CN108101549A - A kind of preparation method of flat nano ceramics film - Google Patents
A kind of preparation method of flat nano ceramics film Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of flat nano ceramics film, this method is will to use special nozzle spray printing on planar ceramic membrane supporter with different chemical compositions and particle size for nano level ceramic membrane slurry, then the ceramic membrane with different chemical compositions and nanoaperture structure is formed in supporting body surface using Rapid Microwave Sintering at different temperature.Effective control to ceramic film thickness and uniformity can be realized by the amount for the ceramic membrane slurry for accurately controlling ejection using ink-jet sheet technology.Flat nano ceramics film prepared by this method has the characteristics that even film layer, thickness controllable precise and is tightly combined with supporter, by multiple ink-jet die can realize film layer inner hole structure by table to inner in ascending graded, so as to reduce filtration resistance, filtration flux is improved.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic membrane, more particularly to a kind of system of flat nano ceramics film
Preparation Method belongs to ceramic membrane preparing technical field.
Background technology
Ceramic membrane just obtains more and more extensive answer in trade effluent and sanitary wastewater processing, drink water purifying etc.
With playing the effect to become more and more important in environmental protection.But the aperture of ceramic super-filtering film is usually between 100~200nm, right
Some fine particles, particularly in water microorganism and organic matter to be separated by filtration effect undesirable, therefore, to some industrial wastewaters
In COD and BOD removal effects it is not notable, be still difficult to after single Ceramic excessive filtration membrane filtration the discharge for reaching industrial wastewater or return
With requiring.For this purpose, it often needs to add other chemical agents or COD and BOD in waste water is reduced using biodegradable method
Content, technological process and processing cost which not only adds wastewater treatment also make the chemical composition in waste water more complicated,
It is unfavorable for the circulating and recovering of waste water.For fine particle, microorganism and organic matter in waste water is made more effectively to be separated by filtration,
The aperture of ceramic membrane must be made to be reduced to below 50nm, and the manufacturing process of nanofiltration membrane has the following problems at present：
1. due to nanoparticle activated height, easily there is uneven grow up and makes hole in particle in the sintering process of ceramic membrane
The phenomenon that footpath is uneven, and porosity reduces causes filtering accuracy and filtration flux to reduce.
2. the paint-on technique of existing nanofiltration film layer is mainly realized by silk-screen printing technique, due to wire diameter sizes and aperture
Limitation, the thicknesses of layers printed every time easily lead to film layer usually at 5 microns or more, and when supporter flatness is not good enough
The phenomenon that gage distortion is even bitten influences filter efficiency and filtering accuracy.
Therefore, how to provide a kind of preparation method of the controllable nano ceramics film of uniform pore diameter, thicknesses of layers becomes this
The problem of field technology personnel's urgent need to resolve.
The content of the invention
In view of this, the present invention provides a kind of preparation method of flat nano ceramics film, the pottery that single can be printed
Porcelain thicknesses of layers is controlled within 1 micron, and even film layer, and by the slurry and grain size of each film layer of Reasonable Regulation And Control, it can be real
Existing pore structure, to film surface from micron order to nano level graded, so as to effectively reduce filtration resistance, is carried from supporter
High filtration flux.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of preparation method of flat nano ceramics film, comprises the following steps：
(1) the plastic mud vacuum for preparing ceramic film support is extruded as the wet base of hollow type flat ceramic film support,
Microwave drying obtains ceramic film support dry body；
(2) ceramic film support dry body is sintered at a certain temperature, obtains ceramic film support biscuit；
(3) it is the surface modifier of ceramic membrane powder quality 0.5~3%, 0.5~3% by ceramic membrane powder and gross mass
Dispersant, 1~5% binding agent and 300~800% water uniformly mix, ceramic membrane slurry is made；
(4) it is no more than 5 microns of organic sealing agent in ceramic film support biscuit surface spray printing a layer thickness first；Then
It is starched using the nozzle difference spray printing with different ink-jet apertures with the ceramic membrane of identical or different chemical composition and different-grain diameter
Material, the grain size of ceramic membrane slurry are sequentially reduced from the inside to the outside, and ceramic film overall thickness is controlled at 5~20 microns；
(5) the supporter biscuit Rapid Microwave Sintering of ceramic membrane slurry by spray printing obtains flat nano ceramics film production
Product.
It is designed by the graded pore structure of film layer, the ceramic membrane slurry with varying particle size is used into special nozzle
It is printed on planar ceramic membrane supporting body surface by several times.Since the slurry that nozzle unit area sprays can accurately be adjusted by computer
Control, control accuracy can be within 0.5 micron, therefore can effectively control the thickness of each tunic.Further, since ink-jet die not with
Supporter contacts, and the supporting body surface poor to flatness can also realize uniform die, effectively overcomes in silk-screen printing because of branch
Support body out-of-flatness and the problem of make film layer uneven or even bite.Branch can effectively be mitigated by the graded of film layer chemical composition
Thermal stress between support body and film layer improves the bond strength between supporter and film layer.
