CN104959611A - Porous film and preparation method of porous film - Google Patents
Porous film and preparation method of porous film Download PDFInfo
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- CN104959611A CN104959611A CN201510274798.3A CN201510274798A CN104959611A CN 104959611 A CN104959611 A CN 104959611A CN 201510274798 A CN201510274798 A CN 201510274798A CN 104959611 A CN104959611 A CN 104959611A
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Abstract
The invention discloses a porous film and a preparation method of the porous film, which can easily achieve high porosity and guarantee the formability during the preparation, and are simple and practical in preparation process. The thickness of the porous film is 200-1500[mu]m, the average aperture of the porous film is 0.05-100[mu]m, and the porosity of the porous film is 25-75%. The preparation method includes (1) acquiring a support film which has a porous first material, and forming primary pores in the first material; (2) preparing slurry containing a powder-like second material; (3) coating the support film with the slurry to prepare a base substrate; (4) sintering the base substrate, generating a porous third material through the self-reaction of the second material during the sintering, and further generating secondary pores communicated with the primary pores; and (5) cooling the base substrate to obtain the porous film after the sintering. The porous film at least contains the primary pores and the secondary pores, so that the porous film is easy to achieve high porosity.
Description
Technical field
The present invention relates to the preparation of porous membrane and porous membrane, particularly relate to porous inorganic membrane, particularly porous metal film.
Background technology
Sintering inorganic porous material such as sintering diamond bit, the main of sintered ceramic porous material are used as filtering material.In a particular application, the filter element of definite shape and structure need be made into, then filter element be installed in filter.Existing sintering inorganic porous material filter element is all cast or the plate profile structure of rigidity substantially.Their preparation principle is similar, is namely haply: the pressed compact (generally adopting equal pressing forming technology) first by special mould, raw meal being pressed into cast or template, and then sinters pressed compact, obtains product after sintering.
The filter element of above-mentioned cast or template is due to by its shape, structure and the subsidiary and impact of the corresponding requirements on filter and system that is that come, and the scope of application is limited.Owing to comparing current filter element (such as organic filter film) on sintering inorganic porous material filter element is in the repellence, material irreversible membrane fouling repellence etc. of chemical erosion, there is stronger advantage, therefore, to develop in multiple field can the novel sintered inorganic porous material filter element of the original filter element of corresponding substitute especially sintering diamond bit filter element is highly significant.
On above-mentioned background basis, it is 2014106089803 that applicant successively have submitted application number, name is called " flexible, porous metal forming and preparation method thereof ", application number is 2015101531163, name is called that " preparation method of flexible, porous metal forming and flexible, porous metal forming " and application number are 201510153106X, name is called multinomial patent applications such as " preparation methods of multicellular metal foil ", for exploitation has the nothing support porous membrane sintering inorganic porous material good characteristic, (implication of " without supporting " refers to that porous membrane itself has self-supporting, need not be attached on support frame and just can use) provide solution route.
But applicant finds in practice: no matter take which kind of current technique to support porous membrane to prepare above-mentioned nothing, the intensity of the porosity of porous membrane and the formability of material and shaping rear porous membrane is often conflicting.The porosity of porous membrane is improved in order to pursue better strainability requirement, but the porosity improving porous membrane will reduce the intensity of the formability of porous membrane (be mainly reflected in the situation such as material cracks and distortion in preparation process, product fraction defective promotes) and porous membrane product accordingly.
Summary of the invention
For above-mentioned situation, technical problem to be solved by this invention is: provide several preparation method easily reaching higher porosity, can ensure again the porous membrane that formability, preparation technology when preparing is simple and practical and porous membrane.
The first porous membrane of the present invention, thickness is 5 ~ 200 μm, average pore size is 0.05 ~ 100 μm, porosity is 25 ~ 75%, the step of its preparation method comprises: (1) obtains support membrane, described support membrane has cavernous first material, described first material is formed with a hole; (2) slurry is produced, containing pulverous second material in described slurry; (3) described slurry is coated on support membrane then makes base substrate; (4) described base substrate is sintered, react between the first material and the second material during sintering and generate cavernous 3rd material and produce the secondary hole with a porosity communication simultaneously; (5) after sintering, cooling obtains porous membrane.When also containing the first material do not reacted with the second material in the porous membrane that step (5) obtains, described preparation method also can comprise step (6) further, namely with etching solution porous membrane soaked thus selectively on porous membrane form three holes by after the first material dissolves, then drying being carried out to porous membrane and obtain finished product.
