CN115445445A - Method for preparing porous nano metal film - Google Patents
Method for preparing porous nano metal film Download PDFInfo
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- CN115445445A CN115445445A CN202211217613.1A CN202211217613A CN115445445A CN 115445445 A CN115445445 A CN 115445445A CN 202211217613 A CN202211217613 A CN 202211217613A CN 115445445 A CN115445445 A CN 115445445A
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- porous
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 35
- 239000002184 metal Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000000725 suspension Substances 0.000 claims abstract description 19
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 239000011148 porous material Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 43
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 23
- 239000010936 titanium Substances 0.000 claims description 20
- 229910052719 titanium Inorganic materials 0.000 claims description 20
- 239000002270 dispersing agent Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 239000000853 adhesive Substances 0.000 claims description 8
- 230000001070 adhesive effect Effects 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000007888 film coating Substances 0.000 claims description 3
- 238000009501 film coating Methods 0.000 claims description 3
- 238000000713 high-energy ball milling Methods 0.000 claims description 3
- 238000000462 isostatic pressing Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000009692 water atomization Methods 0.000 claims description 3
- 238000009736 wetting Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000011001 backwashing Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 230000004907 flux Effects 0.000 abstract description 2
- 238000012797 qualification Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 7
- 238000000926 separation method Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/04—Tubular membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
-
- 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
- B22F3/24—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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
- B22F5/106—Tube or ring forms
-
- 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
- B22F2003/241—Chemical after-treatment on the surface
- B22F2003/242—Coating
Abstract
The invention discloses a method for preparing a porous nano metal film, which comprises the following steps: the method comprises the following steps: preparing a support body; step two: preparing a suspension; step three: putting the porous support body into a mechanical coating device, then adding the suspension, screwing down an upper cover of the mechanical coating device, starting a motor, adjusting to the rotating speed of 600r/min-800r/min, and working the mechanical coating device for 10-15 minutes; step four: the invention relates to a method for preparing a porous nano metal film, which is characterized in that the prepared porous nano metal film is subjected to pore diameter detection, and unqualified metal films are recycled to obtain the finished metal film. The filtering flux and the precision are high, the pressure drop is small, the back washing cycle is long, the back washing effect is good, the sintered metal film cannot peel and crack, and the qualification rate of the porous nano metal film is increased.
Description
Technical Field
The invention relates to a method for preparing a porous nano metal film, belonging to the technical field of nano metal film preparation.
Background
The membrane separation technology is greatly concerned by governments and industries due to the advantages of low-temperature non-phase change operation, low energy consumption, high efficiency, less loss of active ingredients of materials and the like. It has become one of the most successful and promising high-new technologies in the current generation. Practice has shown that the development of membrane materials and membrane separation techniques is inseparable. The new development of membrane materials has promoted the improvement of membrane separation techniques, and the expansion of the application range of membrane separation techniques has put new demands on membrane materials.
In the process of preparing and processing the organic film, the shrinkage force is large during sintering, and the film layer is easy to peel and crack, resulting in low yield, so a method for preparing the porous nano metal film is urgently needed.
Disclosure of Invention
The present invention is directed to a method for preparing a porous nanometal film to solve the problems of the background art mentioned above.
In order to achieve the purpose, the invention provides the following technical scheme: a method of preparing a porous nanometal film comprising the steps of:
the method comprises the following steps: preparing a support body, sintering the titanium tube formed by isostatic pressing at 1000-1200 ℃ to obtain a porous titanium tube;
step two: preparing suspension, weighing 50cm 3 2g of TiH powder which is ball-milled for 20 hours by a high-energy ball mill is weighed and put into a ball mill, and then suspension with uniform concentration is prepared by ball milling for 10 min;
step three: putting the porous titanium tube into a mechanical coating device, then adding the suspension, screwing down an upper cover of the mechanical coating device, starting a motor, adjusting to a rotating speed of 600r/min-800r/min, and working the mechanical coating device for 10-15 minutes;
step four: and (3) detecting the aperture of the prepared porous nano metal film, and recovering unqualified metal films to obtain the finished metal film.
As a preferred technical solution of the present invention, in the first step, the material selection of the porous support body affects the material selection of the porous metal film, when the porous metal film is prepared, the matching problem between the film material and the base material is firstly considered, only two materials form strong adhesion, the two materials do not peel off when dried or sintered, the strength of the adhesion can be described by the adhesion work between the film material and the base material, and the adhesion work between the film material and the base material;
W a =Y 1 +Y 2 -Y 12
the method comprises the following steps: w a : work of adhesion, J; y is 1： Surface tension of the material, N.m -1 ; Y 12： Interfacial tension between two materials, N.m -1 ;。
In the first step, the porous titanium tube is selected as the support, the porous titanium tube has large adhesion work, the expansion coefficient is close to the melting point of the two materials, and the porous titanium tube does not form alloy at low temperature.
