CN109761638A - A method of porous ceramic layer is prepared on metal, ceramics, enamel or glass baseplate - Google Patents
A method of porous ceramic layer is prepared on metal, ceramics, enamel or glass baseplate Download PDFInfo
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- CN109761638A CN109761638A CN201910115697.XA CN201910115697A CN109761638A CN 109761638 A CN109761638 A CN 109761638A CN 201910115697 A CN201910115697 A CN 201910115697A CN 109761638 A CN109761638 A CN 109761638A
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Abstract
The present invention provides a kind of method that porous ceramic layer is prepared on metal, ceramics, enamel or glass baseplate, is related to ceramic layer preparation field.This prepares the method for porous ceramic layer on metal, ceramics, enamel or glass baseplate, by oxide, carbide, nitride or sulfide powder particle of the size between about 3nm and 100nm and hydroxycarboxylic acid and at least one solvent and at least one polymer adhesive (or combination of monomer and radical initiator) are combined to form the mixture with the greater than about nano particle solid content of 30 volume %, and mixture is applied to dip-coating on substrate, spin coating, dipping, dipping, spraying, silk-screen printing or film in the following manner and is cast；By the mixture drying of coating and it is solidified into porous layer.This prepares the method for porous ceramic layer on metal, ceramics, enamel or glass baseplate, and porous, the fine and close chemical resistance that can ensure that improvement stratiform substrate with porous ceramic layer can be made, and improves scratch resistance and improves temperature stability.
Description
Technical field
The present invention relates to ceramic layer preparation field, specially one kind is prepared more on metal, ceramics, enamel or glass baseplate
The method of hole ceramic layer.
Background technique
Press ceramic layer must carry out at a relatively low temperature in predetermined substrate, as implemented at present in the prior art
As.This means that the particle size of initial ceramic powders used must be reduced, because the diffusion of particle is logical during sintering
Crossing biggish available surface is enhanced, and reduces the sintering temperature of ceramic particle used again in turn.In order in metal, pottery
Ceramic layer is formed on porcelain, enamel or glass baseplate, the basic granularity of ceramic powders used has to be lower than 200nm, preferably shorter than
100nm, especially preferably less than 50nm.Compared with the organic bond accounting in layer, the accounting of ceramic particle must be high, with
Enough contacts are provided between grain, this is the basic prerequisite of sintering process.This means that being coated in intended substrate uniform
The solid content of nanoparticle ceramic layer had to be larger than for 30% (by volume), preferably greater than 35% (by volume), especially
Preferably greater than 40% (by volume).
This is required considerably beyond the prior art.The processing of nanoparticle is present existing main difficulty.For partial size
About the particle of 10nm, specific surface area increase to 250m2/g.Related to this to be, the part of organic bond must sharply increase
Add, because of existing large surface combination organic processing aid, then organic processing aid is no longer available for setting rheological characteristic.This is again
Lead to very small solid content, such as ceramic coated layer, thus the linear contraction of ceramic layer and tension become during the sintering process
Greatly, ceramic layer is made to rupture and fall off.In addition, commercially available nano particle is usually (the realization nano particle of agglomeration
The basic prerequisite of indefectible layer is that nano particle is isolated from each other) or only can be used as the precursor of ceramic particle.These are commercially available
One example is presoma nanoscale boehmite (bohmit), during the sintering process release water outlet, this also leads to the separation of layer.
Document is provided only about nano particle to be processed into some instructions of ceramic layer, because being always difficult to realize enough
High solid content is for being sintered.Most wide-scale distribution is research by silk-screen printing that nano particle processing is layered.
Carotta produces the composition of Nano titanium dioxide, and maximum filer content was 5.4% (by volume).From document
The optimum for the nano-scale particle ceramic composition handled by silk-screen printing known is solid content 17% (by volume).