The second porous membrane of the present invention, thickness is 5 ~ 200 μm, average pore size is 0.05 ~ 100 μm, porosity is 25 ~ 75%, the step of its preparation method comprises: (1) obtains support membrane, described support membrane has cavernous first material, the first material is formed with a hole; (2) slurry is produced, containing pulverous second material in described slurry; (3) described slurry is coated on support membrane then makes base substrate; (4) sinter described base substrate, during sintering, the second material id reaction generates the secondary hole of cellular the 3rd material and then generation and a porosity communication; (5) after sintering, cooling obtains porous membrane.Described preparation method also can comprise step (6) further, namely with etching solution porous membrane soaked thus form three holes after selective the first material dissolves to staying on porous membrane, then drying being carried out to porous membrane and obtain finished product.
The third porous membrane of the present invention, thickness is 200 ~ 1500 μm, average pore size is 0.05 ~ 100 μm, porosity is 25 ~ 75%, the step of its preparation method comprises: (1) obtains support membrane, described support membrane has cavernous first material, described first material is formed with a hole; (2) slurry is produced, containing pulverous second material in described slurry; (3) described slurry is coated on support membrane then makes base substrate; (4) described base substrate is sintered, react between the first material and the second material during sintering generate cavernous 3rd material and and then produce and the secondary hole of a porosity communication; (5) after sintering, cooling obtains porous membrane.When also containing the first material do not reacted with the second material in the porous membrane that step (5) obtains, described preparation method also can comprise step (6) further, namely with etching solution porous membrane soaked thus selectively on porous membrane form three holes by after the first material dissolves, then drying being carried out to porous membrane and obtain finished product.
4th kind of porous membrane of the present invention, thickness is 200 ~ 1500 μm, average pore size is 0.05 ~ 100 μm, porosity is 25 ~ 75%, the step of its preparation method comprises: (1) obtains support membrane, described support membrane has cavernous first material, the first material is formed with a hole; (2) slurry is produced, containing pulverous second material in described slurry; (3) described slurry is coated on support membrane then makes base substrate; (4) sinter base substrate, during sintering, the second material id reaction generates the secondary hole of cellular the 3rd material and then generation and a porosity communication; (5) after sintering, cooling obtains porous membrane.Described preparation method also can comprise step (6) further, namely with etching solution porous membrane soaked thus form three holes after selective the first material dissolves to staying on porous membrane, then drying being carried out to porous membrane and obtain finished product.
All employ support membrane in the preparation process of above-mentioned four kinds of porous membranes, described support membrane is final or form the part of porous membrane finished product, or is dissolved by etching solution, or part forms a part for porous membrane finished product and part is dissolved by etching solution.In a word, because these four kinds of porous membranes all at least contain once hole and secondary hole, therefore porous membrane easily reaches higher porosity; And supported by support membrane due to base substrate in the preparation process of porous membrane, the fine situation such as material cracks and distortion when avoiding sintering, therefore effectively can reduce without the shaping difficulty supporting porous membrane and improve Forming Quality.
In the preparation process of above-mentioned four kinds of porous membranes, the support membrane of use is preferably net type film, and its mesh size is generally 20 ~ 1000 orders.So-called " net type film " refers to the film constructing similar screen cloth.In the present invention, the mesh size of net type film is set as that 20 ~ 1000 orders are proper.If mesh increases further on this number range basis, after easily causing slurry to cover imperfect, sintering during coating slurry, there is the defects such as trachoma in porous membrane; If mesh reduces further on this number range basis, some adverse effects will be caused because the coated weight of slurry is less to porous membrane.The large I of mesh more preferably 40 ~ 400 orders of net type film.Certainly, support membrane not can only adopt net type film, adopts the porous material of non-net form (multicellular metal foil mentioned in such as background technology) to be also feasible.
