CN107051223B - Preparation method of ceramic composite membrane - Google Patents
Preparation method of ceramic composite membrane Download PDFInfo
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- CN107051223B CN107051223B CN201710314515.2A CN201710314515A CN107051223B CN 107051223 B CN107051223 B CN 107051223B CN 201710314515 A CN201710314515 A CN 201710314515A CN 107051223 B CN107051223 B CN 107051223B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D67/0039—Inorganic membrane manufacture
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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Abstract
A preparation method of a high-stability ceramic composite membrane comprises the steps of firstly adding 1/2-2/3 ceramic powder with the particle size of the average pore diameter of the surface of a support body into an organic solvent or water, adding a dispersing agent and a thickening agent to prepare stable and uniformly dispersed metal particle suspension slurry, then putting a porous ceramic support body into the ceramic particle suspension slurry to carry out suction negative pressure slurry dipping adsorption, enabling ceramic particles to enter pore channels on the surface of the ceramic support body, and filling the pore channels on the surface of the ceramic support body. And repeating the above steps for 1-5 times, wherein the particle size of the ceramic particles used in each time is 1/2-2/3 of the particle size of the ceramic particles used in the previous time. And finally, cleaning the surface of the modified ceramic support body, and then placing the ceramic support body in a muffle furnace for sintering treatment to generate a mixed ceramic film layer containing ceramic oxide.
Description
Technical Field
The invention relates to a preparation technology of a ceramic composite membrane.
Background
The membrane has the characteristics of small occupied area, high separation efficiency, no pollution to the environment and the like, and is widely applied to the fields of chemical industry, biology, medicine, energy, environment, metallurgy and the like. The ceramic membrane is widely applied due to uniform pore size distribution, high mechanical strength, and good acid and alkali resistance and corrosion resistance. The traditional nanofiltration membrane is prepared by sequentially and repeatedly preparing a plurality of ceramic membranes with the particle sizes from large to small on the surface of a macroporous support body, and sintering is carried out for each ceramic membrane, so that the preparation period is long, the energy consumption is high, and the binding force between the membranes is poor. The method has simple process and low energy consumption, and disperses the nano-film into the pores of the macroporous support body, and the damage of the performance of individual film has little influence on the performance of the whole film. Secondly, the problem of poor bonding force between the film layers is effectively avoided.
Disclosure of Invention
The invention aims to provide a preparation method of a ceramic composite membrane.
The invention relates to a preparation method of a ceramic composite membrane, which comprises the following steps:
(1) selecting ceramic particles with the particle size of 1/2-2/3 of the average surface pore size of the porous ceramic support, adding 0.05-20 percent of the ceramic particles into an organic solvent or water by weight percent based on the mass of the solvent or water, and sequentially adding 0.1-5 percent of a dispersing agent and 1-5 percent of a thickening agent by weight percent based on the mass of the solvent or water to prepare uniformly dispersed and stable ceramic particle suspension slurry.
(2) Immersing the cleaned porous ceramic support body into the slurry prepared in the step (1), and adsorbing ceramic particles in the slurry in a pore channel on the surface of the porous ceramic support body by adopting a negative pressure pumping method; the negative pressure is 0.01-0.1MPa, the slurry soaking time is 10-300s, and the redundant ceramic particles attached to the surface are cleaned after slurry soaking.
(3) Repeating the processes (1) and (2) for 1-5 times, wherein the grain diameter of the ceramic particles used in each time is 1/2-2/3 of the grain diameter of the ceramic particles used in the last time.
(4) And (4) placing the support body filled with the ceramic powder in the step (3) into a muffle furnace, and sintering at the temperature of 400-900 ℃ for 1-20 hours to generate the ceramic composite film layer.
The invention has the advantages that: compared with the traditional film preparation method, the invention has simple film preparation process and easy operation. The method only needs one-time sintering, has low energy consumption, and effectively solves the problem of high energy consumption caused by repeated slurry soaking and repeated sintering in the traditional film preparation process. The method of the invention is used for preparing the membrane in the membrane hole, the prepared membrane has better stability, and the problem of poor binding force between membrane layers in the traditional membrane preparing process is effectively avoided.