Preferably, the plastic mud of ceramic film support described in step (1) includes aluminium oxide, carborundum, cordierite, titanium
At least one of sour aluminium.
Preferably, sintering temperature control, can be according to the unlike material of supporter between 1200~1500 DEG C in step (2)
Determine corresponding sintering temperature.
Preferably, the chemical composition of ceramic membrane powder described in step (3) is aluminium oxide, zirconium oxide, silica, oxidation
One or more in titanium, for size controlling between 20~200nm, pattern is subsphaeroidal particle.
Preferably, surface modifier described in step (3) is silane coupling agent, titanate coupling agent, aluminate coupling agent
With one or more combinations in stearic acid.
Preferably, dispersant described in step (3) is polyethyleneimine, brocide, polyvinylpyrrolidine
One or more combinations in ketone, polyacrylate, polyethylene carboxylic acid, hydroxypropyl acrylate copolymer.
Preferably, binding agent described in step (3) is polyvinyl alcohol, polyethylene glycol, hydroxypropyl methyl cellulose, carboxymethyl
It is one or more in cellulose.
Preferably, organic sealing agent described in step (4) is by polyvinyl alcohol, dextrin, hydroxypropyl methyl cellulose and poly- second
Glycol forms, and is modulated into the aqueous solution of mass fraction 5~10%.
Preferably, for the control of sintering temperature described in step (5) between 600~1200 DEG C, sintering temperature should be according to ceramics
The material of film and grain size determine, and must not be higher than the sintering temperature of its ceramic film support.Achievable film layer need to be relatively low
At a temperature of burn till so that the sintering of neck is without finding apparent densification between membrane-coating granules, so that it is guaranteed that the hole that film layer is higher
Gap rate and relatively narrow pore-size distribution.
Preferably, the aperture of gained ceramic membrane is sequentially reduced by one lateral outer of supporter, and outermost layer aperture 5~
50nm。
Further explanation is made to the present invention below.
In order to obtain, bond strength is high and the big nanofiltration ceramic membrane of filtration flux, it is necessary to try to improve ceramic film support with
Bond strength between membrane material, while reduce the filtration resistance of film layer.In the present invention, set by the graded pore structure of film layer
Ceramic membrane slurry with varying particle size is printed on planar ceramic membrane support body surface by meter by several times using special nozzle
Face, the ceramic film thickness control printed every time print varigrained ceramic membrane from thick to thin successively between 1~5 micron
Slurry 3~5 times.Since the slurry that nozzle unit area sprays can be micro- 0.5 by computer accuracy controlling, control accuracy
Within rice, therefore it can effectively control the thickness of each tunic.Further, since ink-jet die is not contacted with supporter, to flatness compared with
The supporting body surface of difference can also realize uniform die, and effectively overcome in silk-screen printing makes film layer uneven due to supporter out-of-flatness
It is even or even the problem of bite.Thermal stress between supporter and film layer can effectively be mitigated by the graded of film layer chemical composition,
Improve the bond strength between supporter and film layer.By the graded of membrane-coating granules size, then effectively have adjusted in film layer
Pore structure and pore-size make pore-size inwardly gradually be increased by film surface, and porosity also increased, and effectively reduce
Filtration resistance adds filtration flux.Film layer can realize that film layer is burnt till at a lower temperature using Rapid Microwave Sintering technology,
Promote between membrane-coating granules neck sintering without finding apparent densification, ensure that the higher porosity of film layer and relatively narrow
Pore-size distribution.
The beneficial effects of the present invention are：
(1) the ceramic membrane slurry of spray printing different-grain diameter on unit area is controlled by computer using special nozzle, it can
Accurately control the thickness of each tunic, due to being non-contact spray printing, effectively overcome screen printing technique preparation film layer it is thicker and
The technical barrier high to supporter flatness requirement.
(2) by adjusting the chemical composition graded of each film layer, the chemical composition of film layer is made by the group close to supporter
It into the surface composition for changing to film successively, can effectively alleviate the thermal stress between supporter and film layer, improve between supporter and film layer
Bond strength.