The present invention's the first porous membrane above-mentioned and the third porous membrane preferably a kind of the 3rd material be made up of solid solution alloy are the metal film of matrix phase, wherein, described first material forms the solvent source of this solid solution alloy, second material forms the solute source of this solid solution alloy, and during sintering, the first material and the second material occur partially to spread pore-creating and react.Such as, porous membrane is a kind of the 3rd material be made up of Ag-Au solid solution, Ti-Zr solid solution, Mg-Cd solid solution, Fe-Cr solid solution, Ni-Cu solid solution, Cu-Al solid solution, Cu-Zn solid solution or Fe-C-Cr solid solution is the metal film of matrix phase.The first porous membrane above-mentioned and the third porous membrane generally have have flexibility, excellent corrosion resistance, can be high temperature resistant etc. characteristic, wherein, this the first porous membrane thinner thickness (5 ~ 200 μm), its industrially can be used for weave and leather industry in waste heat recovery, medicament recovery, Environmental capacity, purification in food-processing industry, concentrated, sterilization, byproduct reclaim, medicine and healthcare industry in artificial tracheae, Co ntrolled release, blood filtration, Water warfare, the cleaner in auto industry; The dust-filtering material of mouth mask and the curtain material of static electrification dedusting function is can be used as on civilian; The third porous membrane thickness thicker (200 ~ 1500 μm), therefore intensity is higher, a typical example application is made into the filter bag filtered, thus replace the filter element " cloth bag " in current sack cleaner.Visible, this first porous membrane and the third porous membrane have the purposes of differentiation.In addition, " partially the diffusion pore-creating reaction " mentioned in foregoing is actual refers to Kinkendal Effect (kirkendall effect), belongs to the conventional pore-creating means in the preparation of powder sintered inorganic porous material.
In the preparation process of the above-mentioned the second porous membrane of the present invention and the 4th kind of porous membrane, described second material preferably includes at least two kinds of powders, during described at least two kinds of powder sinterings, formation is the 3rd material of matrix phase by solid solution alloy, in these two kinds of powders, wherein a kind of powder forms the solvent source of this solid solution alloy, another kind of powder forms the solute source of this solid solution alloy, and diffusion pore-creating reaction partially occurs between at least two kinds of powders described in during sintering; Described first material is then a kind of metal material showing as inertia under described sintering condition relative to the second material.Such as, described second material id reaction generates the 3rd material being matrix phase with Ag-Au solid solution, Ti-Zr solid solution, Mg-Cd solid solution, Fe-Cr solid solution, Ni-Cu solid solution, Cu-Al solid solution, Cu-Zn solid solution or Fe-C-Cr solid solution; When described 3rd material is made up of Ni-Cu solid solution, described first Material selec-tion is 304 stainless steels.Above-mentioned the second porous membrane and the 4th kind of porous membrane generally have have flexibility, excellent corrosion resistance, can be high temperature resistant etc. characteristic, wherein, this the second porous membrane is thinner, its industrially can be used for weave and leather industry in waste heat recovery, medicament recovery, Environmental capacity, purification in food-processing industry, concentrated, sterilization, byproduct reclaim, medicine and healthcare industry in artificial tracheae, Co ntrolled release, blood filtration, Water warfare, the cleaner in auto industry; The dust-filtering material of mouth mask and the curtain material of static electrification dedusting function is can be used as on civilian; The metal film of the 4th kind of porous membrane is thicker, and intensity is higher, and a typical example application is made into the filter bag filtered, thus replace " cloth bag ".Visible, this second porous membrane and the 4th kind of porous membrane have the purposes of differentiation equally.
The preparation method of the first porous membrane of the present invention, its step comprises: (1) adopts Cu net to be support membrane, and the thickness of described support membrane is set as 0.05 ~ 0.1 millimeter, and mesh size is set as 40 ~ 200 orders; (2) by particle diameter be that-400 object Ni powder take ethanol as dispersant, PVB for binding agent by adding 2 ~ 5 grams of PVB in every 100 milliliters of ethanol, the proportional arrangement of 50 ~ 100 grams of Ni powder becomes slurry; (3) described slurry to be coated on support membrane and to dry and make base substrate; (4) segmented sintering is carried out to base substrate, first stage rises to 120 ~ 250 DEG C from room temperature and is incubated 120 ~ 180 minutes, second stage is warming up to 500 ~ 600 DEG C and is incubated 60 ~ 240 minutes, and the phase III is warming up to 900 ~ 1090 DEG C and is incubated 90 ~ 240 minutes; (5) the obtained porous membrane of cooling after sintering.When in porous membrane also containing the Cu do not reacted with Ni powder time, described method also can comprise step (6) further, is namely the FeCl of 0.5 ~ 1mol/L by concentration
3solution carries out immersion 20 ~ 40 minutes to porous membrane thus selectively on porous membrane Cu is dissolved formation three holes, then carries out drying to porous membrane and obtains finished product.The method can prepare the Ni-Cu flexible, porous metal forming belonging to the first porous membrane above-mentioned.Recognize the file that the advantage of Ni-Cu flexible, porous metal forming can be quoted as proof from background technology part of the present invention, therefore do not repeat them here.
