CN109570513A - A kind of preparation method of porous metal powder - Google Patents
A kind of preparation method of porous metal powder Download PDFInfo
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- CN109570513A CN109570513A CN201910034414.9A CN201910034414A CN109570513A CN 109570513 A CN109570513 A CN 109570513A CN 201910034414 A CN201910034414 A CN 201910034414A CN 109570513 A CN109570513 A CN 109570513A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 78
- 239000002184 metal Substances 0.000 title claims abstract description 74
- 239000000843 powder Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 84
- 239000004917 carbon fiber Substances 0.000 claims abstract description 84
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 84
- 238000000498 ball milling Methods 0.000 claims abstract description 36
- 238000000713 high-energy ball milling Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 47
- 238000000137 annealing Methods 0.000 abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 28
- 229910052799 carbon Inorganic materials 0.000 abstract description 23
- 239000000463 material Substances 0.000 abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 11
- 239000001257 hydrogen Substances 0.000 abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 11
- 150000002739 metals Chemical class 0.000 abstract description 11
- 238000003860 storage Methods 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000013528 metallic particle Substances 0.000 abstract description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003780 insertion Methods 0.000 abstract description 3
- 230000037431 insertion Effects 0.000 abstract description 3
- 229910052744 lithium Inorganic materials 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 3
- 239000012188 paraffin wax Substances 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 14
- 238000002791 soaking Methods 0.000 description 14
- 238000012545 processing Methods 0.000 description 13
- 239000002994 raw material Substances 0.000 description 13
- 230000008030 elimination Effects 0.000 description 12
- 238000003379 elimination reaction Methods 0.000 description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 239000007769 metal material Substances 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000004513 sizing Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000002923 metal particle Substances 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000012224 working solution Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 238000010316 high energy milling Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910000048 titanium hydride Inorganic materials 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910000568 zirconium hydride Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B22F1/0007—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The present invention relates to a kind of preparation methods of porous metal powder, belong to technology of metal powder field.Preparation method are as follows: first pass through and short carbon fiber is subjected to degumming process; the short carbon fiber of degumming process and metal powder are obtained into the metal powder of ultra-fine carbon particle insertion by ball-milling technology appropriate again; annealing removal carbon particle is carried out in oxygen-containing air later; it finally restores and anneals in atmosphere or protective atmosphere or vacuum, obtain hole uniformly and high-purity porous metals powder of high degree of dispersion.In porous metal powder prepared by the present invention, the size adjustable of metallic particles, controlled porosity, pore-size is 1~3 μm.Prepared material shows good oil storage, hydrogen storage, storage paraffin, storage lithium performance, and preparation process is simple, at low cost.
Description
Technical field
The present invention relates to a kind of preparation methods of porous metal powder, belong to technology of metal powder field.
Background technique
Porous metal material is a kind of new metallic material containing a large amount of holes for being connected to or being closed in matrix.Together
Compact metal is compared, and porous metals have good compressibility, and Poisson's ratio can change in deformation process；Same polymer
Foam is compared, and has high rigidity and high use temperature, while will not be dissolved by an organic solvent；Compared with foamed ceramics,
With good toughness, heat transfer property and electric conductivity.Since it is with excellent performance, auto industry, aerospace,
The fields such as environment protection field, building have broad prospects.
The preparation process of porous metal material mainly includes liquid metal solidification method, solid metallic sintering process and metal deposit
Method three categories.Wherein foam melt method utilizes metal hydride, such as TiH2Or ZrH2Molten metal is added to Deng as foaming agent
In, by heating so that foaming agent decomposition releases gas, cooling melting liquid stream can make gas be sealed in metal inside shape
At porous metals.This method applies in general to the metal material of the low melting points such as aluminium, magnesium, and simple process, cost is relatively low, sample obtained
Product porosity is high, but Air Bubble Size and the hole uniformity are difficult to control.Prepare metal particle size, porosity size and aperture ruler
The preparation method of very little controllable porous metals powder is current technical problem.