As a preferred technical scheme of the invention, the ratio of the maximum bubble pore diameter to the average particle size of the powder of the stainless steel powder produced by the water atomization method in the first step is 0.18.
As a preferred technical scheme of the invention, the dispersant in the second step is a dispersant which has high viscosity, small wetting angle with powder and density similar to that of suspended particles, the powder is dispersed by high-energy ball milling, the dispersant is polyvinyl alcohol for titanium powder and stainless steel powder, the concentration of the polyvinyl alcohol is 3-7 wt%, and the optimal concentration of the suspension is 0.4g/cm under the condition of manual film coating process 2 。
In the second step, the suspension is suspended, and then the suspension is coated on the outer surface of the porous titanium tube which is pre-sintered at the temperature of 400-1000 ℃, and then drying treatment is carried out, wherein the temperature is 50-60 ℃, and the time is 5-15 min.
In a preferred embodiment of the present invention, in the third step, the porous metal film is slowly heated during sintering, and especially, before the dispersant is volatilized, the temperature is kept at the volatilization temperature of the dispersant, and the temperature is heated after the dispersant is volatilized.
Compared with the prior art, the invention has the beneficial effects that: the metal film prepared by the method has high temperature stability and compressive strength superior to those of a polymer film, and has toughness which a ceramic film does not have. The filtering flux and the precision are high, the pressure drop is small, the back washing cycle is long, the back washing effect is good, the sintered metal film cannot peel and crack, and the qualification rate of the porous nano metal film is increased.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for preparing a porous nano metal film,
the first embodiment is as follows: the porous nano metal film is prepared by the following steps:
the method comprises the following steps: preparing a support body, sintering the titanium tube formed by isostatic pressing at 1000-1200 ℃ to obtain a porous titanium tube;
step two: the suspension is prepared and taken 50cm 3 2g of TiH powder which is ball-milled for 20 hours by a high-energy ball mill is weighed and put into a ball mill, and then suspension with uniform concentration is prepared by ball milling for 10 min;
step three: putting the porous titanium tube into a mechanical coating device, then adding the suspension, screwing down an upper cover of the mechanical coating device, starting a motor, adjusting to a rotating speed of 600r/min-800r/min, and working the mechanical coating device for 10-15 minutes;
step four: and (3) detecting the aperture of the prepared porous nano metal film, and recovering unqualified metal films to obtain the finished metal film.
The second embodiment: in the first step, the material selection of the porous support body influences the material selection of the porous metal film, the matching problem between the film layer material and the base material is firstly considered when the porous metal film is prepared, only the two materials form stronger adhesive force, the two materials can not be peeled off when dried or sintered, the strength of the adhesive force can be described by the adhesive work between the film layer material and the base material, and the adhesive work between the film layer material and the base material;
W a =Y 1 +Y 2 -Y 12
the method comprises the following steps: w a : work of adhesion, J; y is 1： Surface tension of the material, N.m -1 ; Y 12： Interfacial tension between two materials, N.m -1 ;。
Furthermore, in the first step, a porous titanium tube is selected as the support body, the adhesion work of the porous titanium tube is large, the expansion coefficient is close to the melting point of the two materials, and the porous titanium tube does not form an alloy at low temperature.
Furthermore, the ratio of the maximum pore diameter of the bubbles to the average particle size of the powder is 0.18 in the porous material prepared by pressing and forming the stainless steel powder produced by the water atomization method in the step one.
Example three: the dispersing agent in the second step is a dispersing agent with high viscosity, small wetting angle with the powder and density similar to that of suspended particles, the powder is dispersed by high-energy ball milling, the dispersing agent is polyvinyl alcohol for titanium powder and stainless steel powder, the concentration of the polyvinyl alcohol is 3-7 wt%, and the optimal concentration of the suspension is 0.4g/cm under the condition of manual film coating process 2 。
Preferably, in the second step, the suspension is suspended, then the suspension is coated on the outer surface of the porous titanium tube which is pre-sintered at 400-1000 ℃, and then drying treatment is carried out, wherein the temperature is 50-60 ℃ and the time is 5-15 min.