(3) by adjusting the graded of each membrane layer pulp particle size, the porosity in film layer and hole are effectively had adjusted
Gap size makes pore-size inwardly gradually be increased by film surface, and porosity also increased, and effectively reduce filtration resistance,
Add the filtration flux of nanofiltration ceramic membrane.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, those of ordinary skill in the art's all other embodiments obtained without making creative work, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of preparation method of flat nano ceramics film, comprises the following steps：
(1) alumina powder of about 5 microns of average grain diameter is prepared as plastic mud, is wide with vacuum agent process forming
Surface and edge, are polishing to by 300mm, long 1024mm, the flat hollow structure ceramic film support of thickness 8mm after microwave drying
It is smooth to get ceramic film support dry body.
(2) ceramic film support dry body at 1350 DEG C is sintered, obtains ceramic film support biscuit.
(3) be with gross mass respectively by the alumina powder that grain size is 50nm, 100nm and 200nm powder quality 1% table
Face modifying agent, 0.5% dispersant, 2% binding agent mixing, add water be formulated as alumina powder solid content be 20% be suitble to
In the ceramic membrane slurry of ink-jet die；
(4) injection diameter is used on ceramic film support biscuit surface as 100 microns of one layer of ink-jet printer elder generation spray printing
Thickness is no more than 5 microns of the organic sealing agent being made of polyvinyl alcohol and hydroxypropyl methyl cellulose；
(5) on the ceramic film support biscuit surface for having printed organic sealing agent, using 100/75/50 micron of the spray in aperture
The mouth ceramic membrane slurry that spray printing grain size is 200/100/50nm successively, it is 3~5 microns to control the thickness per tunic.
(6) the supporter biscuit of ceramic membrane slurry Rapid Microwave Sintering at 1050 DEG C by spray printing, obtains flat nanometer
Ceramic membrane product.
Through flat nano ceramics film product made from above-mentioned steps, the bending strength of supporter connects not less than 45MPa
Logical porosity about 40%, about 5 microns of average pore size.About 15 microns of ceramic film overall thickness, the porosity about 33% of superficial film,
About 20 nanometers of average pore size.
Embodiment 2
A kind of preparation method of flat nano ceramics film, comprises the following steps：
(1) by the carborundum (mass fraction 93%) of about 15 microns of average grain diameter and the dioxy of 100 nanometers of average grain diameter
SiClx micro mist (mass fraction 7%) is mixed with as plastic mud, vacuum extrude for hollow type flat ceramic film support it is wet
Base, microwave drying obtain ceramic film support dry body.
(2) ceramic film support dry body at 1500 DEG C is sintered, obtains ceramic film support biscuit.
(3) it is respectively powder quality 0.5% with gross mass by the silica powder that grain size is 10nm, 80nm and 200nm
Surface modifier, 2% dispersant, 4% binding agent, add water be formulated as silica powder solid content be 15% or so be suitble to
In the ceramic membrane slurry of ink-jet die；
(4) injection diameter is used on ceramic film support biscuit surface as 100 microns of one layer of ink-jet printer elder generation spray printing
Thickness is no more than 5 microns of the organic sealing agent being made of dextrin and hydroxypropyl methyl cellulose；
(5) on the ceramic film support biscuit surface for having printed organic sealing agent, using 100/75/50 micron of the spray in aperture
The mouth ceramic membrane slurry that spray printing grain size is 200/100/50nm successively, it is 3~5 microns to control the thickness per tunic.
(6) the supporter biscuit of ceramic membrane slurry Rapid Microwave Sintering at 650 DEG C by spray printing obtains flat nanometer pottery
Porcelain film product.
Through flat nano ceramics film product made from above-mentioned steps, the bending strength of supporter connects not less than 40MPa
Logical porosity about 42%, about 4 microns of average pore size.About 10 microns of ceramic film overall thickness, the porosity about 36% of superficial film,
About 5 nanometers of average pore size.
Embodiment 3
A kind of preparation method of flat nano ceramics film, comprises the following steps：
(1) the cordierite powder of about 10 microns of average grain diameter is prepared as plastic mud, vacuum extrudes makes pottery for hollow type tablet
The wet base of porcelain film support, microwave drying obtain ceramic film support dry body.
(2) ceramic film support dry body at 1300 DEG C is sintered, obtains ceramic film support biscuit.
(3) be with gross mass respectively by the silicon carbide powder that grain size is 50nm, 80nm and 100nm powder quality 1% table
Face modifying agent, 2% dispersant, 3% binding agent, it is 20% or so to be suitable for that water is added, which to be formulated as silicon carbide powder solid content,
The ceramic membrane slurry of ink-jet die；
(4) injection diameter is used on ceramic film support biscuit surface as 100 microns of one layer of ink-jet printer elder generation spray printing
Thickness is no more than 5 microns of the organic sealing agent being made of polyvinyl alcohol and polyethylene glycol；
(5) on the ceramic film support biscuit surface for having printed organic sealing agent, using 100/75/50 micron of the spray in aperture
The mouth ceramic membrane slurry that spray printing grain size is 200/100/50nm successively, it is 3~5 microns to control the thickness per tunic.