108232160 A of Chinese invention patent CN discloses porous metals-carbon of a kind of high metal content, high degree of dispersion
The preparation method of composite material.It allows the compound MX of metal target to carry out mechanical ball mill with the carbide of active metal A to react, A
Carbide be both reducing agent and carbon source.In this way, MX locally produces carbon when being reduced into metal, to realize metallic particles
It is compound with the high degree of dispersion of carbon material, and the content of metal is measured by the chemical reaction than determining.It is porous prepared by the present invention
In composite material, the size adjustable of metallic particles, controlled porosity.Prepared material shows good storage sodium, storage lithium
Energy.
102274975 A of Chinese invention patent CN discloses a kind of method for preparing metal micro-nano hollow spherical powder, master
Wanting content is: tool-electrode and piece pole remain gap needed for spark discharge and are accordingly immersed in working solution, connect arteries and veins
Rush power supply and melt tool-electrode and piece pole spark discharge, gasification, at the same during spark discharge to tool-electrode with
Working solution between piece pole implements ultrasonic frequency vibration, and the working solution in gap is made to generate microbubble, tool-electrode and workpiece
Electrode melting, gasification metal material adventitious deposit on microbubble surface, form metal micro-nano hollow sphere.Using of the invention
Metal micro-nano hollow sphere powder made from method, the hollow degree of hollow sphere is high, and particle diameter distribution is between 20nm to 100 μm, wall
Thickness is not more than 1 μm, and hollow sphere ratio is high.The insufficient place of the preparation method is that complex process, production efficiency is low, production cost
High, template is not easy removal completely and easily causes environmental pollution.
A kind of method that Chinese invention patent CN105506336 A discloses high-temperature oxydation and reduction prepares porous metals,
The present invention relates to a kind of preparation methods of porous metals, that is, one, cleaning metal material；Two, it will be held under the protection of inert gas
Carrier is warming up to 100~850 DEG C, is exposed to metal material in oxidizing gas and carries out oxidation processes；Three, oxic gas is drained
Body is warming up to 300~850 DEG C, oxidizes metal object and is exposed in reducing gas and carries out reduction treatment, in the protection of inert gas
Porous metals are obtained after lower cooling.It is more that the present invention directly forms micron order in metal surface and inside using oxidation and reducing gas
Pore structure, preparation process is simple, and can realize secondary operation on the complicated metal material device prepared.But the party
The pore size that method obtains is too small (micron order), and needs the diffusion and richness spontaneous on the surface of material and internal generation by oxygen
Collection ultimately forms porous metal structure, and the diffusion and enrichment of oxygen are difficult to control, therefore the size and uniformity of the porosity of metal
It is difficult to control.
So far, it yet there are no the related note that porous metal powder is prepared using high-energy ball milling cooperation oxidationreduction processing
It carries.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of preparation method of porous metal powder,
The simple process solves the problems, such as that metal particle size, porosity size and aperture size are controllable with low cost, prepared
Material show good oil storage, hydrogen storage, storage paraffin, storage lithium performance, and preparation process is simple, at low cost.
Degumming short carbon fiber and metal powder are carried out high energy ball by a kind of preparation method of porous metal powder of the present invention
Mill first carries out first time heat treatment under oxidizing atmosphere, carries out second of heat treatment under nonoxidizing atmosphere then to get porous
Metal powder.
The preparation process of the degumming short carbon fiber are as follows: by short carbon fiber beam under protective atmosphere, in 650~800 DEG C
It is heat-treated 20~90min to obtain the final product.Carbon fiber surface cladding solidification organic colloid layer, removes on carbon fiber surface after degumming process
Agent is starched, the roughness of carbon fiber surface is increased, so that subsequent ball milling processing can release " constraint/limitation " of sizing agent, and is gone
Except the impurity and active function groups of carbon fiber surface, the percentage of damage of short carbon fiber is improved.
The protective atmosphere is inert atmosphere or vacuum, such as nitrogen, argon gas.
The short carbon fiber beam diameter is 6~8 μm, 1~4mm of length.
Staple fiber is too long, and winding is easy when ball milling and is reunited, too short, not only improves cost, but also separating difficulty is bigger.
Preferably, the volume ratio of the degumming short carbon fiber and metal powder be 1~9:19~1, further it is excellent
It is selected as 1~4:9~1, is still more preferably 1~4:4~1.
