CN101721921A - Preparation method of porous metal film - Google Patents
Preparation method of porous metal film Download PDFInfo
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- CN101721921A CN101721921A CN200910264172A CN200910264172A CN101721921A CN 101721921 A CN101721921 A CN 101721921A CN 200910264172 A CN200910264172 A CN 200910264172A CN 200910264172 A CN200910264172 A CN 200910264172A CN 101721921 A CN101721921 A CN 101721921A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 69
- 239000002184 metal Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 30
- 238000000576 coating method Methods 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000000945 filler Substances 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 239000011148 porous material Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000006259 organic additive Substances 0.000 claims abstract description 8
- 239000000428 dust Substances 0.000 claims description 26
- 229910001220 stainless steel Inorganic materials 0.000 claims description 22
- 239000010935 stainless steel Substances 0.000 claims description 22
- 238000005245 sintering Methods 0.000 claims description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 239000005416 organic matter Substances 0.000 claims description 9
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 239000005446 dissolved organic matter Substances 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 239000003082 abrasive agent Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000011247 coating layer Substances 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 239000012047 saturated solution Substances 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims 1
- 239000000155 melt Substances 0.000 claims 1
- 230000007704 transition Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000012528 membrane Substances 0.000 description 12
- 239000010410 layer Substances 0.000 description 7
- 238000001914 filtration Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
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- 230000000694 effects Effects 0.000 description 2
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- 239000008246 gaseous mixture Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000005088 metallography Methods 0.000 description 2
- 238000001471 micro-filtration Methods 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- -1 pottery Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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Abstract
The invention relates to a preparation method of a porous metal film. The surface pores of the porous metal substrate are plugged by using a filling agent, then a metal powder coating is carried out, the filling agent and organic additives in the coating are removed through heat treatment, and finally the metal powder coating is sintered at high temperature to obtain the metal film. The method can directly prepare the metal film on the macroporous base material without a transition layer, and effectively avoids the blockage of metal powder to the pore canal of the base material. The method has the advantages of simple production process, uniform film layer and low mass transfer resistance.
Description
Technical field
The present invention relates to a kind of preparation method of porous metal film, promptly by directly preparing metal film at enterprising row metal powder coating of macropore metal base and sintering.
Background technology
Porous metals especially porous stainless steel are important filtering materials, but owing to mutual restriction between the performance parameters such as its filtering accuracy, mechanical strength and filtration resistance, the use of common porous metals filter material is very limited.For example, improving filtering accuracy then needs to reduce the aperture, but this will certainly increase resistance to mass tranfer; Reduce filter material thickness and can reduce resistance to mass tranfer, but can reduce mechanical strength.Effectively solution is the metal film that forms bore diameter gradient.Specifically, promptly provide mechanical strength with wide-aperture porous metals as supporter, area load one deck micropore metal is controlled the aperture, has so not only guaranteed filtering accuracy and mechanical strength but also has reduced resistance to mass tranfer.Except that as the filtering material, porous metal film can also be used as the carrier of various functional materials such as pottery, molecular sieve, biomaterial, polymer, metal.For example be used to prepare the composite palladium film [Yu Jian, Hu Xiaojuan, Huang Yan. the pottery on porous stainless steel surface is modified and the hydrogen permeating palladium membrane of institute's load. chemical progress .2008,20 (7-8): 1208-1215.].
Porous metal film is generally by metal dust coating preparation, and coating layer thickness is tens to the hundreds of micron.But when directly on the macropore metal base, carrying out coating, metal dust can enter and stop up the duct of base material, so not only can increase resistance to mass tranfer but also can cause holiday, therefore, between rete and base material, also need one or more layers to have the transition zone in different apertures.Business-like porous stainless steel micro-filtration membrane often has this gradient aperture structure.On the one hand, increasing transition zone not only needs to increase coating operation, also needs corresponding increase sintering circuit, thereby has increased production cost; On the other hand, increase the increase that transition zone also means resistance to mass tranfer.Application number is that 200510033633.3 the disclosed a kind of metal film preparation method of Chinese patent is that metal dust with different-grain diameter is made into suspension and places mould, make the tubulose base substrate by centrifugal casting, with blank sintering, the particle diameter of metal dust reduces from outside to inside gradually along tube wall at last.This method has been avoided repeatedly the problem of coating and sintering, but during the disposable sintering of metallic particles that particle diameter is differed greatly, because the suitable sintering condition of metal dust depends on particle size separately, therefore attends to one thing and lose sight of another unavoidably when selecting sintering condition.