These compositions do not allow to produce ceramic layer on metal, ceramics, enamel or glass baseplate.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides one kind prepared on metal, ceramics, enamel or glass baseplate it is more
The method of hole ceramic layer solves the problems, such as to be difficult to produce ceramic layer on metal, ceramics, enamel or glass baseplate.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs: it is a kind of metal, ceramics, enamel or
The method of porous ceramic layer is prepared on glass baseplate, which comprises by oxidation of the size between about 3nm and 100nm
Object, carbide, nitride or sulfide powder particle and hydroxycarboxylic acid and combine at least one solvent and at least one polymer
Adhesive (or combination of monomer and radical initiator) has the nano particle solid content of greater than about 30 volume % to be formed
Mixture；In the following manner by mixture be applied to dip-coating on substrate, spin coating, dipping, dipping, spraying, silk-screen printing or
Film casting；By the mixture drying of coating and it is solidified into porous layer.
Preferably, the step of the method also includes selection technological parameters to fill the porous layer with substance.
Preferably, the step of the method also includes selection fractal structure of the technological parameter to establish porous layer.
Preferably, the mixture has the solid content of the greater than about nano particle of 35% (by volume).
Preferably, the mixture has the solid content of the greater than about nano particle of 40% (by volume).
Preferably, including by the mixture sintering to close to theoretical density.
Preferably, further include into porous layer be added selected from hydrophobization, hydrophiling, it is antifouling, corrosion inhibit, sterilization, fragrance,
The step of fragrance, drug and inhaled material.
Preferably, the porous ceramic layer includes that material transport can be made to the hole of the porous ceramics layer surface.
A method of porous ceramic layer being prepared on metal, ceramics, enamel or glass baseplate, is included the following steps,
It is characterized in that:
S1: by the zirconium dioxide (primary particle size 10nm) of 30g nanoscale stabillzed with yttrium and diluted hydroxycarboxylic acid in water
Mixing.4.5g polyvinyl alcohol is added into the suspension, and suspension is homogenized.Translucent solution will be clear to apply by dipping
It is arranged on 10 × 10cm steel substrate (1.4511 or 1.4301), and dry in 80 DEG C of drying box.Then by the steel of coating
Substrate is kept for 1 hour at 500 DEG C.The rate of heat addition is 5K/min.Form porous ceramic layer.
S2: (porous to porous ceramic layer progress functionalization in the duct that second group is assigned to porous ceramic layer by introducing
Ceramic layer can be filled hydrophobization, hydrophiling, it is antifouling and corrosion inhibiting substances, these substances be retained in matrix or as needed with
After supply, or the Fungicidal substance with the exact dose for being transmitted to room air, aromatic hydrocarbons, fragrance or inhaled material are filled together).
S3: by noble metal such as silver, gold and copper are deposited in solid substrate from solution.
S4: these layers must solidify in substrate, wherein adhering in substrate on one side, another side must assure that each ceramics
Connection between particle.
(3) beneficial effect
The present invention provides a kind of methods that porous ceramic layer is prepared on metal, ceramics, enamel or glass baseplate.Have
Below the utility model has the advantages that
This prepares the method for porous ceramic layer on metal, ceramics, enamel or glass baseplate, and ceramic composition allows in gold
Ceramic layer is prepared on category, glass, enamel or ceramics, thickness degree is between 100nm and 10 μm.These layers be it is transparent, completely
It is flexible.These layers can be bent on 0.5nm steel plate and be bent to 160 degree of angles, without rupturing or peeling off the layer.This flexibility
It has been more than the flexibility of the ceramic layer of the prior art.Ceramic layer of the invention can be made porous.Fine and close and porous ceramic layer
It can ensure that the chemical resistance for improving stratiform substrate, improve scratch resistance and improve temperature stability.In addition, porous ceramic layer has
There is very big inner surface, which can fill the second component so that porous ceramic layer is functionalized.Porous ceramic layer can be with
Hydrophobization is filled, antifouling and corrosion inhibiting substances, these substances of hydrophiling are retained in matrix or supply when needed, or
Equipped with Fungicidal substance, aromatic, fragrance or inhaled material, it is then delivered in room air.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
The embodiment of the present invention provides a kind of method that porous ceramic layer is prepared on metal, ceramics, enamel or glass baseplate,
The described method includes: the oxide by size between about 3nm and 100nm, carbide, nitride or sulfide powder particle with
Hydroxycarboxylic acid and at least one solvent of combination and at least one polymer adhesive (or combination of monomer and radical initiator)
To form the mixture with the greater than about nano particle solid content of 30 volume %；Mixture is applied in the following manner
Dip-coating, spin coating, dipping, dipping, spraying, silk-screen printing or film casting on substrate；By the mixture drying of coating and it is solidified into
Porous layer.