In the metal powder, metallic element is zeroth order, and the metallic element is in Cu, Ti, Fe, Co, Ni, Mo, Ag
It is at least one.
Preferably, the mode of the high-energy ball milling is planetary ball mill or vibratory milling.
Preferably, in the high-energy ball milling gross mass and abrading-ball of degumming short carbon fiber and metal powder quality
Than for 1:5~8.
The high-energy ball milling revolving speed is 220~350r/min, and the time is at least 6h.
The condition of the first time heat treatment: 250~400 DEG C of temperature.Time determines (its purpose according to carbon degree for the treatment of
Be to force inlay and/or through metal-powder carbon complete oxidation).Generally 10~60min.Time cannot be too long, too long
It can make metal powder complete oxidation, once complete oxidation, is easy for rupturing；During transfer and storage, edge will lead to
The rupture in hole direction.
The nonoxidizing atmosphere is reducing atmosphere, inert atmosphere or vacuum.
The condition of second of the heat treatment: temperature is 0.3~0.65 times of melting point metal.Time is according to the demand of product
It adjusts, generally 10~60min.The purpose of second of heat treatment is to realize the reduction of the metal powder of partial oxidation.
A kind of preparation method of porous metal powder of the present invention is adjusted by adjusting additional amount and the rotational speed of ball-mill of carbon fiber
Metal particle size, porosity and aperture size are saved, porosity is up to 90%.
A kind of preparation method of porous metal powder of the present invention；The short carbon fiber is degumming process short carbon fiber.Market
Upper existing carbon fiber surface cladding solidification organic colloid layer, it is necessary to by degumming process, to remove carbon fiber surface sizing agent,
Increase the roughness of carbon fiber surface, so that subsequent (grinding) processing can release " constraint/limitation " of sizing agent, and eliminates
The impurity of carbon fiber surface, otherwise percentage of damage is very low.In the present invention, the length of strict control raw material short carbon fiber and it is necessary for
Product after degumming process can be very good to realize its object is to cooperate rotational speed of ball-mill and mill ball and proportion of the invention
The control of the fine of carbon fiber and being uniformly embedded into metallic particles and metal particle size, in conjunction with going after ball milling
Carbon and deoxidized annealing processing, can obtain porous metal powder.
The designed aperture with the porous metal powder of preparation of the invention corresponds to the size of ultra-fine carbon particle, only 1~3 μ
M, and be evenly distributed.
The present invention attempts for the first time, and the short carbon fiber prepared using degumming process technique passes through the height of appropriate ball milling parameter
Energy ball milling, carbon elimination and deoxidized annealing technique prepare porous metal powder.
Principle and advantage:
(1) short carbon fiber is selected.Since there are a large amount of active function groups for carbon fiber surface, directly with long carbon fiber
It is crushed, it is easy to reunite between fiber, it can not be crushed, therefore select short carbon fiber, can avoid this problem.
(2) for the processing method of short carbon fiber.Degumming tech is used first, this is because commercially available carbon fiber surface bread
Cover solidification colloid layer, it is necessary to by degumming process, to remove carbon fiber surface sizing agent, so that subsequent (grinding) processing can solve
Except " constraint/limitation " of sizing agent, and the impurity and active function groups of carbon fiber surface are eliminated using degumming tech, otherwise broken
Broken rate is very low.Secondly ball-milling technology is selected, the optimization of rotational speed of ball-mill and mill ball and proportion can be very good to realize carbon fiber
Fine.Last carbon elimination and deoxidized annealing technique obtains for removing the metal powder of carbon fiber particles and reduction-oxidation
The higher porous metal powder of purity.
By the short carbon fiber 250r/min of 700 DEG C of degumming process and metal powder high-energy ball milling method, moved back in conjunction with 300 DEG C of air
The porous metal powder pattern of -350 DEG C hydrogen annealing processing preparations of fire is as shown in Figure 2.
As shown in Figure 2, suitable high-energy-milling and subsequent carbon elimination-deoxidation impurity elimination is combined to anneal using degumming process
Technique, obtains aperture and porosity is controllable, and the uniform porous metal powder of hole.
