CN103752831B - A kind of preparation method of porous metal film - Google Patents
A kind of preparation method of porous metal film Download PDFInfo
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- CN103752831B CN103752831B CN201310721927.XA CN201310721927A CN103752831B CN 103752831 B CN103752831 B CN 103752831B CN 201310721927 A CN201310721927 A CN 201310721927A CN 103752831 B CN103752831 B CN 103752831B
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Abstract
The preparation method that the invention discloses a kind of porous metal film.First metal dust is deposited on mould (1) upper surface, the powder packed mixed by volume with metal dust by pore creating material again to surface has in the cavity between mould (1) and the mould (2) of metal-powder coating, use powder compressing machine that the powder in mould (1,2,3) is suppressed, prepare double-decker perforated membrane base substrate, before sintering, adopting the mode that heat resolve or solvent dissolve to be removed by pore creating material, last porous metal film base substrate prepares double-deck porous metal film after high temperature sintering.The present invention increases porosity and the aperture of base layer by pore creating material, substantially increases gas-liquid permeability；Base layer is identical with rete powder diameter, once sintered porous metal film of preparing, and saves the energy.
Description
Technical field
The preparation method that the present invention relates to a kind of porous metal film, particularly relating to a kind of structure is double-decker, the preparation method of the porous metal film that gas-liquid flux is big.
Background technology
Porous metals refer to particulate metal material being made up of metallic framework and hole.For dense material, a large amount of ducts within porous metals impart the many excellent properties of porous metals, as big in specific surface area, permeability is excellent (through hole body), energy absorption is good, proportion is little, heat exchange heat-sinking capability high (through hole body), sound absorption properties good (through hole body), electromagnetic wave absorbability good (through hole body), heat and flame, resistance flame, anti-thermal shock, can regenerate, processability good etc..Just because of this, porous metals are widely used in the technical processs such as the separation of the industries such as Aero-Space, electrochemistry, petrochemical industry, metallurgy, atomic energy, machinery, medicine, environmental protection, building, filtration, gas distribution, catalysis, electrochemical process, noise reduction, shock-absorbing, shielding, heat exchange.
Filtering and separating is one of most important application of metal polyporous material.Porous metals, as filtering material, are generally used in the process technique of microfiltration and ultrafiltration.Compared with traditional organic membrane and ceramic membrane, there is bigger development and application space.Because the shortcoming of organic membrane is mainly: 1, operating environment requirements is high, and the bearing capacity of organic membrane, heat-resisting ability, acid and alkali-resistance ability is all poor.2, organic membrane cleans more difficult after polluting, and membrane lifetime is short.And ceramic membrane preferably resolves the defect of organic membrane, but the property of ceramic material is crisp, bad mechanical property, fragile.And porous metals largely avoid the defect of organic membrane and ceramic membrane.
Porous metals advantage compared with organic membrane and ceramic membrane is as follows: 1: mechanical strength is high, can use (pressure up to 7MPa) at elevated pressures.2: there is good thermal conductivity performance and better heat-sinking capability, therefore reduce the thermal stress of membrane module, thus improve the service life of film.3: good seal performance.Having good welding performance, membrane module is easily attached.4: there is very strong using value.In filter process, porous metal film adsorbance is big, and supportive is good, and filter area is big, can on-line cleaning, do not affect production.
Can meeting requirement of actual working condition because porous metals must have certain mechanical strength, in order to reach required intensity, the wall thickness of porous metals is all at more than 2mm, and when using as filter, filtration wall thickness only needs 0.1mm.The wall thickness of more than 2mm causes certain pressure intensity loss, wastes mass energy, and gas-liquid flux is low, reduces service efficiency.In order to solve as above produced problem, the porous metals preparing multiple structure are the solution routes that research worker is unanimously thought.
The method of multi-layer porous metal is prepared in the exploitation of current research worker mainly hot spray process, magnetron sputtering method, wet-milling spraying process, spread coating, centrifugal top and bottom process etc..And these preparation technologies more or less also exist defect, such as wet-milling spraying process and spread coating etc. also exist matrix needs multi-time modification, and rete is easy to fall off；Centrifugal top and bottom process matrix powder cannot realize co-sintering etc. with rete powder.Researcher research is additionally also had to prepare ceramic coating [Huang Yan, Yu Jian on porous metals surface, a kind of preparation method of porous ceramics one metal composite membrane material, application number: CN201110168259], but owing to pottery is different with the thermal coefficient of expansion of metal, the fastness of rete is poor, although claim ceramic-metal composite film commercialization, but without this series products on market.In general, the method preparing gradient porous metal at present also exists problems.