The preparation method of the second porous membrane of the present invention, its step comprises: (1) adopts 304 stainless (steel) wires to be support membrane, and the thickness of support membrane is set as 0.05 ~ 0.1 millimeter, and mesh size is set as 60 ~ 400 orders; (2) to be the Ni powder of 3 ~ 5 μm and particle diameter by particle diameter be-400 object Cu powder are 20 ~ 40% be configured to mixed powder by the percentage by weight of Cu, be then dispersant with ethanol, PVB for binding agent by adding 2 ~ 5 grams of PVB in every 100 milliliters of ethanol, the proportional arrangement of 50 ~ 100 grams of mixed powders becomes slurry; (3) described slurry to be coated on support membrane and to dry and make base substrate; (4) segmented sintering is carried out to base substrate, first stage rises to 120 ~ 250 DEG C from room temperature and is incubated 120 ~ 180 minutes, second stage is warming up to 500 ~ 600 DEG C and is incubated 60 ~ 240 minutes, and the phase III is warming up to 900 ~ 1090 DEG C and is incubated 90 ~ 240 minutes; (5) the obtained described porous membrane of cooling after sintering.Method also can comprise step (6) further, is namely the FeCl of 0.4 ~ 0.8mol/L by concentration
2solution carries out immersion 30 ~ 60 minutes to porous membrane thus selective on porous membrane 304 stainless steels is dissolved formation three holes, then carries out drying to porous membrane and obtains finished product.The method can prepare the Ni-Cu base flexible, porous metal forming belonging to above-mentioned the second porous membrane.
The preparation method of the third porous membrane of the present invention, its step comprises: (1) adopts Cu net to be support membrane, and the thickness of described support membrane is set as 0.5 ~ 1 millimeter, and mesh size is set as 40 ~ 200 orders; (2) by particle diameter be that-400 object Ni powder take ethanol as dispersant, PVB for binding agent by adding 2 ~ 5 grams of PVB in every 100 milliliters of ethanol, the proportional arrangement of 50 ~ 100 grams of Ni powder becomes slurry; (3) described slurry to be coated on support membrane and to dry and make base substrate; (4) segmented sintering is carried out to base substrate, first stage rises to 120 ~ 250 DEG C from room temperature and is incubated 120 ~ 180 minutes, second stage is warming up to 500 ~ 600 DEG C and is incubated 60 ~ 240 minutes, and the phase III is warming up to 900 ~ 1090 DEG C and is incubated 90 ~ 240 minutes; (5) the obtained porous membrane of cooling after sintering.When in porous membrane also containing the Cu do not reacted with Ni powder time, described method also can comprise step (6) further, is namely the FeCl of 0.5 ~ 1mol/L by concentration
3solution carries out immersion 20 ~ 40 minutes to porous membrane thus selectively on porous membrane Cu is dissolved formation three holes, then carries out drying to porous membrane and obtains finished product.The method can prepare the Ni-Cu flexible, porous metal forming belonging to the third porous membrane above-mentioned.