Summary of the invention
The objective of the invention is to provide a kind of preparation method of porous metal film in order to improve the problem that is faced in the existing porous metal film production process; This technological operation is more simple, promptly can be directly on the macropore metal base the flawless metal micro-filtration membrane of preparation and need not transition zone.
Technical scheme of the present invention is: a kind of preparation method of porous metal film, it is characterized in that earlier the filler shutoff of the surface holes of porous metal substrate, carry out the metal dust coating at substrate surface then, remove organic additive in filler and the coating by heat treatment, at last metal dust coating and base material are carried out sintering and promptly get metal film.
The average pore size of described porous metal substrate surface holes is generally 10～500 μ m.Filler is that filler is fusible change into liquid organic matter or dissolved organic matter.The preferred fusible organic matter that changes into liquid state is solid paraffin or stearic acid; Preferred dissolved organic matter is preferably carboxymethyl cellulose (CMC), methylcellulose (MC), polyvinyl alcohol (PVA) or polyvinyl butyral (PVB), and organic matter quality concentration is 10～80% of its saturated solution.With the filler heat fused or use dissolution with solvents, make it infiltrate the porous substrate duct, treat condensation or drying after, filler solidifies and the surface holes of shutoff base material.Adopting fusiblely when changing into liquid organic matter shutoff surface holes, is will base material to immerse in the organic matter of fusing to take out condensation behind 1～10min; When adopting dissolved organic matter shutoff surface holes, be that base material is immersed 1～5min in the organic solution, take out drying, repeat this operation 2～10 times.If handle and directly carry out coating operation on the macropore metal base without filler, then the metal dust slurry can be inhaled under the effect of capillary force in the base material duct, causes the duct to stop up.The art of this patent not only can prevent this problem, but also help to improve the quality of metal dust coating, because base material becomes smooth, fine and close with surface after the filler preliminary treatment, in fact the coating operation of this moment is equivalent to eliminate the adverse effect that substrate surface hole and roughness are brought fine and close and coating is carried out on smooth surface.
Carry out before the metal dust coating, must adopt abrasive material that base material is polished, the substrate surface metal is exposed and directly contact with metal dust, abrasive material is preferably 400～1000 purpose sand paper.Coating is preferably stainless steel powder, nickel powder or silver powder with metal dust; Coating is generally 0.1～25 μ m with the metal dust granularity.The metal dust coating can adopt conventional dip coating, spread coating, spraying process, sedimentation etc., and coating layer thickness generally is preferably 20～200 μ m.After coating is finished; filler is removed by the mode of heat treatment (as thermal decomposition, volatilization or distillation) together with the organic additive in the metal dust coating; heat treatment process is carried out in air or protective atmosphere (preferably as N2, Ar or gaseous mixture); treatment temperature is 200～500 ℃; heating rate is 0.5～2 ℃/min, and temperature retention time is 0.5～5h.Heating rate in the heat treatment process should not be too fast, destroys the metal dust coating to prevent organic too quick decomposition or volatilization, also will avoid vibrating base material in heat treatment process, with protective finish and prevent that metal dust from falling into the matrix duct.Heat treatment is removed after filler and the various organic additive, generally adopts original position to carry out high temperature sintering, make the metal dust coating form metal film and with the base material strong bonded; Sintering process needs vacuum or protective atmosphere (as H
2, N
2, Ar or gaseous mixture), concrete sintering temperature depends on the kind and the particle diameter of metal dust.