The step of the method also includes selection technological parameters to fill the porous layer with substance.
The step of the method also includes selection fractal structure of the technological parameter to establish porous layer.
The mixture has the solid content of the greater than about nano particle of 35% (by volume).
The mixture has the solid content of the greater than about nano particle of 40% (by volume).
The mixture sintering is to close to theoretical density.
It is added into porous layer selected from hydrophobization, hydrophiling, antifouling, corrosion inhibition, sterilization, fragrance, fragrance, drug and suction
The step of entering substance.
Porous ceramic layer includes that material transport can be made to the hole of the porous ceramics layer surface.
A method of porous ceramic layer is prepared on metal, ceramics, enamel or glass baseplate, comprising the following steps:
S1: by the zirconium dioxide (primary particle size 10nm) of 30g nanoscale stabillzed with yttrium and diluted hydroxycarboxylic acid in water
Mixing.4.5g polyvinyl alcohol is added into the suspension, and suspension is homogenized.Translucent solution will be clear to apply by dipping
It is arranged on 10 × 10cm steel substrate (1.4511 or 1.4301), and dry in 80 DEG C of drying box.Then by the steel of coating
Substrate is kept for 1 hour at 500 DEG C.The rate of heat addition is 5K/min.Form porous ceramic layer.In this manner it is achieved that group
The content of powder in object is closed, it is sufficiently high to allow at low temperature (depending on the application between 400 DEG C and 1200 DEG C) corresponding
Applied ceramic layer is compacted in substrate (preferably metal, enamel, glass).It, can be with by using the hydroxycarboxylic acid of surface-active
Realize the composition of high uniformity, the present composition preferably comprises nano-scale particle, be preferably Si, Al, B, Zn, Cd, Ti,
Oxide, oxide hydrate, chalkogenide, nitride or the carbide of Ce, Sn, In, La, Fe, Cu, Ta, Nb, V, Mo or
W, particularly preferred Si, Zr, Al, B, W and Ti.Most preferably with oxide.Preferred nano grade inorganic solid particle is oxidation
Aluminium, boehmite (bohmit), zirconium oxide, yttrium stable zirconium oxide, iron oxide and titanium dioxide, the inorganic grain contained in composition
The average primary particle diameter of son is usually 1-100nm, preferably 5-50nm, particularly preferably 5-20nm.Primary granule can be with attached
Combinate form formula exists, preferably their not agglomeration or substantially not agglomeration.
In order to form the layer, initial powder is mixed with organic bond, plasticizing needed for which provides mixture.
Ceramic composition of the invention contains at least one polymer adhesive, at least one hydroxycarboxylic acid and at least one solvent.