Drawings
FIG. 1 is a schematic diagram comparing the preparation process flow of the present invention with a conventional in-situ oxidation flow, and FIG. 2 is a SEM photograph of the surface of a ceramic support without high temperature oxidation.
Detailed Description
As shown in figure 1, the invention relates to a preparation method of a ceramic composite membrane, which comprises the following steps:
(1) selecting ceramic particles with the particle size of 1/2-2/3 of the average surface pore diameter of the porous ceramic support body, adding the ceramic particles into an organic solvent or water according to the weight percentage of 0.05-20% by taking the mass of the solvent or water as a reference, and sequentially adding 0.1-5% of a dispersing agent and 1-5% of a thickening agent according to the mass percentage of the solvent or water as a reference to prepare uniformly dispersed and stable ceramic particle suspension slurry;
(2) immersing the cleaned porous ceramic support body into the slurry prepared in the step (1), and adsorbing ceramic particles in the slurry in a pore channel on the surface of the porous ceramic support body by adopting a negative pressure pumping method; the pumped negative pressure is 0.01-0.1MPa, the slurry soaking time is 10-300s, and redundant ceramic particles attached to the surface are cleaned after slurry soaking;
(3) repeating the processes of the step (1) and the step (2) for 1-5 times, wherein the grain size of the ceramic particles used each time is 1/2-2/3 of the grain size of the ceramic particles used last time;
(4) and (4) placing the support body filled with the ceramic powder in the step (3) into a muffle furnace, and sintering at the temperature of 400-900 ℃ for 1-20 hours to generate the ceramic composite film layer.
The ceramic particles in the preparation method are titanium dioxide powder, aluminum oxide, zirconia powder, silicon dioxide or a mixture of two ceramic powders; the ceramic particles with the particle size of 1/2-2/3 on the average surface pore size of the porous ceramic support are selected, and the adding amount is 0.05-20% by weight based on the mass of the used solvent or water.
The organic solvent in the preparation method is methanol, ethanol or isopropanol or a mixture of two or three of the methanol, the ethanol and the isopropanol.
The dispersant is polyethylene, or polymethacrylic acid, or polyacrylamide, or hexadecyl trimethyl quaternary ammonium salt, or sodium dodecyl sulfate, or sodium dodecyl benzene sulfonate, or polyethylene glycol, or a mixture of two or three of the above; the addition amount is 0.1-5% by mass based on the mass of the solvent or water; the thickening agent is methyl cellulose, or ethyl cellulose, or polyvinyl alcohol, or polypropylene formate, or sodium carboxymethyl cellulose, or a mixture of two or three of the two; the addition amount is 1-5% by mass based on the mass of the solvent or water.
The porous ceramic support body in the preparation method is alumina ceramic, or silicon oxide ceramic, or titanium oxide ceramic, or zirconium oxide ceramic, or mixed ceramic of two or more of the above; the pore diameter range is 1-15 μm.
The negative pressure pumping range of the preparation method is 0.01-0.1MPa, and the slurry soaking time is 10-300 s.
The sintering temperature of the preparation method is 400-900 ℃, and the sintering time is 1-20 hours.
EXAMPLE 1 porosity α -Al2O3The sheet ceramic is a support and has a pore diameter of 3 μm.