Beneficial effect:
Compare with the metal film of conventional gradient aperture structure, the technology of the present invention need not transition zone and can directly make metal film at the macropore substrate surface, and not only production technology is simple, and even film layer, resistance to mass tranfer are low.
Description of drawings
Fig. 1 porous stainless steel membrane surface SEM photo.
Fig. 2 porous stainless steel membrane section metallography microscope photo.
Specific embodiments
Embodiment 1
(1) base material is the porous stainless steel disk, diameter 3cm, thick 0.2cm, the average pore size 200 μ m of surface holes.Selected filler is a solid paraffin.
(2) with 2min in the melted paraffin of 80 ℃ of porous stainless steel substrate immersions, take out cooling,, remove the unnecessary paraffin in surface with 400 order sand paperings.
(3) be that the SS-310L stainless steel powder of 3 μ m mixes with polyvinyl alcohol (PVA) solution of 50ml 3% (mass percentage concentration) and strong agitation forms slip with the 10g average grain diameter, slip evenly is sprayed at substrate surface, dry naturally.
(4) base substrate speed with 1 ℃/min under argon gas atmosphere is heated to 400 ℃, insulation 1h is to remove various organic additives.Then under vacuum condition, be warming up to 1050 ℃ with the speed of 5 ℃/min, insulation 1.5h can make the porous stainless steel membrane.
(5) its surperficial SEM microphoto as shown in Figure 1, visible porous stainless steel membrane surfacing, even aperture distribution, defective are few; Its section metallography microscope photo as shown in Figure 2, the visible thick about 120 μ m of rete, film thickness distribution is even, does not see that powder of stainless steel stops up the base material duct.In bigger base material aperture, powder of stainless steel is the mode continuous film forming to build bridge successfully.The average pore size that adopts the bubble platen press to record stainless steel membrane is 0.2 μ m.
Embodiment 2
(1) selected base material is a porous stainless steel, internal diameter 0.8cm, and external diameter 1.3cm, long 10cm, the average pore size of surface holes is 200 μ m.Filler is a solid paraffin.
(2) with the step (2) of embodiment 1.
(3) be that particle diameter mixes with polyvinyl alcohol (PVA) solution of 50ml 3% (mass percentage concentration) and strong agitation formation slip at the SS-316L stainless steel powder of 10～25 μ m with the 50g average grain diameter, slip is evenly brushed in substrate surface, dry naturally.
(4) base substrate speed with 1 ℃/min under air atmosphere is heated to 300 ℃, insulation 1h is to remove various organic additives.Then under vacuum condition, be warming up to 1200 ℃ with the speed of 5 ℃/min, insulation 1.5h can make the porous stainless steel membrane.
(5) the about 100 μ m of the thicknesses of layers of gained stainless steel membrane, it is 3.6 μ m that the bubble platen press records its average pore size.
Embodiment 3
(1) selected base material is the porous-metal nickel pipe, internal diameter 0.9cm, and external diameter 1.3cm, long 10cm, the average pore size of surface holes is 50 μ m.Filler is a stearic acid.
(2) with 2min in the fusing stearic acid of 80 ℃ of nickel porous pipe immersions, take out cooling,, remove the unnecessary stearic acid in surface with 1000 order sand paperings.
(3) with step (3), (4) of embodiment 1.
(4) the about 50 μ m of the thicknesses of layers of gained stainless steel membrane, it is 0.4 μ m that the bubble platen press records its average pore size.
Embodiment 4
(1) with the step (1) of embodiment 2.
(2) with the step (2) of embodiment 1.
(3) with the step (3) of embodiment 1, be the metal nickel powder of 3 μ m but metal dust is an average grain diameter.
(4) base substrate speed with 0.5 ℃/min under argon gas atmosphere is heated to 300 ℃, insulation 5h is to remove various organic additives.Then under vacuum condition, be warming up to 700 ℃ with the speed of 2 ℃/min, insulation 1.5h can make the nickel porous film.