The preparation method of the 4th kind of porous membrane of the present invention, its step comprises: (1) adopts 304 stainless (steel) wires to be support membrane, and the thickness of described support membrane is set as 0.5 ~ 1 millimeter, and mesh size is set as 60 ~ 400 orders; (2) to be the Ni powder of 3 ~ 5 μm and particle diameter by particle diameter be-400 object Cu powder are 20 ~ 40% be configured to mixed powder by the percentage by weight of Cu, be then dispersant with ethanol, PVB for binding agent by adding 2 ~ 5 grams of PVB in every 100 milliliters of ethanol, the proportional arrangement of 50 ~ 100 grams of mixed powders becomes slurry; (3) described slurry to be coated on support membrane and to dry and make base substrate; (4) segmented sintering is carried out to base substrate, first stage rises to 120 ~ 250 DEG C from room temperature and is incubated 120 ~ 180 minutes, second stage is warming up to 500 ~ 600 DEG C and is incubated 60 ~ 240 minutes, and the phase III is warming up to 900 ~ 1090 DEG C and is incubated 90 ~ 240 minutes; (5) the obtained described porous membrane of cooling after sintering.Method also can comprise step (6) further, is namely the FeCl of 0.4 ~ 0.8mol/L by concentration
2solution carries out immersion 30 ~ 60 minutes to porous membrane thus selective on porous membrane 304 stainless steels is dissolved formation three holes, then carries out drying to porous membrane and obtains finished product.The method can prepare the Ni-Cu base flexible, porous metal forming belonging to above-mentioned 4th kind of porous membrane.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.The aspect that the present invention adds and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Embodiment 1
The step preparing porous membrane comprises: (1) adopts Cu net to be support membrane (outsourcing red copper screen cloth), and the thickness of described support membrane is set as 0.08 millimeter, and mesh size is set as 200 orders, (2) by particle diameter be that-400 object Ni powder (purity 99.7%) take ethanol as dispersant, PVB for binding agent by adding 3 grams of PVB in every 100 milliliters of ethanol, the proportional arrangement of 70 grams of Ni powder becomes slurry, (3) described slurry to be sprayed on support membrane (quantity for spray of slurry is every square metre of support membrane spraying 500g slurry) and to dry at 60 DEG C after 4 hours and make base substrate, (4) segmented sintering is carried out to base substrate, first stage rises to 220 DEG C from room temperature and is incubated 150 minutes, the Main Function in this stage removes moisture remaining in base substrate and impurity, ensure that film causes the phenomenon of cracking in later stage sintering process without other undesirable elements, second stage is warming up to 550 DEG C and is incubated 200 minutes, the Main Function in this stage is that the PVB removed in material makes subsequent reactions abundant, the uniformity of proof strength performance, phase III is warming up to 1000 DEG C and is incubated 220 minutes, the Main Function in this stage makes Ni-Cu alloy phase homogenising, during sintering, second stage heating rate is 1 ~ 3 DEG C/min, phase III heating rate 5 ~ 7 DEG C/min, (5) the obtained porous membrane of cooling after sintering.The thickness of this porous membrane is 0.12mm, average pore size 15 μm, and porosity is 54%, and air permeability is 1500m
3/ m
2hkpa (represents every m per hour under every kpa filtration pressure
2filter area under the infiltration capacity of air (by m
3represent)).
Embodiment 2
Embodiment 2 is identical haply with the porous membrane preparation process of embodiment 1, but difference is: phase III during sintering be warming up to 1000 DEG C after only insulation 120 minutes, thus the Cu element in support membrane is not all reacted with Ni; After this, be the FeCl of 0.5mol/L by concentration
3solution carries out immersion 35 minutes to the porous membrane that step (5) obtains thus selectively on porous membrane Cu is dissolved formation three holes, then carries out drying to porous membrane and obtains finished product.The thickness of finally obtained porous membrane is 0.12mm, and average pore size 17 μm, porosity is 63%, and air permeability is 1820m
3/ m
2hkpa.
