CN108147793A - A kind of preparation method of gradient porous ceramics film - Google Patents
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Abstract
The invention discloses a kind of preparation methods of gradient porous ceramics film, include the following steps：(1) suspension slurry of the ceramic powder of grain size consecutive variations is prepared；(2) pending porous matrix is placed in slurry bottom, gradient film is obtained in matrix surface using different-grain diameter powder rate of settling difference；(3) gradient film is heat-treated and is sintered, finally obtain gradient porous ceramics film.Porous ceramics Gradient Film prepared by this method has continuous pore-size distribution gradient, farthest reduces in sintering process caused by different parts shrinking percentage difference the defects of film peeling, while transition subtracts aperture layer and micro-filtration active separating layer one-pass film-forming, simple for process.
Description
Technical field
The present invention relates to a kind of preparation methods of gradient porous ceramics film, belong to inorganic material film and application field.
Background technology
Using porous material as matrix, one layer of porous ceramics coating is prepared on surface as microfiltration membranes, this composite membrane is being cured
Medicine industry, food industry, paint industry and biotechnological industries etc. fields have a wide range of applications.Improve the hole of basis material
Degree can improve the flux of pending gas or liquid, improve the working efficiency of device, but larger surface apertures also give aperture
The preparation of diameter micro-filtration active separating layer brings difficulty.The way generally used industrial at present is more using ceramic material preparation
Hole transition zone carries out matrix to subtract hole processing, finally obtains the ceramic micro filter active separating layer in required aperture.
In recent years, carry out subtracting the technology in hole to porous supporting body material by extensive pass using multistage porous ceramic layer
Note.CN201210180930.0 discloses a kind of preparation method of ceramic film with hierarchical pore structure, chooses the original of different-grain diameter respectively
Feed powder end and the pore creating material of different acid-base property and grain size, using dip-coating technique by the granularity and its acid-base property of pore creating material
Different films successively.Realize that aperture is controllable and is distributed multi-stage porous with gradient by the variation of powder and pore creating material granularity
The preparation of the ceramic membrane of structure.This method can preferably control thickness, porosity and the aperture of seperation film, but be related to thin
The slightly aobvious complexity of the multiple coating processes of film, and still have certain aperture span between every layer of transition zone, in sintering process by
Defect is easily formed in the difference of percent thermal shrinkage.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of gradient porous ceramics film, can be porous using this method
The porous ceramic film with continuous bore diameter gradient distribution is obtained on matrix, farthest reduces different parts in sintering process
Caused by shrinking percentage difference the defects of film peeling.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of gradient porous ceramics film, includes the following steps：
(1) suspension slurry of the ceramic powder of grain size consecutive variations is prepared；
(2) pending porous matrix is placed in slurry bottom, using different-grain diameter powder rate of settling difference in matrix table
Face obtains gradient film；
(3) it is heat-treated and is sintered, finally obtain gradient porous ceramics film.
In the step (1), in the suspension slurry of preparation ceramic powder account for the volume ratio of suspension for 1%~
80%.Solvent used in formulated suspension slurry is methanol, ethyl alcohol, acetone, terpinol, isopropanol, chloroform, water, benzene, chlorobenzene,
One or more of petroleum ether, carbon tetrachloride, ethyl acetate, the binding agent added in for methylcellulose, ethyl cellulose,
One or more of polytetrafluoroethylene (PTFE), PVDF, PVA, PVB, gum arabic, surfactant used for PEI, CTAB,
One or more of lauryl sodium sulfate, benzene sulfonic acid sodium salt.
In the step (2), the difference of the ceramic powder rate of settling is formed by the method for centrifugation or gravitational settling.
In the step (3), the temperature and condition of heat treatment depend on the type of organic additive used, selected ceramics
The tolerable temperature of the sintering condition of powder body material and selected porous matrix, preferably between 900-1200 DEG C.
The ceramic material is Al2O3、Cr2O3、TiO2、CuO、MgO、ZnO、SiO2、ZrO2, one or more of YSZ.
The porous matrix is flake porous metal or porous ceramics, and surface maximum diameter of hole is less than 50 μm.
The particle size range of the ceramic material is between 20nm to 50 μm, and the D90 of powder is between the 1/ of substrate surface aperture
Between 50 to 1/5, span is that (D90-D10)/D50 is more than 1.
The thickness of the gradient porous ceramics film is 100-250 μm.
The beneficial effects of the invention are as follows：
Gradient porous ceramics film prepared by the method for the present invention has continuous pore-size distribution gradient, can be farthest
In reduction sintering process the quality of coating, while transition are improved the defects of film peeling caused by different parts shrinking percentage difference
Subtract aperture layer and micro-filtration active separating layer one-pass film-forming, it is simple for process.
Description of the drawings
Fig. 1 is the structure diagram of gradient porous ceramics film.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and embodiments, but the invention is not limited in following implementations
Example.
