphere and reducing atmosphere combine the heat treatment of condition；The heating rate of heat treatment be 3-50 DEG C/
Min, it is 300～2000 DEG C to be warming up to heat treatment temperature, heat treatment time 0.5-5h；Then cooled down, cooldown rate is 1-
100 DEG C/min, it is cooled to room temperature and obtains product.
2. the preparation method of according to claim 1 hollow or solid spherical metal-powder, it is characterised in that：Step（2）
In the mixture that is made up of the mixed alcohol of deionized water and ethanol or propanol or the two any ratio of water-based solvent, deionized water with
The mass ratio of alcohol is 1: 0.3～1.
3. the preparation method of according to claim 1 hollow or solid spherical metal-powder, it is characterised in that：Step（2）
In binding agent be hybrid adhesive, be made up of polyvinyl alcohol and phenolic resin, the mass ratio of polyvinyl alcohol and phenolic resin is 1
: 0.2～4.
4. the preparation method of according to claim 1 hollow or solid spherical metal-powder, it is characterised in that：Step（2）
In dispersant be carboxylic acidss and amide analog anion surfactants, or polyalcohols neutral surface active agent.
5. the preparation method of according to claim 1 hollow or solid spherical metal-powder, it is characterised in that：Step（2）
In defoamer be n-butyl alcohol.
6. the preparation method of according to claim 1 hollow or solid spherical metal-powder, it is characterised in that：Step（3）
In spray dryer, 12000～22000rpm of atomizing disk rotating speed therein or atomizing pressure 5-50kg/cm2。
7. the preparation method of according to claim 1 hollow or solid spherical metal-powder, it is characterised in that：Step（4）
Vacuum its vacuum be less than 13.3Pa, the noble gases of inert atmosphere are nitrogen, argon, helium or wherein both or three
Gaseous mixture；The reducibility gas of reducing atmosphere are that hydrogen, methane, carbon monoxide or acetylene gas are mixed with above-mentioned inert atmosphere
Close gas.
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| CN110893465A (en) * | 2018-08-22 | 2020-03-20 | 西门子股份公司 | 3D printing metal powder, 3D printing method and method for preparing 3D printing metal powder |
| CN109741839A (en) * | 2018-12-24 | 2019-05-10 | 哈尔滨工程大学 | A kind of heat insulating metal and ceramic multilayer hollow sphere and preparation method thereof |
| CN109718779A (en) * | 2018-12-26 | 2019-05-07 | 万华化学集团股份有限公司 | A kind of ball-type skeleton Ni hydrogenation catalyst and its preparation method and application |
| CN110961619A (en) * | 2019-12-23 | 2020-04-07 | 北京科技大学 | Low-cost 3D printing method for titanium product |
| CN113020613B (en) * | 2021-03-12 | 2022-06-03 | 深圳航天科创实业有限公司 | Hollow powder and method for producing same |
| CN114210991B (en) * | 2021-11-30 | 2022-08-19 | 达高工业技术研究院(广州)有限公司 | Spherical silver powder with cavity structure and preparation method thereof |
| CN116422224B (en) * | 2023-04-14 | 2024-03-12 | 北京华圻生态科技有限公司 | Spherical hollow powder and preparation method and application thereof |
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