Embodiment 3
The step preparing porous membrane comprises: (1) adopts 304 stainless (steel) wires to be support membrane (outsourcing 304 stainless steel mesh), and the thickness of support membrane is set as 0.08 millimeter, and mesh size is set as 250 orders, (2) to be the Ni powder of 3 ~ 5 μm and particle diameter by particle diameter be-400 object Cu powder are 30% be configured to mixed powder by the percentage by weight of Cu, be then dispersant with ethanol, PVB for binding agent by adding 3 grams of PVB in every 100 milliliters of ethanol, the proportional arrangement of 70 grams of mixed powders becomes slurry, (3) described slurry to be sprayed on support membrane (quantity for spray of slurry is every square metre of support membrane spraying 400g slurry) and to dry at 60 DEG C and make base substrate (4) after 4 hours segmented sintering is carried out to base substrate, first stage rises to 220 DEG C from room temperature and is incubated 150 minutes, the Main Function in this stage removes moisture remaining in base substrate and impurity, ensure that film causes the phenomenon of cracking in later stage sintering process without other undesirable elements, second stage is warming up to 550 DEG C and is incubated 200 minutes, the Main Function in this stage is that the PVB removed in material makes subsequent reactions abundant, the uniformity of proof strength performance, phase III is warming up to 1050 DEG C and is incubated 220 minutes, the Main Function in this stage makes Ni-Cu alloy phase homogenising, during sintering, second stage heating rate is 1 ~ 3 DEG C/min, phase III heating rate 5 ~ 7 DEG C/min, (5) the obtained described porous membrane of cooling after sintering.The thickness of this porous membrane is 0.12mm, average pore size 13 μm, and porosity is 52%, and air permeability is 1490m
3/ m
2hkpa.
Embodiment 4
Embodiment 4 also further comprises step (6) on the basis of embodiment 3, is namely the FeCl of 0.5mol/L by concentration
2solution carries out immersion 45 minutes to porous membrane thus selective on porous membrane 304 stainless steels is dissolved formation three holes, then carries out drying to porous membrane and obtains finished product.The thickness of finally obtained porous membrane is 0.12mm, and average pore size 18 μm, porosity is 72%, and air permeability is 2050m
3/ m
2hkpa.
Embodiment 5
The step preparing porous membrane comprises: (1) adopts Cu net to be support membrane (outsourcing red copper screen cloth), and the thickness of described support membrane is set as 0.2 millimeter, and mesh size is set as 80 orders, (2) by particle diameter be that-400 object Ni powder (purity 99.7%) take ethanol as dispersant, PVB for binding agent by adding 3 grams of PVB in every 100 milliliters of ethanol, the proportional arrangement of 70 grams of Ni powder becomes slurry, (3) described slurry to be sprayed on support membrane (quantity for spray of slurry is every square metre of support membrane spraying 500g slurry) and to dry at 60 DEG C after 4 hours and make base substrate, (4) segmented sintering is carried out to base substrate, first stage rises to 220 DEG C from room temperature and is incubated 150 minutes, the Main Function in this stage removes moisture remaining in base substrate and impurity, ensure that film causes the phenomenon of cracking in later stage sintering process without other undesirable elements, second stage is warming up to 550 DEG C and is incubated 200 minutes, the Main Function in this stage is that the PVB removed in material makes subsequent reactions abundant, the uniformity of proof strength performance, phase III is warming up to 1000 DEG C and is incubated 220 minutes, the Main Function in this stage makes Ni-Cu alloy phase homogenising, during sintering, second stage heating rate is 1 ~ 3 DEG C/min, phase III heating rate 5 ~ 7 DEG C/min, (5) the obtained porous membrane of cooling after sintering.The thickness of this porous membrane is 0.3mm, average pore size 23 μm, and porosity is 45%, and air permeability is 800m
3/ m
2hkpa.
Embodiment 6
Embodiment 6 is identical haply with the porous membrane preparation process of embodiment 5, but difference is: phase III during sintering be warming up to 1000 DEG C after only insulation 120 minutes, thus the Cu element in support membrane is not all reacted with Ni; After this, be the FeCl of 0.5mol/L by concentration
3solution carries out immersion 35 minutes to the porous membrane that step (5) obtains thus selectively on porous membrane Cu is dissolved formation three holes, then carries out drying to porous membrane and obtains finished product.The thickness of finally obtained porous membrane is 0.3mm, and average pore size 25 μm, porosity is 50%, and air permeability is 1000m
3/ m
2hkpa.
