CN110899703A - Preparation method of high-porosity metal film - Google Patents
Preparation method of high-porosity metal film Download PDFInfo
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- CN110899703A CN110899703A CN201911138919.6A CN201911138919A CN110899703A CN 110899703 A CN110899703 A CN 110899703A CN 201911138919 A CN201911138919 A CN 201911138919A CN 110899703 A CN110899703 A CN 110899703A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 157
- 239000002184 metal Substances 0.000 title claims abstract description 157
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000012188 paraffin wax Substances 0.000 claims abstract description 17
- 239000012528 membrane Substances 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 230000008595 infiltration Effects 0.000 claims abstract description 3
- 238000001764 infiltration Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical group ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 230000035699 permeability Effects 0.000 abstract description 3
- 238000009295 crossflow filtration Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000004907 flux Effects 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000009694 cold isostatic pressing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Images
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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/03—Press-moulding apparatus therefor
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a preparation method of a high-porosity metal film, which comprises the following specific steps: directly adding metal powder raw materials into a cavity consisting of a metal outer die, a metal inner die and upper and lower annular seal heads; then placing the whole die in a high-temperature sintering furnace with protective atmosphere for sintering to obtain a metal sintered body with the die; then the annular end sockets at the two ends of the sintered body are removed, the metal external mold, the metal internal mold and the metal powder sintered body are placed in molten paraffin for full infiltration, and the sintered body is taken out and cooled; placing the metal outer die and the metal inner die in an acid solution to dissolve; the metal sintered body is then soaked in an organic solvent sufficiently to remove the paraffin, and a high-porosity metal film is obtained. The prepared metal membrane with smooth inner and outer walls can be applied to inner cross flow or outer cross flow filtration, and the loosely-packed sintered metal membrane has high porosity and good permeability.
Description
Technical Field
The invention relates to a preparation method of a metal film, in particular to a preparation method of a high-porosity metal film, and belongs to the field of powder metallurgy porous films.
Background
With the rapid development of membrane science and technology, membrane separation, as a novel and efficient separation technology, has been widely applied in many fields such as energy, petrochemical, biology, health and medicine, environment, metallurgy, food, and the like.
The die pressing method is a common method for preparing a metal film at present, metal powder is filled into a die, the powder is extruded into a blank by cold isostatic pressing, the blank is removed from the die and then sintered in a high-temperature furnace, gaps among particles are greatly reduced due to the hydrostatic forming, the porosity of porous metal is basically kept at about 30%, and the permeability of the film is further influenced. Patent CN103386486B mixes metal powder and polyvinyl alcohol aqueous solution to make slurry, then coats the surface of the substrate, puts the dried and stripped metal film blank into a mould to sinter, the porosity of the prepared metal film is only 20-32%, the metal powder with 20 micron grain diameter and mixed with organic additive affect the strength of the metal film. Patent CN104550980A utilizes inorganic powder to carry out the shutoff hole to metal matrix surface, then makes the powder coating, adopts chemical reagent to wash or the ultrasonic process is clear away inorganic powder after the sintering is accomplished, through preparing the membrane that the aperture is littleer on large aperture matrix surface, can make the membrane have very little filter fineness, can keep certain permeability simultaneously again, the complicated preparation technology of asymmetric metal membrane, the cost of the asymmetric metal membrane of commercialization is all more expensive at present.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art, solve the problems of porosity, flux, preparation process and the like of the existing metal film, and provide a preparation method of a high-porosity metal film.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a high-porosity metal film comprises the following specific steps:
(A) directly adding metal powder raw materials into a cavity consisting of a metal outer die, a metal inner die and upper and lower annular seal heads;
(B) putting the whole die into a high-temperature sintering furnace with protective atmosphere or vacuum for sintering to obtain a metal sintered body with the die;
(C) after the annular end sockets at the two ends of the metal sintered body are removed, placing the metal external mold, the metal internal mold and the metal powder sintered body in molten paraffin for full infiltration, taking out and cooling;
(D) then placing the metal outer mold and the metal inner mold in an acid solution to dissolve the metal outer mold and the metal inner mold;
(E) and then the metal sintered body in which the metal external mold and the metal internal mold are dissolved is placed in an organic solvent to be fully soaked so as to remove paraffin, and the high-porosity metal film is obtained.
Preferably, the metal powder is made of stainless steel, nickel-based alloy, nickel or titanium; the metal powder has an average particle diameter of 0.1 to 300 μm.
Preferably, the metal outer mold and the metal inner mold are made of iron or copper. The inner diameter of the metal outer mold is 6-200mm, and the wall thickness is 1-5 mm; the outer diameter of the metal inner membrane is 4-190mm, and the wall thickness is 1-5 mm.