Summary of the invention
It is an object of the invention to provide that a kind of thickness is controlled, the preparation technology of rete and matrix energy co-sintering and the big porous metal film of the penetrating amount of gas-liquid.
The resolving ideas of the present invention is by preparing layer of metal powder bed on mould (1) surface, the powder packed mixed by volume with metal dust by pore creating material again is to the cavity between mould (1) and mould (2), compressing through press, before sintering, pore creating material is removed by the mode adopting heat resolve or Solvents Solvent, and last porous metal film base substrate makes double-deck porous metal film after high temperature sintering.The present invention increases aperture and the porosity of matrix by adding pore creating material in matrix powder, thus realizing the double-skinned of structure, and matrix powder and rete powder belong to the same particle diameter metal dust with material, are absent from the problem that co-fired temperature selects, once sintered molding, saves the energy.
The technical solution used in the present invention is as follows:
A kind of preparation method of porous metal film.First metal dust is deposited on mould (1) upper surface, the powder packed mixed by volume with metal dust by pore creating material again is to the cavity between mould (1) and mould (2), compressing through press, before sintering, pore creating material is removed by the mode adopting heat resolve or Solvents Solvent, and last porous metal film base substrate prepares porous metal film through high temperature sintering.
The preparation method of the present invention, its advantage at least includes: 1, preparing metallic diaphragm base substrate at mould (1) upper surface, the film surface of preparation is highly polished；2, by adding pore creating material, under the premise not changing sintering temperature, it is achieved porous metal structure double-skinned；3, rete powder is after repressed molding, and compared with rete prepared by conventional coating techniques, porous metals aperture prepared by diameter powders of the same race is less, it is narrower to be distributed；4, once sintered, save the energy.
The preparation method of described a kind of porous metal film, it is characterised in that comprise the following steps: a, configuration metal powder suspensions, prepare layer of metal powder coating at mould (1) upper surface；B, pore creating material mix by 0.5: 1 to 1: 50 volume ratios with metal dust；In c, cavity mixture being filled between mould (1) and mould (2)；Powder in mould (1,2,3) is suppressed by d, use press；Pore creating material is removed by the mode that e, employing heat resolve or solvent dissolve；F, porous metals base substrate is put under protective atmosphere or vacuum environment sinter, after cooling prepare double-decker porous metals membrane material.
Described coating production is be scattered in the alcoholic solution of PVB or PVP by metal dust, forms stable suspension, adopts the spraying of infusion process, wet-milling, cladding process or straight pressing to prepare metallic diaphragm at mould (1) upper surface.
Described metal dust material is the one in rustless steel, nickel, copper, titanium and silver, and powder average particle size is 1-300 μm.
Described pore creating material is the one in carbamide, polymethyl acrylate, starch, sodium chloride, mixing at 0.5: 1 to 1: 50 by volume of pore creating material and metal dust.
The removing method of described pore creating material is the one during solvent dissolves and thermally decomposes.
The pressing pressure of described press is 2-20MPa, press time 10-900s.
Described is sintered under vacuum or reducing atmosphere to carry out, and heating rate 1-10 DEG C/min, sintering temperature is 600-1200 DEG C.
Beneficial effects of the present invention: present invention achieves the double-deck porous metals of particle diameter metal powder preparation of the same race, this method solves the problem of co-sintering temperature time prepared by double-decker porous metals, the porous metals gas-liquid flux prepared is big, and once sintered, saves the energy.
Accompanying drawing
Fig. 1 is the schematic diagram of mould (1,2,3)
Fig. 2 is the section metallograph of porous stainless steel membrane
Detailed description of the invention
Embodiment 1
A kind of preparation process of porous stainless steel:
1, configuration 2wt.%PVB alcoholic solution, puts into the powder of stainless steel that mean diameter is 25 μm and is wherein uniformly dispersed.
2, one layer of powder of stainless steel rete is prepared by cladding process at mould (1) upper surface.