Embodiment 7
The step preparing porous membrane comprises: (1) adopts 304 stainless (steel) wires to be support membrane (outsourcing 304 stainless steel mesh), and the thickness of support membrane is set as 0.2 millimeter, and mesh size is set as 80 orders, (2) to be the Ni powder of 3 ~ 5 μm and particle diameter by particle diameter be-400 object Cu powder are 30% be configured to mixed powder by the percentage by weight of Cu, be then dispersant with ethanol, PVB for binding agent by adding 3 grams of PVB in every 100 milliliters of ethanol, the proportional arrangement of 70 grams of mixed powders becomes slurry, (3) described slurry to be sprayed on support membrane (quantity for spray of slurry is every square metre of support membrane spraying 500g slurry) and to dry at 60 DEG C and make base substrate (4) after 4 hours segmented sintering is carried out to base substrate, first stage rises to 220 DEG C from room temperature and is incubated 150 minutes, the Main Function in this stage removes moisture remaining in base substrate and impurity, ensure that film causes the phenomenon of cracking in later stage sintering process without other undesirable elements, second stage is warming up to 550 DEG C and is incubated 200 minutes, the Main Function in this stage is that the PVB removed in material makes subsequent reactions abundant, the uniformity of proof strength performance, phase III is warming up to 1050 DEG C and is incubated 220 minutes, the Main Function in this stage makes Ni-Cu alloy phase homogenising, during sintering, second stage heating rate is 1 ~ 3 DEG C/min, phase III heating rate 5 ~ 7 DEG C/min, (5) the obtained described porous membrane of cooling after sintering.The thickness of this porous membrane is 0.3mm, average pore size 21 μm, and porosity is 44%, and air permeability is 650m
3/ m
2hkpa.
Embodiment 8
Embodiment 8 also further comprises step (6) on the basis of embodiment 7, is namely the FeCl of 0.5mol/L by concentration
2solution carries out immersion 45 minutes to porous membrane thus selective on porous membrane 304 stainless steels is dissolved formation three holes, then carries out drying to porous membrane and obtains finished product.The thickness of finally obtained porous membrane is 0.3mm, and average pore size 24 μm, porosity is 48%, and air permeability is 900m
3/ m
2hkpa.
Claims (10)
1. a porous membrane, thickness is 200 ~ 1500 μm, average pore size is 0.05 ~ 100 μm, porosity is 25 ~ 75%, it is characterized in that: the step of its preparation method comprises: (1) obtains support membrane, described support membrane has cavernous first material, the first material is formed with a hole; (2) slurry is produced, containing pulverous second material in described slurry; (3) described slurry is coated on support membrane then makes base substrate; (4) sinter base substrate, during sintering, the second material id reaction generates cellular the 3rd material and produces the secondary hole with a porosity communication simultaneously; (5) after sintering, cooling obtains porous membrane.
2. porous membrane as claimed in claim 1, it is characterized in that: described support membrane is net type film, its mesh size is 20 ~ 1000 orders.
3. porous membrane as claimed in claim 2, is characterized in that: the mesh size of described support membrane is chosen as 40 ~ 400 orders further.
4. as the porous membrane in claims 1 to 3 as described in any one claim, it is characterized in that: described second material comprises at least two kinds of powders, during described at least two kinds of powder sinterings, formation is the 3rd material of matrix phase by solid solution alloy, in these two kinds of powders, wherein a kind of powder forms the solvent source of this solid solution alloy, another kind of powder forms the solute source of this solid solution alloy, and diffusion pore-creating reaction partially occurs between at least two kinds of powders described in during sintering; Described first material is then a kind of metal material showing as inertia under described sintering condition relative to the second material.
5. porous membrane as claimed in claim 4, is characterized in that: described second material id reaction generates the 3rd material being matrix phase with Ag-Au solid solution, Ti-Zr solid solution, Mg-Cd solid solution, Fe-Cr solid solution, Ni-Cu solid solution, Cu-Al solid solution, Cu-Zn solid solution or Fe-C-Cr solid solution; When described 3rd material is made up of Ni-Cu solid solution, described first Material selec-tion is 304 stainless steels.
6. as the porous membrane in claims 1 to 3 as described in any one claim, it is characterized in that: described slurry is the thick slurry configured by material powder dispersant and binding agent.
7. as the porous membrane in claims 1 to 3 as described in any one claim, it is characterized in that: described preparation method also comprises step (6), namely with etching solution porous membrane soaked thus form three holes after selective the first material dissolves to staying on porous membrane, then drying being carried out to porous membrane and obtain finished product.