(6) the supporter biscuit of ceramic membrane slurry Rapid Microwave Sintering at 1150 DEG C by spray printing, obtains flat nanometer
Ceramic membrane product.
Through flat nano ceramics film product made from above-mentioned steps, the bending strength of supporter connects not less than 30MPa
Logical porosity about 40%, about 3 microns of average pore size.About 10 microns of ceramic film overall thickness, the porosity about 30% of superficial film,
About 10 nanometers of average pore size.
The foregoing description of the disclosed embodiments enables professional and technical personnel in the field to realize or use the present invention.
A variety of modifications of these embodiments will be apparent for those skilled in the art, it is as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and the principles and novel features disclosed herein phase one
The most wide scope caused.
Claims (10)
1. a kind of preparation method of flat nano ceramics film, which is characterized in that comprise the following steps：
(1) the plastic mud vacuum for preparing ceramic film support is extruded as the wet base of hollow type flat ceramic film support, microwave
It is dry, obtain ceramic film support dry body；
(2) ceramic film support dry body is sintered at a certain temperature, obtains ceramic film support biscuit；
(3) by the surface modifier of ceramic membrane powder and gross mass for ceramic membrane powder quality 0.5~3%, 0.5~3% point
Powder, 1~5% binding agent and 300~800% water uniformly mix, and ceramic membrane slurry is made；
(4) it is no more than 5 microns of organic sealing agent in ceramic film support biscuit surface spray printing a layer thickness first；Then use
Nozzle difference ceramic membrane slurry of the spray printing with identical or different chemical composition and different-grain diameter with different ink-jet apertures, pottery
The grain size of porcelain film slurry is sequentially reduced from the inside to the outside, and ceramic film overall thickness is controlled at 5~20 microns；
(5) the supporter biscuit Rapid Microwave Sintering of ceramic membrane slurry by spray printing, obtains flat nano ceramics film product.
2. the preparation method of a kind of flat nano ceramics film according to claim 1, which is characterized in that in step (1)
The plastic mud of the ceramic film support includes at least one of aluminium oxide, carborundum, cordierite, aluminium titanates.
3. the preparation method of a kind of flat nano ceramics film according to claim 1, which is characterized in that in step (2)
Sintering temperature is controlled between 1200~1500 DEG C.
4. the preparation method of a kind of flat nano ceramics film according to claim 1, which is characterized in that in step (3)
The chemical composition of the ceramic membrane powder is aluminium oxide, the one or more in zirconium oxide, silica, titanium oxide, grain size
Between 20~200nm, pattern is subsphaeroidal particle for control.
5. the preparation method of a kind of flat nano ceramics film according to claim 1, which is characterized in that in step (3)
The surface modifier is one or more combinations in silane coupling agent, titanate coupling agent, aluminate coupling agent and stearic acid.
6. the preparation method of a kind of flat nano ceramics film according to claim 1, which is characterized in that in step (3)
The dispersant for polyethyleneimine, brocide, polyvinylpyrrolidone, polyacrylate, polyethylene carboxylic acid,
One or more combinations in acrylic hydroxypropyl ester copolymer.
7. the preparation method of a kind of flat nano ceramics film according to claim 1, which is characterized in that in step (3)
The binding agent is polyvinyl alcohol, one or more in polyethylene glycol, hydroxypropyl methyl cellulose, carboxymethyl cellulose.
8. the preparation method of a kind of flat nano ceramics film according to claim 1, which is characterized in that in step (4)
The organic sealing agent is made of polyvinyl alcohol, dextrin, hydroxypropyl methyl cellulose and polyethylene glycol, is modulated into mass fraction 5
~10% aqueous solution.
9. the preparation method of a kind of flat nano ceramics film according to claim 1, which is characterized in that in step (5)
The sintering temperature control is between 600~1200 DEG C.
10. according to the preparation method of any flat nano ceramics films of claim 1-9, which is characterized in that gained
The aperture of ceramic membrane is sequentially reduced by one lateral outer of supporter, 5~50nm of outermost layer aperture.
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| CN110860213A (en) * | 2018-08-28 | 2020-03-06 | 美国分子工程股份有限公司 | Thin metal/ceramic hybrid membrane and filter |
| CN110860213B (en) * | 2018-08-28 | 2022-03-29 | 美国分子工程股份有限公司 | Thin metal/ceramic hybrid membrane and filter |
| CN110256112A (en) * | 2019-06-26 | 2019-09-20 | 深圳市商德先进陶瓷股份有限公司 | Ceramic filter membrane and preparation method thereof |
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