As shown in Figure 1, method using the present invention can obtain the gradient porous ceramics film being deposited on porous matrix 12.
Gradient porous ceramics film 2 has continuous pore-size distribution gradient.
Embodiment 1
Porous Al is prepared on porous NiCrAl alloy sheets2O3Gradient film, wherein NiCrAl alloy sheets surface maximum diameter of hole are about
15 μm, step is as follows：
(1) α phases Al is selected2O3Powder (particle diameter distribution D10=150nm, D50=1.6 μm, D90=2.7 μm) is prepared
Al2O3The suspension slurry of powder.2g gum arabics are dissolved in 80mL absolute ethyl alcohols in 20mL terpinols, adding in Al2O3Powder
Body 100g, is sufficiently stirred.
(2) dried porous NiCrAl alloy sheets will be cleaned by ultrasonic through acetone and be placed in slurry bottom, stand 48h, utilized
Different-grain diameter powder rate of settling difference obtains gradient film in matrix surface.
(3) 30min is heat-treated in 500 DEG C of air atmospheres, then 1h, warming and cooling rate are sintered under 1000 DEG C of vacuum conditions
For 1 DEG C/min, porous Al is finally obtained2O3Gradient film.
Obtained porous Al2O3About 70 μm of gradient film thickness, surface maximum diameter of hole are less than 1 μm, and film is uniform, with reference to
Power is good.
Embodiment 2
Porous stainless steel on piece prepares porous TiO2Gradient film, wherein about 50 μm of porous stainless steel surface maximum diameter of hole,
Step is as follows：
(1) rutile TiO is selected2Powder (particle diameter distribution D10=600nm, D50=3 μm, D90=4.5 μm) is prepared
TiO2The suspension slurry of powder.5g PVB are dissolved in 100mL absolute ethyl alcohols, add in PEI 1g, add in TiO2Powder 40g, fills
Divide stirring.
(2) dried porous stainless steel disc will be cleaned by ultrasonic through acetone and be placed in slurry bottom, stand for 24 hours, utilize difference
Grain size powder rate of settling difference obtains gradient film in matrix surface.
(3) 30min is heat-treated in 300 DEG C of air atmospheres, then 2h, warming and cooling rate are sintered under 1000 DEG C of hydrogen atmospheres
For 1 DEG C/min, porous TiO is finally obtained2Gradient film.
Obtained porous TiO2About 20 μm of gradient film thickness, surface maximum diameter of hole are less than 2 μm, and film is uniform, with reference to
Power is good.
Embodiment 3
Woelm Alumina on piece prepares porous YSZ gradient films, wherein about 1 μm of porous oxidation aluminium flake surface maximum diameter of hole,
Step is as follows：
(1) YSZ powders (particle diameter distribution D10=40nm, D50=110nm, D90=180nm) is selected to prepare YSZ powders
Suspension slurry.1gPVA is dissolved in 100mL deionized waters, adds in benzene sulfonic acid sodium salt 0.5g, YSZ powder 2g is added in, fully stirs
It mixes.
(2) dried porous oxidation aluminium flake will be cleaned by ultrasonic through acetone and be placed in slurry bottom, 72h is stood, utilize difference
Grain size powder rate of settling difference obtains gradient film in matrix surface.
(3) 2h is sintered under 1200 DEG C of air atmospheres, warming and cooling rate is 1 DEG C/min, finally obtains porous ceramics gradient
Film layer.
Obtained about 2 μm of porous YSZ gradient films thickness, surface maximum diameter of hole are less than 500nm, and film is uniform, with reference to
Power is good.
Embodiment 4
Porous YSZ on pieces prepare porous SiO2Gradient film, wherein porous YSZ pieces surface maximum diameter of hole about 500nm, step
It is as follows：
(1) SiO is selected2Powder (particle diameter distribution D10=20nm, D50=40nm, D90=70nm) prepares SiO2Powder
Suspension slurry.1g methylcellulose is dissolved in 100mL deionized waters, adds in CTAB 0.1g, adds in SiO2Powder 1g, fills
Divide stirring.
(2) dried porous YSZ pieces will be cleaned by ultrasonic through acetone and be placed in slurry bottom, 72h is stood, utilize different-grain diameter
Powder rate of settling difference obtains gradient film in matrix surface.
(3) 1h is sintered under 600 DEG C of air atmospheres, warming and cooling rate is 1 DEG C/min, finally obtains porous ceramics Gradient Film
Layer.
Obtained porous SiO2About 1 μm of gradient film thickness, surface maximum diameter of hole are less than 200nm, and film is uniform, with reference to
Power is good.
Claims (9)
1. a kind of preparation method of gradient porous ceramics film, which is characterized in that include the following steps：
(1) suspension slurry of the ceramic powder of grain size consecutive variations is prepared；
(2) pending porous matrix is placed in slurry bottom, is obtained using different-grain diameter powder rate of settling difference in matrix surface
Obtain gradient film；
(3) gradient film is heat-treated and is sintered, finally obtain gradient porous ceramics film.