Any thermoplastic polymer is used as polymer adhesive.The example for the thermoplastic polymer that can be used is poly-
Alkene, such as polyethylene, dipropionate (repefral, diethyl phthalate, dipropyl phthalate and
Dibutyl phthalate), polypropylene and poly-1-butylene, poly- methyl-(methyl) acrylate, polyacrylonitrile, polystyrene and
Polyolefin.Polyvinyl alcohol, polyurethane and corresponding copolymer such as ethane-acetic acid ethyenyl ester (EVA) copolymer and biopolymer
Such as cytopathy, long amber etc., wherein it is preferred that polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyamides compound, poly- methyl-prop
Olefin(e) acid ester.Thermoplastic polymer or the mixture of two or more thermoplastic polymers, acrylate and methyl can be used
Acrylate is used as polymers compositions, is crosslinked using radical initiator for example, by vinyl esters.UV radiation or
It is hot after forming, to establish polymers compositions needed for the present composition.Commercially available all acrylate and metering system
Ester compound is all suitable.It is preferred that BASF distribution Lucirin trade mark and Laromer trade mark, as LR8765,
ES81、LR8713、 LR8986、PE55F、PE56F、LR8793、LR8846、LR9004、LR8799、LR8800、LR8907、
LR8981、LR8992、PE55W、LR8895、LR8949、LR8983、LR8739、LR8987、LR8748、 LR8863、LR8945、
LR8967、LR8982、LR8812、LR8894、LR8997、LR8864、LR8889、 LR8869、LR8996、LR8946、
LR8899、LR8985。
As activation initiator, all radical initiators well known by persons skilled in the art can be used.Work as silk-screen printing
When as ceramic shaping method and producing precision architecture by engineering, this method is especially suitable.
In order to generate required compatibility between ceramic particle and polymer substrate, surface active molecules are used.These
Molecule must have difunctional structure, so that a part of molecule is in conjunction with particle surface, and another part of molecule is real
Now with the compatibility of matrix.Therefore, it is appropriate that especially from carboxylic acid, carboxylic acid amides, carboxylate, carboxylic acid chloride, diketone, alkane
The bifunctional molecule of base silane and especially hydroxycarboxylic acid.Hydroxycarboxylic acid for the method for the present invention embodiment is trioxane acid
With dioctyl heptanesulfonic acid.
As other components, ceramic composition contains organic solvent or the mixture of two or more organic solvents, preferably
Aklylene glycol, especially ethylene glycol, propylene glycol, diethylene glycol monobutyl ether, diethylene glycol monoether, diglycol monotertiary hexyl ether, diethyl
The molecule of glycol monododecyl ether, divinyl triol list ether and similar structures.In a preferred embodiment, make
The alcohol mixture of spent glycol and diethylene glycol monobutyl ether.In particularly preferred embodiments, water is used as solvent.
By nanometer grade powder and polymer, hydroxycarboxylic acid and solvent or solvent mixture are mixed, and pass through spin coating, dip-coating,
Dipping, dipping or spraying are applied on required substrate.They are dried, adhesive is then removed, is then compacted into them
Flawless porous ceramic layer.The layer produced in this way can be impregnated with substance, i.e., filled with imparting porous layer new function
Substance.
S2: (porous to porous ceramic layer progress functionalization in the duct that second group is assigned to porous ceramic layer by introducing
Ceramic layer can be filled hydrophobization, hydrophiling, it is antifouling and corrosion inhibiting substances, these substances be retained in matrix or as needed with
After supply, or the Fungicidal substance with the exact dose for being transmitted to room air, aromatic hydrocarbons, fragrance or inhaled material are filled together).
S3: by noble metal such as silver, gold and copper are deposited in solid substrate from solution.
S4: these layers must solidify in substrate, wherein adhering in substrate on one side, another side must assure that each ceramics
Connection between particle, ceramic powders used are that nanometer scale ceramics form powder.It is especially nanoscale chalcogenide,
Carbide or nitride powder.Chalcogenide powder can be oxide, sulfide, selenides or tellurides powder.Nanoscale
Oxide powder is preferred.It can be used commonly used in powder sintered any powder.Example is (being optionally hydrated) oxidation
Object, such as ZnO, CeO2, SnO2, Al2O3, CdO, SiO2, TiO2, In2O3, ZrO2, the stable ZrO2, Al2O3 of yttrium,
La2O3, Fe2O3, F3O4, Cu2O, Ta2O5, Nb2O5, V2O5, MoO3 or WO3 and phosphate, silicate, zirconates, aluminium
Hydrochlorate and stannate, sulfide such as CdS, ZnS, PbS and Ag2S, selenides such as GaSe, CdSe and ZnSe, silicide such as ZnTe
Or CdTe, carbide such as VC, CdC2 or SiC, nitride such as BN, AlN, Si3N4 and Ti3N4, corresponding mixed oxide, example
Such as metallic tin oxides indium tin (ITO), antimony tin, the Al2O3 of tin oxide and the Zn doping of Fluorin doped, have containing Y or
The luminous pigment of the compound of Eu or mixed oxide with Perowshit structure, such as BaTiO3 and lead zirconate titanate
(PZT).Also the mixture of the powder particle can be used.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (8)
1. a kind of method for preparing porous ceramic layer on metal, ceramics, enamel or glass baseplate, which comprises by ruler
It the very little oxide between about 3nm and 100nm, carbide, nitride or sulfide powder particle and hydroxycarboxylic acid and is incorporated into
A kind of few solvent and at least one polymer adhesive (or combination of monomer and radical initiator) have greater than about to be formed
The mixture of the nano particle solid content of 30 volume %；In the following manner by mixture be applied to dip-coating on substrate, spin coating,
Dipping, dipping, spraying, silk-screen printing or film casting by the mixture drying of coating and are solidified into porous layer.