Furthermore, in the third step, the porous metal film is slowly heated during sintering, especially before the dispersant is volatilized, the temperature is kept at the volatilization temperature of the dispersant, and the temperature is heated after the dispersant is volatilized.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A method for preparing a porous nanometal film, characterized in that the porous nanometal film is prepared by the following steps:
the method comprises the following steps: preparing a support body, sintering the titanium tube formed by isostatic pressing at 1000-1200 ℃ to obtain a porous titanium tube;
step two: preparing suspension, weighing 50cm 3 2g of TiH powder which is ball-milled for 20 hours by a high-energy ball mill is weighed and put into a ball mill, and then suspension with uniform concentration is prepared by ball milling for 10 min;
step three: putting the porous titanium tube into a mechanical coating device, then adding the suspension, screwing down an upper cover of the mechanical coating device, starting a motor, adjusting to the rotating speed of 600r/min-800r/min, and working the mechanical coating device for 10-15 minutes;
step four: and (3) detecting the aperture of the prepared porous nano metal film, and recovering unqualified metal films to obtain the finished metal film.
2. The method of claim 1, wherein the porous nanometal film is selected from the group consisting of: in the first step, the material selection of the porous support body influences the material selection of the porous metal film, the matching problem between a film layer material and a base material is firstly considered when the porous metal film is prepared, only two materials form stronger adhesive force, the two materials can not be peeled off when being dried or sintered, the strength of the adhesive force can be described by the adhesive work between the film layer material and the base material, and the adhesive work between the film layer material and the base material;
W a =Y 1 +Y 2 -Y 12
the method comprises the following steps: w is a group of a : work of adhesion, J; y is 1： The surface tension of the material is such that,N·m -1 ; Y 12： interfacial tension between two materials, N.m -1 ;。
3. The method of claim 1, wherein: in the first step, a porous titanium tube is selected as the support body, the porous titanium tube has large adhesion work, the expansion coefficient is close to the melting point of the two materials, and an alloy is not formed at low temperature.
4. The method of claim 1, wherein: in the porous material prepared by pressing and forming the stainless steel powder produced by the water atomization method in the step one, the ratio of the maximum bubble aperture to the average powder particle size is 0.18.
5. The method of claim 1, wherein: the dispersing agent in the second step is selected to be a dispersing agent with high viscosity, small wetting angle with powder and density similar to that of suspended particles, the powder is dispersed by high-energy ball milling, the dispersing agent is selected from polyvinyl alcohol for titanium powder and stainless steel powder, the concentration range of the polyvinyl alcohol is 3-7 wt%, and the optimal concentration of the suspension is 0.4g/cm under the condition of manual film coating process 2 。
6. The method of claim 1, wherein: and in the second step, suspending, then coating the suspension on the outer surface of the porous titanium tube pre-sintered at 400-1000 ℃, and then drying at 50-60 ℃ for 5-15 min.
7. The method of claim 1, wherein: in the third step, the temperature of the porous metal film is slowly increased during sintering, particularly, the temperature is kept at the volatilization temperature of the dispersing agent before the dispersing agent is volatilized, and the temperature is increased after the dispersing agent is volatilized.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211217613.1A CN115445445A (en) | 2022-10-05 | 2022-10-05 | Method for preparing porous nano metal film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211217613.1A CN115445445A (en) | 2022-10-05 | 2022-10-05 | Method for preparing porous nano metal film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115445445A true CN115445445A (en) | 2022-12-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211217613.1A Pending CN115445445A (en) | 2022-10-05 | 2022-10-05 | Method for preparing porous nano metal film |
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| Country | Link |
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| CN (1) | CN115445445A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6309546B1 (en) * | 1997-01-10 | 2001-10-30 | Ellipsis Corporation | Micro and ultrafilters with controlled pore sizes and pore size distribution and methods for making |
| CN1696344A (en) * | 2005-04-08 | 2005-11-16 | 华南理工大学 | Porous composite membrane of ceramics/metal and preparation method |
| CN102500245A (en) * | 2011-12-01 | 2012-06-20 | 西北有色金属研究院 | Preparation method of metal-base ceramic composite filter membrane |
| CN112546734A (en) * | 2020-12-08 | 2021-03-26 | 南京工业大学 | Method for manufacturing filter material |
-
2022
- 2022-10-05 CN CN202211217613.1A patent/CN115445445A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6309546B1 (en) * | 1997-01-10 | 2001-10-30 | Ellipsis Corporation | Micro and ultrafilters with controlled pore sizes and pore size distribution and methods for making |
| CN1696344A (en) * | 2005-04-08 | 2005-11-16 | 华南理工大学 | Porous composite membrane of ceramics/metal and preparation method |
| CN102500245A (en) * | 2011-12-01 | 2012-06-20 | 西北有色金属研究院 | Preparation method of metal-base ceramic composite filter membrane |
| CN112546734A (en) * | 2020-12-08 | 2021-03-26 | 南京工业大学 | Method for manufacturing filter material |
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