3, being that 25 μm of powder of stainless steel mix by volume at 1: 1 by carbamide and mean diameter, filled to the cavity between mould (1) and mould (2) by mixture, press pressing pressure is 10MPa, and the press time is 100s.
4, porous stainless steel blank is put into maintenance 3h in hot water, removes pore creating material carbamide.
5, porous stainless steel blank is put in hydrogen sintering furnace, with the ramp of 1 DEG C/min to 1000 DEG C sinter, be incubated 10h, be naturally down to room temperature, porous stainless steel.
Embodiment 2
A kind of preparation process of nickel porous:
1, configuration 2wt.%PVP alcoholic solution, puts into the nickel by powder that mean diameter is 50 μm and is wherein uniformly dispersed.
2, layer of metal powder rete is prepared by wet-milling spraying process at mould (1) upper surface.
3, starch and the nickel by powder that mean diameter is 50 μm being mixed at 1: 10 by volume, filled to the cavity between mould (1) and mould (2) by mixture, the pressing pressure of press is 5MPa, and the press time is 500s.
4, nickel porous base substrate being put into high-temperature atmosphere furnace, the first step under an argon atmosphere, adopts the heating rate of 4 DEG C/min to be heated to 400 DEG C, is incubated 1h, elimination pore creating material and Organic substance；Second step in a hydrogen atmosphere, sinters with the ramp of 2 DEG C/min to 800 DEG C, is incubated 5h, is naturally down to room temperature, can obtain nickel porous.
Embodiment 3
A kind of preparation process of POROUS TITANIUM:
1, configuration 3wt.%PVP alcoholic solution, puts into the titanium powder that mean diameter is 100 μm and is wherein uniformly dispersed.
2, one layer of titanium valve rete is prepared by infusion process at mould (1) upper surface.
3, sodium chloride and the titanium powder that mean diameter is 100 μm being mixed at 1: 40 by volume, filled to the cavity between mould (1) and mould (2) by mixture, the pressing pressure of press is 15MPa, and the press time is 100s.
4, POROUS TITANIUM base substrate is put into maintenance 5h in hot water, removes pore creating material sodium chloride.
5, POROUS TITANIUM base substrate is put in vacuum sintering furnace, sinter with the ramp of 1 DEG C/min to 1000 DEG C, be incubated 10h, be naturally down to room temperature, double-decker POROUS TITANIUM can be obtained.
Above example is intended merely to the explanation present invention, any equivalence change done when without departing from spirit of the present invention, broadly falls into the scope of the claims in the present invention.
Claims (8)
1. the preparation method of a porous metal film, it is characterized in that: metal dust is deposited on mould (1) upper surface, the powder packed mixed by volume with metal dust by pore creating material again to surface has in the cavity between the mould (1,2) of metal-powder coating, use press that the powder in mould (1,2,3) is suppressed, prepare double-decker perforated membrane base substrate, before sintering, adopting the mode that heat resolve or solvent dissolve to be removed by pore creating material, last porous metal film base substrate prepares porous metal film after high temperature sintering.
2. the preparation method of a kind of porous metal film according to claim 1, it is characterised in that comprise the following steps: a, configuration metal powder suspensions, prepare layer of metal powder coating at mould (1) upper surface；B, pore creating material mix by volume with metal dust；In c, cavity mixture being filled between the mould (1,2) of the existing metal-powder coating in surface；Powder in mould (1,2,3) is suppressed by d, use press；Pore creating material is removed by the mode that e, employing heat resolve or solvent dissolve；F, porous metals base substrate is put under protective atmosphere or vacuum environment sinter, after cooling prepare double-decker porous metals membrane material.
3. the preparation method of a kind of porous metal film according to claim 2, it is characterized in that described coating production is be scattered in the alcoholic solution of PVB or PVP by metal dust, form stable suspension, adopt the spraying of infusion process, wet-milling, cladding process or straight pressing to prepare metallic diaphragm at mould (1) upper surface.
4. the preparation method of a kind of porous metal film according to claim 2, it is characterised in that described metal dust material is the one in rustless steel, nickel, copper, titanium and silver, and powder average particle size is 1-300 μm.
5. the preparation method of a kind of porous metal film according to claim 2, it is characterized in that described pore creating material is the one in carbamide, polymethyl acrylate, starch, sodium chloride, calcium carbonate, mixing at 0.5: 1 to 1: 50 by volume of pore creating material and metal dust.