(1) Taking water as a solvent, and adding 1.7 mu m TiO in the mass percentages of 2%, 0.5% and 1% respectively based on the mass of the water2The composite material comprises particles, polyethyleneimine, a mixture of ethyl cellulose and sodium carboxymethyl cellulose (1: 1 wt), wherein the polyethyleneimine is a dispersant, and the mixture of ethyl cellulose and sodium carboxymethyl cellulose (1: 1 wt) is a thickening agent;
(2) immersing the cleaned porous ceramic support body into the slurry prepared in the step (1), and adopting a negative pressure pumping method to carry out TiO extraction on the slurry2Particles adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.03MPa, the slurry soaking time is 40s, and redundant Ti particles attached to the surface are cleaned off after the slurry is soaked;
(3) selecting TiO with particle size of 1.1 μm2Repeating the step (1), putting the ceramic support body containing the Ti particles in the step (2) into the prepared slurry for negative pressure slurry dipping adsorption, and adsorbing the Ti particles in the slurry in the pore channels on the surface of the porous ceramic support body; the negative pressure is 0.02MPa, the slurry soaking time is 60s, and the redundant TiO attached to the surface is cleaned off after slurry soaking2Particles;
(4) TiO with the grain diameter of 0.5 mu m is selected again2Repeating the step (1) to obtain particles containing TiO with two particle sizes in the step (3)2Putting the ceramic support body of the particles into the prepared slurry for negative pressure slurry pumping and adsorption, and then TiO in the slurry is adsorbed2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.01MPa, the slurry soaking time is 100s, and the redundant TiO attached to the surface is cleaned off after slurry soaking2Particles；
(5) And (5) placing the assembly prepared in the step (4) into a muffle furnace for sintering treatment, wherein the sintering temperature is 500 ℃, and the sintering time is 8 hours. Wherein the temperature rising and falling speed is 1 ℃/min. Successfully prepares the ceramic membrane with compact surface.
Example 2: porous tubular titanium oxide ceramic is used as a support body, and the pore diameter of the porous tubular titanium oxide ceramic is 8 mu m.
(1) Taking absolute ethyl alcohol as a solvent, and respectively adding 10 percent, 2 percent and 3 percent of Al with the mass of 7.3 mu m by taking the mass of the absolute ethyl alcohol as a reference2O3The preparation method comprises the following steps of (1) mixing particles, polyethylene glycol, ethyl cellulose and polyvinyl alcohol (1: 1 wt), wherein polyethyleneimine is used as a dispersing agent, and a mixture of ethyl cellulose and sodium carboxymethyl cellulose (1: 1 wt) is used as a thickening agent;
(2) immersing the cleaned porous ceramic support body into the slurry prepared in the step (1), and pumping negative pressure to remove Al in the slurry2O3Particles adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.1MPa, the slurry soaking time is 80s, and the excessive Al attached to the surface is cleaned off after the slurry soaking2O3Particles;
(3) selecting Al with a particle size of 3.5 μm2O3Repeating the step (1) to add Al to the particles obtained in the step (2)2O3Putting the ceramic support body of the particles into the prepared slurry for negative pressure slurry pumping and adsorption, and carrying out Al adsorption on the slurry2O3The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.06MPa, the slurry soaking time is 100s, and the excessive Al attached to the surface is cleaned off after the slurry soaking2O3Particles;
(4) al having a grain size of 1.7 μm is selected again2O3Repeating the step (1) to obtain particles, wherein the step (3) contains Al with two particle sizes2O3Putting the ceramic support body of the particles into the prepared slurry for negative pressure slurry pumping and adsorption, and carrying out Al adsorption on the slurry2O3The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.03MPa, the time for soaking is 150s, and the surplus attached to the surface is cleaned off after soakingAl of (2)2O3Particles;
(5) and (5) placing the assembly prepared in the step (4) into a muffle furnace for sintering treatment, wherein the sintering temperature is 650 ℃, and the sintering time is 6 hours. Wherein the temperature rising and falling speed is 1 ℃/min. Successfully prepares the ceramic membrane with compact surface.
Example 3-porous α -Al2O3The plate-like ceramic was a support having an average pore diameter of 14 μm.