In short, the present invention has preparation process simple (only degumming, ball milling, carbon elimination-deoxidation impurity elimination annealing), at low cost
Honest and clean, gained porous metal powder function admirable and uniformly, have good market prospects.
Detailed description of the invention
Attached drawing 1 is the preparation flow figure of porous metal powder provided by the invention；
Attached drawing 2 is the short carbon fiber and metal powder 250r/min high energy ball of 700 DEG C of degumming process prepared by the present invention
Mill method, in conjunction with the powder SEM pattern of -350 DEG C of hydrogen annealing processing preparations of 300 DEG C of air anneals.
As can be seen from Figure 1 the preparation flow for the porous metal powder that the present invention designs, specifically: it first passes through short carbon
Fiber carries out degumming process, then the short carbon fiber of degumming process and metal powder are obtained ultra-fine carbon by ball-milling technology appropriate
The metal powder of particle insertion carries out annealing removal carbon particle in oxygen-containing air later, and finally hydrogen reducing obtains again
Hole uniformly and high degree of dispersion porous metals powder.
As shown in Figure 2, degumming process combines suitable high-energy-milling and carbon elimination-deoxidation impurity elimination annealing process, obtains
Aperture be about 1~3 μm, hole equally distributed porous metal powder.
Specific embodiment
Below with reference to attached drawing of the invention, technical solution of the present invention is clearly and completely described, it is clear that retouched
The embodiment stated is only a part of the embodiment in technical solution recorded in the present invention, instead of all the embodiments.It is based on
The embodiment of the present invention, every other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, protection scope of the present invention is belonged to.
Comparative example 1
The electrolytic copper powder that this comparative example 1 uses partial size to be 120 μm for 120 μm of flaky graphite and partial size is ball milling original
Material, natural flake graphite volume percentage 20%, electrolytic copper powder are added volume percentage 80%, the two are added to ball milling
High-energy ball milling, revolving speed 250r/min, Ball-milling Time 6h, ratio of grinding media to material 5:1 are carried out in equipment.The spontaneous group of natural flake graphite
It is poly-, do not occur broken.After the duplicate subsequent processing of embodiment 1, porous metal powder is not obtained.
Comparative example 2
The electrolytic copper powder that this comparative example 2 uses partial size to be 120 μm for 120 μm of granular graphite and partial size is ball milling original
Material, granular graphite volume percentage 20%, electrolytic copper powder are added volume percentage 80%, the two are added to ball milling and is set
Standby middle carry out high-energy ball milling, revolving speed 250r/min, Ball-milling Time 6h, ratio of grinding media to material 5:1.It is broken granular graphite part
It is broken, and and be not apparent from insertion copper powder.After the duplicate subsequent processing of embodiment 1, porous metal powder is not obtained.
Comparative example 3
This comparative example 3 use it is commercially available, without any pretreated short carbon fiber and partial size be for 120 μm of electrolytic copper powder
Volume percentage 80% is added in ball milling raw material, carbon fiber volume percentage 20%, electrolytic copper powder, and the diameter of short carbon fiber is
8 μm, the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 250r/min, Ball-milling Time 6h, ball
Material is than being 5:1.Short carbon fiber is simultaneously unbroken, is sticked at ball milling tank skin.After the duplicate subsequent processing of embodiment 1, not
To porous metal powder.
Comparative example 4
It for 120 μm of electrolytic copper powder is ball that this comparative example 4, which uses commercially available, 1000 DEG C of degumming process short carbon fiber and partial size,
Raw material, short carbon fiber volume percentage 20% are ground, volume percentage 80% is added in electrolytic nickel powder, and the diameter of short carbon fiber is
8 μm, the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 250r/min, Ball-milling Time 6h, ball
Material is than being 5:1.Short carbon fiber is simultaneously not apparent from broken.After the duplicate subsequent processing of embodiment 1, porous metals powder is not obtained
End.
Comparative example 5
It for 120 μm of electrolytic copper powder is ball that this comparative example 5, which uses commercially available, 700 DEG C of degumming process short carbon fiber and partial size,
Raw material, short carbon fiber volume percentage 20% are ground, volume percentage 80% is added in electrolytic nickel powder, and the diameter of short carbon fiber is
12 μm, the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 250r/min, Ball-milling Time 6h,
Ratio of grinding media to material is 5:1.Short carbon fiber is simultaneously not apparent from broken, after the duplicate subsequent processing of embodiment 1, does not obtain porous metals
Powder.