8. the preparation method of porous membrane, its step comprises: (1) adopts 304 stainless (steel) wires to be support membrane, and the thickness of described support membrane is set as 0.5 ~ 1 millimeter, and mesh size is set as 60 ~ 400 orders; (2) to be the Ni powder of 3 ~ 5 μm and particle diameter by particle diameter be-400 object Cu powder are 20 ~ 40% be configured to mixed powder by the percentage by weight of Cu, be then dispersant with ethanol, PVB for binding agent by adding 2 ~ 5 grams of PVB in every 100 milliliters of ethanol, the proportional arrangement of 50 ~ 100 grams of mixed powders becomes slurry; (3) described slurry to be coated on support membrane and to dry and make base substrate; (4) segmented sintering is carried out to base substrate, first stage rises to 120 ~ 250 DEG C from room temperature and is incubated 120 ~ 180 minutes, second stage is warming up to 500 ~ 600 DEG C and is incubated 60 ~ 240 minutes, and the phase III is warming up to 900 ~ 1090 DEG C and is incubated 90 ~ 240 minutes; (5) the obtained described porous membrane of cooling after sintering.
9. method as claimed in claim 8, is characterized in that: second stage heating rate≤5 DEG C/min during sintering, phase III heating rate≤10 DEG C/min.
10. as claimed in claim 8 or 9 method, is characterized in that: also comprise step (6), is namely the FeCl of 0.4 ~ 0.8mol/L by concentration
2solution carries out immersion 30 ~ 60 minutes to porous membrane thus selective on porous membrane 304 stainless steels is dissolved formation three holes, then carries out drying to porous membrane and obtains finished product.
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Cited By (9)
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| CN105854633A (en) * | 2016-05-27 | 2016-08-17 | 成都易态科技有限公司 | Porous film and preparation method thereof |
| CN105854629A (en) * | 2016-03-23 | 2016-08-17 | 成都易态科技有限公司 | Porous film and preparation method thereof |
| CN107486024A (en) * | 2017-06-22 | 2017-12-19 | 成都易态科技有限公司 | The manufacture method of sintered porous filtration membrane |
| CN107914015A (en) * | 2016-10-09 | 2018-04-17 | 成都易态科技有限公司 | Prepare the sintering method of porous membrane |
| CN108249947A (en) * | 2018-03-12 | 2018-07-06 | 成都易态科技有限公司 | The preparation method of porous membrane green body and preparation method thereof and porous membrane |
| WO2019009672A1 (en) * | 2017-07-06 | 2019-01-10 | 주식회사 엘지화학 | Method for preparing metal foam |
| CN114289720A (en) * | 2021-11-30 | 2022-04-08 | 成都易态科技有限公司 | Method for preparing green body and sintered porous metal film and dust removing method |
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| CN105435536A (en) * | 2015-12-02 | 2016-03-30 | 成都易态科技有限公司 | Denitration catalysis membrane filtering material and preparation method thereof |
| CN105854629A (en) * | 2016-03-23 | 2016-08-17 | 成都易态科技有限公司 | Porous film and preparation method thereof |
| CN105854633A (en) * | 2016-05-27 | 2016-08-17 | 成都易态科技有限公司 | Porous film and preparation method thereof |
| CN107914015A (en) * | 2016-10-09 | 2018-04-17 | 成都易态科技有限公司 | Prepare the sintering method of porous membrane |
| CN107914015B (en) * | 2016-10-09 | 2020-08-18 | 成都易态科技有限公司 | Sintering method for preparing porous film |
| CN107486024A (en) * | 2017-06-22 | 2017-12-19 | 成都易态科技有限公司 | The manufacture method of sintered porous filtration membrane |
| WO2019009672A1 (en) * | 2017-07-06 | 2019-01-10 | 주식회사 엘지화학 | Method for preparing metal foam |
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| CN108249947A (en) * | 2018-03-12 | 2018-07-06 | 成都易态科技有限公司 | The preparation method of porous membrane green body and preparation method thereof and porous membrane |
| CN114289720A (en) * | 2021-11-30 | 2022-04-08 | 成都易态科技有限公司 | Method for preparing green body and sintered porous metal film and dust removing method |
| CN114523108A (en) * | 2021-11-30 | 2022-05-24 | 成都易态科技有限公司 | Green body, sintered porous metal film and dust removal method |
| 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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