(1) Taking isopropanol as a solvent, and respectively adding a mixture of 8.9 mu m zirconium oxide particles, polyethyleneimine, ethyl cellulose and sodium carboxymethylcellulose (1: 1 wt) in mass percent of 19%, 5% and 5% based on the mass of the isopropanol, wherein the polyethyleneimine is used as a dispersing agent, and the mixture of the ethyl cellulose and the sodium carboxymethylcellulose (1: 1 wt) is used as a thickening agent;
(2) immersing the cleaned porous ceramic support body into the slurry prepared in the step (1), and adsorbing the zirconium oxide particles in the slurry in the pore channels on the surface of the porous ceramic support body by adopting a negative pressure pumping method; the negative pressure is 0.3MPa, the slurry soaking time is 150s, and redundant zirconium oxide particles attached to the surface are cleaned after slurry soaking;
(3) selecting zirconia particles with the particle size of 5.8 microns, repeating the step (1), putting the ceramic support body containing the zirconia particles in the step (2) into prepared slurry for suction negative pressure slurry dipping adsorption, adsorbing the zirconia particles in the slurry into pore channels on the surface of the porous ceramic support body, wherein the suction negative pressure is 0.15MPa, the slurry dipping time is 200s, and cleaning off the redundant zirconia particles attached to the surface after slurry dipping;
(4) selecting zirconia particles with the particle size of 3.5 microns again, repeating the step (1), putting the ceramic support body containing the zirconia particles with the two particle sizes in the step (3) into prepared slurry for suction negative pressure slurry dipping adsorption, and adsorbing the zirconia particles in the slurry into pore channels on the surface of the porous ceramic support body; the negative pressure is 0.1MPa, the slurry soaking time is 250s, and redundant zirconium oxide particles attached to the surface are cleaned after slurry soaking;
(5) and (5) placing the assembly prepared in the step (4) into a muffle furnace for sintering treatment, wherein the sintering temperature is 650 ℃, and the sintering time is 5 hours. Wherein the temperature rising and falling speed is 1 ℃/min. Successfully prepares the ceramic membrane with compact surface.
Example 4-porous α -Al2O3The ceramic sheet is a support and has an average pore diameter of 3 μm.
(1) Taking absolute ethyl alcohol as a solvent, and respectively adding 1.7 mu m SiO with the mass percent of 2 percent, 0.5 percent and 1 percent based on the mass of the absolute ethyl alcohol2The preparation method comprises the following steps of (1) mixing particles, polyethylene glycol, ethyl cellulose and polyvinyl alcohol (1: 1 wt), wherein polyethyleneimine is used as a dispersing agent, and a mixture of ethyl cellulose and sodium carboxymethyl cellulose (1: 1 wt) is used as a thickening agent;
(2) immersing the cleaned porous ceramic support body into the slurry prepared in the step (1), and adopting a negative pressure pumping method to enable SiO in the slurry to be in a negative pressure state2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.03MPa, the slurry soaking time is 100s, and the excessive SiO attached to the surface is cleaned off after the slurry soaking2Particles;
(3) selecting Al particles with a particle size of 1.1 μm, repeating step (1), and adding SiO into step (2)2Putting the ceramic support body of the particles into the prepared slurry for negative pressure slurry pumping and adsorption, and then, adding SiO in the slurry2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.02MPa, the slurry soaking time is 70s, and the redundant SiO attached to the surface is cleaned off after the slurry is soaked2Particles;
(4) selecting SiO with particle size of 500nm again2Repeating the step (1) to obtain particles, wherein the SiO with two particle sizes is contained in the step (3)2Putting the ceramic support body of the particles into the prepared slurry for negative pressure slurry pumping and adsorption, and then, adding SiO in the slurry2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.01MPa, the slurry soaking time is 50s, and the excessive SiO attached to the surface is cleaned off after the slurry soaking2Particles;
(5) and (5) placing the assembly prepared in the step (4) into a muffle furnace for sintering treatment, wherein the sintering temperature is 500 ℃, and the sintering time is 8 hours. Wherein the temperature rising and falling speed is 1 ℃/min. Successfully prepares the ceramic membrane with compact surface.
Example 5: the tubular titanium oxide ceramic was used as a support, and the average pore diameter was 8 μm.