Preferably, the sintering temperature is 700-1300 ℃, and the heat preservation time is 2-5 h; the protective atmosphere is hydrogen or argon; the absolute pressure of the vacuum is 0.0001-0.1 Pa.
The annular seal head is generally made of metal, ceramic or graphite which is not melted at the sintering temperature; graphite, stainless steel, alumina, zirconia or the like is preferable.
Preferably, the acid solution is a nitric acid or hydrochloric acid solution; the mass concentration of the acid solution is 5-30%.
Preferably, the organic solvent is carbon tetrachloride, chloroform, diethyl ether, benzene, paraffin ether or carbon disulfide.
Has the advantages that:
the preparation method of the high-porosity metal film provided by the invention has low requirement on equipment, does not need large equipment such as cold isostatic pressing and the like, and reduces the production cost. Compared with the preparation process of the asymmetric membrane, the preparation process does not need to be sintered for many times and is relatively simple. In addition, compared with a cold isostatic pressing formed metal film, the metal film prepared by the method has higher flux and higher porosity, the mounting quantity of the film can be reduced under the same working condition, and resources and cost are saved.
Drawings
FIG. 1 is a schematic structural diagram of the present invention for preparing a high flux metal membrane; wherein: 1. a metal inner mold; 2. an annular seal head; 3. a metal powder; 4. and (6) forming a metal outer die.
Detailed Description
The present invention will be described in detail with reference to specific examples; the following examples the schematic structure of the high flux metal membrane prepared is shown in figure 1. It is intended that the scope of the invention be limited not by this detailed description, but rather by the claims appended hereto.
Example 1
1. Pure iron pipes are selected as an outer metal mould and an inner metal mould, and the specification of the outer metal mould is
The specification of the metal inner mold is
And (3) enabling the metal inner die to penetrate through the metal outer die, fixing one end of the metal inner die by using a graphite end socket, injecting stainless steel powder with the particle size of 50 microns into a cavity between the metal outer die and the metal inner die, and fixing and sealing the other end of the metal inner die by using the graphite end socket after the metal inner die is compacted.
2. And (3) placing the whole die in a high-temperature sintering furnace for sintering, wherein the sintering temperature is 1200 ℃, the heat preservation time is 2 hours, and the sintering atmosphere is hydrogen. And (4) removing end enclosures at two ends after sintering, immersing the die and the sintered metal film into molten paraffin, taking out and cooling, and soaking the die and the sintered metal film into nitric acid with the mass concentration of 30%. And taking out the metal film after the metal inner and outer molds are corroded, soaking the metal film in paraffin ether to remove paraffin, and finally drying the metal film in vacuum to obtain the metal film.
3. It was found that the metal film had a porosity of 62% and a nitrogen flux of 5400m3m-2h-1bar-1。
Example 2
1. The pure copper pipe is selected as an outer metal mold and an inner metal mold, and the specification of the outer metal mold is as follows
The specification of the metal inner mold is
The metal inner mold penetrates through the metal outer mold, one end of the metal inner mold is fixed by a stainless steel seal head, and nickel powder with the particle size of 0.1 micron is injected into the metal outer mold and the metal outer moldAnd the other end of the cavity between the metal internal molds is fixedly sealed by a stainless steel sealing head after the cavity is compacted.
2. And (3) placing the whole die in a high-temperature sintering furnace for sintering, wherein the sintering temperature is 700 ℃, the heat preservation time is 2 hours, and the sintering atmosphere is argon. And (4) removing end enclosures at two ends after sintering, immersing the die and the sintered metal film into molten paraffin, taking out and cooling, and soaking the die and the sintered metal film into nitric acid with the mass concentration of 20%. And taking out the metal film after the metal inner and outer molds are corroded, soaking the metal film in ether to remove paraffin, and finally drying the metal film in vacuum to obtain the metal film.
3. The metal film porosity was found to be 58% and the nitrogen flux was found to be 1400m3m-2h-1bar-1。
Example 3
1. Pure iron pipes are selected as an outer metal mould and an inner metal mould, and the specification of the outer metal mould is
The specification of the metal inner mold is
And (3) enabling the metal inner die to penetrate through the metal outer die, fixing one end of the metal inner die by using a stainless steel end socket, injecting titanium powder with the particle size of 25 microns into a cavity between the metal outer die and the metal inner die, and fixing and sealing the other end of the metal inner die by using a graphite end socket after the metal inner die is vibrated.