Comparative example 6
It for 120 μm of electrolytic nickel powder is ball that this comparative example 6, which uses commercially available, 700 DEG C of degumming process short carbon fiber and partial size,
Raw material, short carbon fiber volume percentage 20% are ground, volume percentage 80% is added in electrolytic nickel powder, and short carbon fiber diameter is 6 μ
The two is added in ball-grinding machine and carries out high-energy ball milling by m, length 2mm, revolving speed 600r/min, Ball-milling Time 6h, ball material
Than for 6:1.Short carbon fiber and be not apparent from it is broken, majority deposition ball grinder top covers at.
Comparative example 7
It for 120 μm of electrolytic nickel powder is ball that this comparative example 7, which uses commercially available, 700 DEG C of degumming process short carbon fiber and partial size,
Raw material, short carbon fiber volume percentage 20% are ground, volume percentage 80% is added in electrolytic nickel powder, and the diameter of short carbon fiber is
6 μm, the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 100r/min, Ball-milling Time 6h, ball
Material is than being 6:1.Short carbon fiber is simultaneously not apparent from broken, after the duplicate subsequent processing of embodiment 1, does not obtain porous metals powder
End.
Embodiment 1
The present embodiment 1 uses commercially available, 700 DEG C of degumming process 60min short carbon fiber and partial size for 120 μm of electrolytic copper powder
For ball milling raw material, short carbon fiber volume percentage 10%, electrolytic copper powder is added volume percentage 90%, short carbon fiber it is straight
Diameter is 6 μm, and the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 250r/min, and Ball-milling Time is
6h, ratio of grinding media to material 6:1, carbon elimination of annealing in air later, annealing temperature are 300 DEG C, soaking time 20min, then in hydrogen
Deoxidation in atmosphere, annealing temperature are 350 DEG C, soaking time 30min, obtain Porous Cu powder oporosity and reach 9%.
Embodiment 2
The present embodiment 2 uses commercially available, 750 DEG C of degumming process 60min short carbon fiber and partial size for 120 μm of electrolytic nickel powder
For ball milling raw material, short carbon fiber volume percentage 25%, electrolytic nickel powder is added volume percentage 75%, short carbon fiber it is straight
Diameter is 6 μm, and the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 280r/min, and Ball-milling Time is
7h, ratio of grinding media to material 6:1, carbon elimination of annealing in air later, annealing temperature are 300 DEG C, soaking time 30min, then in hydrogen
It anneals in atmosphere, annealing temperature is 500 DEG C, soaking time 20min, obtains porous nickel powder oporosity and reaches 22%.
Embodiment 3
The present embodiment 3 uses commercially available, 800 DEG C of degumming process 60min short carbon fiber and partial size for 150 μm of reduced iron powder
For ball milling raw material, short carbon fiber volume percentage 40%, reduced iron powder is added volume percentage 60%, short carbon fiber it is straight
Diameter is 6 μm, and the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 300r/min, and Ball-milling Time is
8h, ratio of grinding media to material 6:1, carbon elimination of annealing in air later, annealing temperature are 300 DEG C, soaking time 20min, then in hydrogen
Deoxidation in atmosphere, annealing temperature are 500 DEG C, soaking time 30min, obtain porous iron powder oporosity and reach 38%.
Embodiment 4
The present embodiment 4 uses commercially available, 750 DEG C of degumming process 60min short carbon fiber and partial size for 50 μm of sized spherical titanium powder
For ball milling raw material, short carbon fiber volume percentage 55%, sized spherical titanium powder is added volume percentage 45%, short carbon fiber it is straight
Diameter is 7 μm, and the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 250r/min, and Ball-milling Time is
10h, ratio of grinding media to material 7:1, carbon elimination of annealing in air later, annealing temperature are 300 DEG C, soaking time 20min, then in hydrogen
Deoxidation in atmosphere, annealing temperature are 600 DEG C, soaking time 30min, obtain POROUS TITANIUM powder oporosity and reach 50%.