(1) Adding 10 percent, 2 percent and 3 percent of SiO with the mass percentage of 7.3 mu m respectively by taking isopropanol as a solvent and taking the mass of the isopropanol as a reference2The composite material comprises particles, polyethyleneimine, a mixture of ethyl cellulose and sodium carboxymethyl cellulose (1: 1 wt), wherein the polyethyleneimine is a dispersant, and the mixture of ethyl cellulose and sodium carboxymethyl cellulose (1: 1 wt) is a thickening agent;
(2) immersing the cleaned porous ceramic support body into the slurry prepared in the step (1), and adopting a negative pressure pumping method to enable SiO in the slurry to be in a negative pressure state2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.15MPa, the slurry soaking time is 100s, and the redundant SiO attached to the surface is cleaned off after the slurry is soaked2Particles;
(3) SiO with a particle size of 3.5 μm is selected2Repeating the step (1) to obtain particles containing SiO in the step (2)2Putting the ceramic support body of the particles into the prepared slurry for negative pressure slurry pumping and adsorption, and then, adding SiO in the slurry2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.07MPa, the slurry soaking time is 150s, and the excessive SiO attached to the surface is cleaned off after the slurry soaking2Particles;
(4) SiO with a grain size of 1.7 μm is selected again2Repeating the step (1) to obtain particles, wherein the SiO with two particle sizes is contained in the step (3)2Putting the ceramic support body of the particles into the prepared slurry for negative pressure slurry pumping and adsorption, and then, adding SiO in the slurry2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.05MPa, the slurry soaking time is 200s, and the excessive SiO attached to the surface is cleaned off after the slurry soaking2Particles;
(5) and (5) placing the assembly prepared in the step (4) into a muffle furnace for sintering treatment, wherein the sintering temperature is 700 ℃, and the sintering time is 6 hours. Wherein the temperature rising and falling speed is 1 ℃/min. Successfully prepares the ceramic membrane with compact surface.
Example 6: the tubular zirconia ceramic was used as a support, and the average pore diameter was 14 μm.
(1) Using water as a solvent, and adding TiO 8.9 μm in an amount of 19 wt%, 5 wt% and 5 wt% based on the mass of water2Particle particles (1: 1 wt), polyethyleneimine, a mixture of ethyl cellulose and sodium carboxymethyl cellulose (1: 1 wt), wherein the polyethyleneimine is a dispersant, and the mixture of ethyl cellulose and sodium carboxymethyl cellulose (1: 1 wt) is a thickening agent;
(2) immersing the cleaned porous ceramic support body into the slurry prepared in the step (1), and adopting a negative pressure pumping method to carry out TiO extraction on the slurry2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.28MPa, the slurry soaking time is 150s, and the redundant TiO attached to the surface is cleaned off after slurry soaking2Particles;
(3) TiO with a particle size of 5.8 mu m is selected2Repeating the step (1) to obtain particles containing TiO in the step (2)2Putting the ceramic support body of the particles into the prepared slurry for negative pressure slurry pumping and adsorption, and then TiO in the slurry is adsorbed2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.2MPa, the slurry soaking time is 200s, and the redundant TiO attached to the surface is cleaned off after slurry soaking2Particles;
(4) TiO with the grain diameter of 3.5 mu m is selected again2Repeating the step (1) to obtain particles containing TiO with two particle sizes in the step (3)2Putting the ceramic support body of the particles into the prepared slurry for negative pressure slurry pumping and adsorption, and then TiO in the slurry is adsorbed2The particles are adsorbed in the pore channels on the surface of the porous ceramic support; the negative pressure is 0.1MPa, the slurry soaking time is 250s, and the redundant TiO attached to the surface is cleaned off after slurry soaking2Particles;
(5) and (5) placing the assembly prepared in the step (4) into a muffle furnace for sintering treatment, wherein the sintering temperature is 800 ℃, and the sintering time is 5 hours. Wherein the temperature rising and falling speed is 1 ℃/min. Successfully prepares the ceramic membrane with compact surface.