6. the preparation method of a kind of porous metal film according to claim 2, it is characterised in that the removing method of described pore creating material is the one during solvent dissolves and thermally decomposes.
7. the preparation method of a kind of porous metal film according to claim 2, it is characterised in that the pressing pressure of described press is 2-20MPa, press time 10-900s.
8. the preparation method of a kind of porous metal film according to claim 2, it is characterised in that described is sintered under vacuum or reducing atmosphere to carry out, and heating rate 1-10 DEG C/min, sintering temperature is 600-1200 DEG C.
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| CN104550980B (en) * | 2015-01-21 | 2016-10-26 | 南京工业大学 | A kind of preparation method of high gradient porous metal film |
| CN104667758A (en) * | 2015-02-25 | 2015-06-03 | 成都易态科技有限公司 | Negative-pressure coating method |
| CN107866105A (en) * | 2016-09-26 | 2018-04-03 | 江苏雄凯过滤技术有限公司 | A kind of production technology of double-layer stainless steel filter material |
| CN106552940B (en) * | 2016-10-17 | 2018-05-25 | 昆明理工大学 | A kind of preparation method of the ordered porous TiAg alloys of gradient |
| CN106474937B (en) * | 2016-11-28 | 2019-07-19 | 南京工业大学 | The burning process of porous stainless steel membrane |
| CN106853529A (en) * | 2016-12-09 | 2017-06-16 | 沈阳理工大学 | A kind of preparation method of porous TiNb alloys |
| CN106756187B (en) * | 2016-12-16 | 2018-05-29 | 西安理工大学 | A kind of powder metallurgic method that porous titanium material is prepared with rice hulls pore creating material |
| CN108115143B (en) * | 2017-12-22 | 2021-03-09 | 苏州第一元素纳米技术有限公司 | Preparation method of filter device |
| CN109304463A (en) * | 2018-10-09 | 2019-02-05 | 中国科学院合肥物质科学研究院 | A kind of aperture, the adjustable high porosity Mn-Cu base high-damping alloy of pass production method |
| CN111085687A (en) * | 2019-11-01 | 2020-05-01 | 嘉善欧本轴承有限公司 | Self-lubricating composite material and production process thereof |
| CN111672338A (en) * | 2020-05-18 | 2020-09-18 | 浙江格尔泰斯环保特材科技股份有限公司 | Preparation method of polytetrafluoroethylene microporous film with ultrahigh porosity |
| CN112809008A (en) * | 2020-07-22 | 2021-05-18 | 张明明 | Heat conduction layer preparation process based on porous sintering of metal powder fiber |
| CN113289558B (en) * | 2021-04-29 | 2022-05-06 | 西安交通大学 | Discretization preparation method of two-dimensional material aerogel with designable three-dimensional structure |
| CN113737171B (en) * | 2021-09-10 | 2022-09-02 | 西北有色金属研究院 | Preparation method of porous tantalum film |
| CN114289720B (en) * | 2021-11-30 | 2023-09-29 | 成都易态科技有限公司 | Preparation method of green body and sintered porous metal film and dust removal method |
| CN114523108B (en) * | 2021-11-30 | 2023-09-29 | 成都易态科技有限公司 | Blank, sintered porous metal film and dust removal method |
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| CN1299808C (en) * | 2005-03-03 | 2007-02-14 | 上海一鸣过滤技术有限公司 | Tubular reducing stainlss steel micro porous film and its preparing method |
| US7896949B2 (en) * | 2005-09-28 | 2011-03-01 | General Electric Company | Membranes for separation of carbon dioxide |
| JP2008055310A (en) * | 2006-08-31 | 2008-03-13 | Sanyo Special Steel Co Ltd | Supporting body for hydrogen-permeable membrane and its manufacturing method |
| CN101791524B (en) * | 2010-03-26 | 2012-06-27 | 南京工业大学 | Asymmetrically-structural ceramic ultrafiltration membrane and preparation method thereof |
| IL213533A (en) * | 2011-06-14 | 2015-11-30 | Leo Mendelovici | Process for thermally spraying a porous metal sacrificial coating on substrate parts of sputtering tools |
| CN102836642B (en) * | 2011-06-22 | 2015-04-01 | 南京髙谦功能材料科技有限公司 | Preparation method of porous ceramic-metal composite film material |
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