Embodiment 5
The present embodiment 5 uses commercially available, 800 DEG C of degumming process 60min short carbon fiber and partial size for 180 μm of ball shape silver powder
For ball milling raw material, short carbon fiber volume percentage 65%, ball shape silver powder is added volume percentage 35%, short carbon fiber it is straight
Diameter is 8 μm, and the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 280r/min, and Ball-milling Time is
8h, ratio of grinding media to material 6:1, carbon elimination of annealing in air later, annealing temperature are 280 DEG C, soaking time 20min, then in vacuum
Middle deoxidation, annealing temperature are 300 DEG C, soaking time 10min, obtain porous aluminum powder end porosity and reach 60%.
Embodiment 6
The present embodiment 6 uses commercially available, 750 DEG C of degumming process 60min short carbon fiber and partial size for 150 μm of spherical cobalt powder
For ball milling raw material, short carbon fiber volume percentage 80%, spherical cobalt powder is added volume percentage 20%, short carbon fiber it is straight
Diameter is 8 μm, and the two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 280r/min, and Ball-milling Time is
8h, ratio of grinding media to material 6:1, carbon elimination of annealing in air later, annealing temperature are 300 DEG C, soaking time 20min, then in hydrogen
Deoxidation in atmosphere, annealing temperature are 500 DEG C, soaking time 20min, obtain porous cobalt dust porosity and reach 75%.
Embodiment 7
It for 200 μm of molybdenum powder is ball that the present embodiment 7, which uses commercially available, 750 DEG C of degumming process 60min short carbon fiber and partial size,
Raw material, short carbon fiber volume percentage 90% are ground, volume percentage 10% is added in molybdenum powder, and the diameter of short carbon fiber is 8 μm,
The two is added in ball-grinding machine and carries out high-energy ball milling by length 2mm, revolving speed 280r/min, Ball-milling Time 10h, ball material
Than for 6:1, carbon elimination of annealing in air later, annealing temperature is 320 DEG C, soaking time 20min, then takes off in hydrogen atmosphere
Oxygen, annealing temperature are 950 DEG C, soaking time 60min, obtain porous molybdenum powder porosity and reach 89%.
Claims (10)
1. a kind of preparation method of porous metal powder, it is characterised in that: degumming short carbon fiber and metal powder are carried out high energy
Ball milling first carries out first time heat treatment under oxidizing atmosphere, carries out second of heat treatment under nonoxidizing atmosphere then to get more
Mesoporous metal powder.
2. preparation method according to claim 1, it is characterised in that；The preparation process of the degumming short carbon fiber are as follows: will
Short carbon fiber beam is under inert atmosphere or vacuum condition, in 650~800 DEG C of 20~90min of heat treatment to obtain the final product.
3. preparation method according to claim 2, it is characterised in that: the short carbon fiber beam diameter is 6~8 μm, length 1
~4mm.
4. preparation method according to claim 1, it is characterised in that: the volume of the degumming short carbon fiber and metal powder
Than for 1~9:19~1.
5. preparation method according to claim 1, it is characterised in that: in the metal powder, metallic element is zeroth order, described
Metallic element is selected from least one of Cu, Ti, Fe, Co, Ni, Mo, Ag.
6. preparation method according to claim 1, it is characterised in that: the mode of the high-energy ball milling is planetary ball mill or vibration
Dynamic ball milling.
7. preparation method according to claim 1, it is characterised in that: degumming short carbon fiber and metal in the high-energy ball milling
The gross mass of powder and the mass ratio of abrading-ball are 1:5~8.
8. preparation method according to claim 1, it is characterised in that: the high-energy ball milling revolving speed is 220~350r/min,
Time is at least 6h.
9. preparation method according to claim 1, it is characterised in that: the condition of the first time heat treatment: temperature 250~
400℃。
10. preparation method according to claim 1, it is characterised in that:
The nonoxidizing atmosphere is reducing atmosphere, inert atmosphere or vacuum；
The condition of second of the heat treatment: temperature is 0.3~0.65 times of melting point metal, 10~60min of time.
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