Claims (1)
1. A preparation method of a ceramic composite membrane is characterized by comprising the following steps:
(1) selecting ceramic particles with the particle size of 1/2-2/3 of the average surface pore diameter of the porous ceramic support body, adding the ceramic particles into an organic solvent or water according to the weight percentage of 0.05-20% by taking the mass of the organic solvent or water as a reference, and sequentially adding a dispersing agent and a thickening agent according to the mass percentage of 0.1-5% and 1-5% by taking the mass of the organic solvent or water as a reference to prepare uniformly dispersed and stable ceramic particle suspension slurry;
(2) immersing the cleaned porous ceramic support body into the slurry prepared in the step (1), and adsorbing ceramic particles in the slurry in a pore channel on the surface of the porous ceramic support body by adopting a negative pressure pumping method; the pumped negative pressure is 0.01-0.1MPa, the slurry soaking time is 10-300s, and redundant ceramic particles attached to the surface are cleaned after slurry soaking;
(3) repeating the processes of the step (1) and the step (2) for 1-5 times, wherein the grain size of the ceramic particles used each time is 1/2-2/3 of the grain size of the ceramic particles used last time;
(4) placing the support body filled with the ceramic particles in the step (3) into a muffle furnace, and sintering at the temperature of 400-900 ℃ for 1-20 hours to generate a ceramic composite film layer;
the ceramic particles are titanium dioxide powder, aluminum oxide, zirconia powder, silicon dioxide or a mixture of the two ceramic particles; ceramic particles with the particle size of 1/2-2/3 of the average surface pore size of the porous ceramic support are selected, the addition amount is 0.05-20 percent by weight based on the mass of the used organic solvent or water;
the organic solvent is methanol, ethanol or isopropanol or a mixture of two or three of the methanol, the ethanol and the isopropanol;
the dispersing agent is polyethylene, or polymethacrylic acid, or polyacrylamide, or hexadecyl trimethyl quaternary ammonium salt, or sodium dodecyl sulfate, or sodium dodecyl benzene sulfonate, or polyethylene glycol, or a mixture of two or three of the polyethylene, the polymethacrylic acid, the polyacrylamide, or the hexadecyl trimethyl quaternary ammonium salt; the addition amount is 0.1-5% by mass based on the mass of the organic solvent or water; the thickening agent is methyl cellulose, or ethyl cellulose, or polyvinyl alcohol, or polypropylene formate, or sodium carboxymethyl cellulose, or a mixture of two or three of the two; the addition amount is 1-5% by mass based on the mass of the organic solvent or water;
the porous ceramic support is alumina ceramic, or silicon oxide ceramic, or titanium oxide ceramic, or zirconium oxide ceramic, or a mixed ceramic of two or more; the pore diameter range is 1-15 μm;
the negative pressure range is 0.01-0.1MPa, and the slurry soaking time is 10-300 s;
the sintering temperature is 400-900 ℃, and the sintering time is 1-20 hours.
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| CN101985084A (en) * | 2010-11-18 | 2011-03-16 | 南京工业大学 | Preparation method of ceramic Ti-Al alloy composite membrane |
| CN104099557A (en) * | 2014-07-21 | 2014-10-15 | 兰州理工大学 | Preparation method of zero-defect porous ceramic/Ti-Al alloy composite membrane |
| CN105854633A (en) * | 2016-05-27 | 2016-08-17 | 成都易态科技有限公司 | Porous film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101985084A (en) * | 2010-11-18 | 2011-03-16 | 南京工业大学 | Preparation method of ceramic Ti-Al alloy composite membrane |
| CN104099557A (en) * | 2014-07-21 | 2014-10-15 | 兰州理工大学 | Preparation method of zero-defect porous ceramic/Ti-Al alloy composite membrane |
| CN105854633A (en) * | 2016-05-27 | 2016-08-17 | 成都易态科技有限公司 | Porous film and preparation method thereof |
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