2. And (3) sintering the whole die in a high-temperature sintering furnace at the sintering temperature of 1100 ℃ for 3h, and sintering in vacuum at the absolute pressure of 0.0002 Pa. And (4) removing end sockets at two ends after sintering, immersing the die and the sintered metal film into molten paraffin, taking out and cooling, and soaking the die and the sintered metal film into hydrochloric acid with the mass concentration of 20%. And taking out the metal film after the metal inner and outer dies are corroded, soaking the metal film in carbon tetrachloride to remove paraffin, and finally drying in vacuum to obtain the metal film.
3. It was found that the metal film had a porosity of 61% and a nitrogen flux of 3800m3m-2h-1bar-1。
Example 4
1. Copper pipe for selectionUsed as an external metal mold and an internal metal mold, the external metal mold has the specification of
The specification of the metal film is
And (3) enabling the metal inner die to penetrate through the metal outer die, fixing one end of the metal inner die by using a ceramic end socket, injecting nickel powder with the particle size of 300 microns into a cavity between the metal outer die and the metal inner die, and fixing and sealing the other end of the metal inner die by using an alumina ceramic end socket after compaction.
2. And (3) sintering the whole die in a high-temperature sintering furnace at 1300 ℃, wherein the heat preservation time is 5 hours, and the absolute pressure is 0.1 Pa. And (4) removing end enclosures at two ends after sintering, immersing the die and the sintered metal film into molten paraffin, taking out and cooling, and soaking the die and the sintered metal film into nitric acid with the mass concentration of 5%. And taking out the metal film after the metal inner and outer molds are corroded, soaking the metal film in benzene to remove paraffin, and finally drying the metal film in vacuum to obtain the metal film.
3. It was found that the metal film had a porosity of 53% and a nitrogen flux of 12800m3m-2h-1bar-1。
Claims (7)
1. A preparation method of a high-porosity metal film comprises the following specific steps:
(A) directly adding metal powder raw materials into a cavity consisting of a metal outer die, a metal inner die and upper and lower annular seal heads;
(B) putting the whole die into a high-temperature sintering furnace with protective atmosphere or vacuum for sintering to obtain a metal sintered body with the die;
(C) removing the annular seal heads at the two ends of the metal sintered body, placing the metal sintered body in molten paraffin for full infiltration, taking out and cooling;
(D) then placing the metal outer mold and the metal inner mold in an acid solution to dissolve the metal outer mold and the metal inner mold;
(E) and soaking the metal sintered body with the metal outer mold and the metal inner mold dissolved in an organic solvent to remove paraffin to obtain the high-porosity metal film.
2. The method of claim 1, wherein: the metal powder is made of stainless steel, nickel-based alloy, nickel or titanium; the metal powder has an average particle diameter of 0.1 to 300 μm.
3. The method of claim 1, wherein: the metal outer mold and the metal inner mold are made of iron or copper.
4. The method of claim 1, wherein: the inner diameter of the metal outer mold is 6-200mm, and the wall thickness is 1-5 mm; the outer diameter of the metal inner membrane is 4-190mm, and the wall thickness is 1-5 mm.
5. The method of claim 1, wherein: the sintering temperature is 700-1300 ℃, and the heat preservation time is 2-5 h; the protective atmosphere is hydrogen or argon; the absolute pressure of the vacuum is 0.0001-0.1 Pa.
6. The method of claim 1, wherein: the acid solution is nitric acid or hydrochloric acid solution; the mass concentration of the acid solution is 5-30%.
7. The method of claim 1, wherein: the organic solvent is carbon tetrachloride, chloroform, diethyl ether, benzene, paraffin ether or carbon disulfide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911138919.6A CN110899703B (en) | 2019-11-20 | 2019-11-20 | Preparation method of high-porosity metal film |
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|---|---|---|---|
| CN201911138919.6A CN110899703B (en) | 2019-11-20 | 2019-11-20 | Preparation method of high-porosity metal film |
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| CN110899703B CN110899703B (en) | 2022-07-05 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112828280A (en) * | 2021-01-06 | 2021-05-25 | 南京工业大学 | Preparation method of metal membrane with gradient pore diameter structure |
| CN113289558A (en) * | 2021-04-29 | 2021-08-24 | 西安交通大学 | Discretization preparation method of two-dimensional material aerogel with designable three-dimensional structure |
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| CN112828280A (en) * | 2021-01-06 | 2021-05-25 | 南京工业大学 | Preparation method of metal membrane with gradient pore diameter structure |
| CN112828280B (en) * | 2021-01-06 | 2022-09-09 | 南京工业大学 | Preparation method of metal membrane with gradient pore diameter structure |
| CN113289558A (en) * | 2021-04-29 | 2021-08-24 | 西安交通大学 | Discretization preparation method of two-dimensional material aerogel with designable three-dimensional structure |
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| CN110899703B (en) | 2022-07-05 |
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