2. the preparation method of gradient porous ceramics film according to claim 1, which is characterized in that in the step (1),
The volume ratio that ceramic powder accounts for suspension in the suspension slurry of preparation is 1%~80%.
3. the preparation method of gradient porous ceramics film according to claim 1, which is characterized in that in the step (1),
Solvent used in formulated suspension slurry is methanol, ethyl alcohol, acetone, terpinol, isopropanol, chloroform, water, benzene, chlorobenzene, oil
One or more of ether, carbon tetrachloride, ethyl acetate；The binding agent added in is methylcellulose, ethyl cellulose, poly- four
One or more of vinyl fluoride, PVDF, PVA, PVB, gum arabic；Surfactant used is PEI, CTAB, 12
One or more of sodium alkyl sulfate, benzene sulfonic acid sodium salt.
4. the preparation method of gradient porous ceramics film according to claim 1, which is characterized in that in the step (2),
The difference of the ceramic powder rate of settling is formed by the method for centrifugation or gravitational settling.
5. the preparation method of gradient porous ceramics film according to claim 1, which is characterized in that in the step (3),
The temperature and condition of heat treatment depend on the type of organic additive used, the sintering condition of selected ceramic powder material and institute
The tolerable temperature of porous matrix is selected, between 900-1200 DEG C.
6. the preparation method of gradient porous ceramics film according to claim 1, which is characterized in that the porous matrix is piece
Shape porous metals or porous ceramics, surface maximum diameter of hole are less than 50 μm.
7. the preparation method of gradient porous ceramics film according to claim 1, which is characterized in that the ceramic material is
Al2O3、Cr2O3、TiO2、CuO、MgO、ZnO、SiO2、ZrO2, one or more of YSZ.
8. the preparation method of gradient porous ceramics film according to claim 1, which is characterized in that the grain of the ceramic material
Diameter range is between 20nm to 50 μm, and for the D90 of powder between 1/50 to the 1/5 of substrate surface aperture, span is (D90-
D10)/D50 is more than 1.
9. the preparation method of gradient porous ceramics film according to claim 1, which is characterized in that the gradient porous ceramics
The thickness of film is 100-250 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109676776A (en) * | 2019-03-01 | 2019-04-26 | 天津大学 | A kind of ceramic membrane and preparation method thereof of aperture distribution gradient |
| CN110408922A (en) * | 2019-08-29 | 2019-11-05 | 西安石油大学 | A kind of preparation method of gradient composite porous membrane tube |
| CN111548125A (en) * | 2020-04-15 | 2020-08-18 | 天津大学 | Preparation method of gradient-hole multilayer ceramic membrane |
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| JPH0650153B2 (en) * | 1987-10-22 | 1994-06-29 | 株式会社ホクコン | Method for producing composite oval tube with inner coating layer |
| CN101114719A (en) * | 2007-06-25 | 2008-01-30 | 南京工业大学 | Process for producing gradient structure film supporting with porous substrate material |
| CN101670244A (en) * | 2009-09-27 | 2010-03-17 | 南京工业大学 | Method for preparing nanofiltration membrane supporting body with gradient holes |
| CN102265438A (en) * | 2008-11-12 | 2011-11-30 | 法国原子能及替代能源委员会 | Substrate made of a porous metal or metal alloy, its method of production and HTE or SOFC cells having a support metal comprising this substrate |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0650153B2 (en) * | 1987-10-22 | 1994-06-29 | 株式会社ホクコン | Method for producing composite oval tube with inner coating layer |
| CN101114719A (en) * | 2007-06-25 | 2008-01-30 | 南京工业大学 | Process for producing gradient structure film supporting with porous substrate material |
| CN102265438A (en) * | 2008-11-12 | 2011-11-30 | 法国原子能及替代能源委员会 | Substrate made of a porous metal or metal alloy, its method of production and HTE or SOFC cells having a support metal comprising this substrate |
| CN101670244A (en) * | 2009-09-27 | 2010-03-17 | 南京工业大学 | Method for preparing nanofiltration membrane supporting body with gradient holes |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109676776A (en) * | 2019-03-01 | 2019-04-26 | 天津大学 | A kind of ceramic membrane and preparation method thereof of aperture distribution gradient |
| CN109676776B (en) * | 2019-03-01 | 2019-11-08 | 天津大学 | A kind of ceramic membrane and preparation method thereof of aperture distribution gradient |
| CN110408922A (en) * | 2019-08-29 | 2019-11-05 | 西安石油大学 | A kind of preparation method of gradient composite porous membrane tube |
| CN111548125A (en) * | 2020-04-15 | 2020-08-18 | 天津大学 | Preparation method of gradient-hole multilayer ceramic membrane |
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