(5) the about 20 μ m of the thicknesses of layers of gained metallic nickel film, it is 0.1 μ m that the bubble platen press records its average pore size.
Embodiment 5
(1) with step (1), (2) of embodiment 1.
(2) with the step (3) of embodiment 1, be the silver powder of 5 μ m but metal dust is an average grain diameter.
(3) with the step (4) of embodiment 1.But last sintering temperature is 600 ℃.
(4) the about 50 μ m of the thicknesses of layers of gained metal silverskin, it is 0.2 μ m that the bubble platen press records its average pore size.
Embodiment 6
(1) with the step (1) of embodiment 1, but filler is polyvinyl butyral (PVB).
(2) the porous stainless steel substrate is immersed 2min in the ethanolic solution of polyvinyl butyral (PVB) of 3wt%,
Naturally dry, repeat this operation 3 times, adopt 1000 order sand paperings, remove the unnecessary polyvinyl butyral in surface.
(3) with step (3), (4) of embodiment 1.
(4) the about 100 μ m of the thicknesses of layers of gained stainless steel membrane, it is 0.5 μ m that the bubble platen press records its average pore size.
Claims (8)
1. the preparation method of a porous metal film, it is characterized in that earlier the filler shutoff of the surface holes of porous metal substrate, carry out the metal dust coating at substrate surface then, remove organic additive in filler and the coating by heat treatment, at last metal dust coating and base material are carried out sintering and promptly get metal film.
2. in accordance with the method for claim 1, the average pore size that it is characterized in that described porous metal substrate surface holes is 10～500 μ m.
3. according to the described preparation method of claim 1, it is characterized in that described filler is fusible change into liquid organic matter or dissolved organic matter; Wherein organic matter quality concentration is 10～80% of its saturated solution.
4. according to the described preparation method of claim 3, it is characterized in that the described fusible organic matter that changes into liquid state is solid paraffin or stearic acid; Dissolved organic matter is carboxymethyl cellulose, methylcellulose, polyvinyl alcohol or polyvinyl butyral.
5. according to the described preparation method of claim 3, when it is characterized in that adopting fusible organic thing shutoff surface holes, be that base material is immersed 1～10min in the organic matter that melts, take out condensation; When adopting dissolved organic matter shutoff surface holes, be that base material is immersed 1～5min in the organic solution, take out drying, repeat this operation 2～10 times.
6. according to the described preparation method of claim 1, before it is characterized in that carrying out the metal dust coating, adopt abrasive material that base material is polished, abrasive material is preferably 400～1000 order sand paper.
7. according to the described preparation method of claim 1, it is characterized in that the coating metal dust is stainless steel powder, nickel powder or silver powder; Coating is 0.1～25 μ m with the particle diameter of metal dust; Coating layer thickness is 20～200 μ m.
8. according to the described preparation method of claim 1, it is characterized in that described heat treated temperature is 200～500 ℃, heating rate is 0.5～2 ℃/min, and temperature retention time is 0.5～5h; Heat treatment process is carried out in air or protective atmosphere.
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| CN102247769A (en) * | 2011-06-23 | 2011-11-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of nano-scale two-dimensional porous metal film |
| CN102389715A (en) * | 2011-10-18 | 2012-03-28 | 南京工业大学 | Method for preparing porous inorganic membrane by carbon skeleton-assisted particle sintering process |
| CN103118772A (en) * | 2010-08-13 | 2013-05-22 | Sk新技术株式会社 | Pore-protected multi-layered composite separator and the method for manufacturing the same |
| CN103301871A (en) * | 2012-03-15 | 2013-09-18 | 山西腾茂科技有限公司 | Catalytic cracking catalyst and preparation method thereof |
| CN103357876A (en) * | 2013-07-29 | 2013-10-23 | 西北有色金属研究院 | Preparation method for nano multihole copper film |
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