2. a kind of side for preparing porous ceramic layer on metal, ceramics, enamel or glass baseplate according to claim 1
Method, it is characterised in that: the step of the method also includes selection technological parameters to fill the porous layer with substance.
3. a kind of side for preparing porous ceramic layer on metal, ceramics, enamel or glass baseplate according to claim 1
Method, it is characterised in that: the step of the method also includes selection fractal structure of the technological parameter to establish porous layer.
4. a kind of side for preparing porous ceramic layer on metal, ceramics, enamel or glass baseplate according to claim 1
Method, it is characterised in that: the mixture has the solid content of the greater than about nano particle of 35% (by volume).
5. a kind of side for preparing porous ceramic layer on metal, ceramics, enamel or glass baseplate according to claim 1
Method, it is characterised in that: the mixture has the solid content of the greater than about nano particle of 40% (by volume).
6. a kind of side for preparing porous ceramic layer on metal, ceramics, enamel or glass baseplate according to claim 1
Method, it is characterised in that: including by the mixture sintering to close to theoretical density.
7. a kind of side for preparing porous ceramic layer on metal, ceramics, enamel or glass baseplate according to claim 1
Method, it is characterised in that: further include into porous layer be added selected from hydrophobization, hydrophiling, it is antifouling, corrosion inhibit, sterilization, fragrance,
The step of fragrance, drug and inhaled material.
8. a kind of side for preparing porous ceramic layer on metal, ceramics, enamel or glass baseplate according to claim 1
Method, it is characterised in that: the porous ceramic layer includes that material transport can be made to the hole of the porous ceramics layer surface.
A method of porous ceramic layer being prepared on metal, ceramics, enamel or glass baseplate, is included the following steps, feature
It is:
S1: the zirconium dioxide (primary particle size 10nm) of 30g nanoscale stabillzed with yttrium is mixed with diluted hydroxycarboxylic acid in water,
4.5g polyvinyl alcohol is added into the suspension, and suspension is homogenized, translucent solution will be clear to and set by dip coated
It is dry on 10 × 10cm steel substrate (1.4511 or 1.4301), and in 80 DEG C of drying box, then by the steel substrate of coating
It is kept for 1 hour, rate of heat addition 5K/min at 500 DEG C, forms porous ceramic layer.
S2: functionalization (porous ceramics is carried out to the porous ceramic layer by introducing in the duct that second group is assigned to porous ceramic layer
The fillable hydrophobization of layer, hydrophiling, antifouling and corrosion inhibiting substances, these substances are retained in matrix or then supply as needed
It answers, or is filled together with the Fungicidal substance for the exact dose for being transmitted to room air, aromatic hydrocarbons, fragrance or inhaled material).
S3: by noble metal such as silver, gold and copper are deposited in solid substrate from solution.
S4: these layers must solidify in substrate, wherein adhering in substrate on one side, another side must assure that each ceramic particle
Between connection.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114478026A (en) * | 2022-01-20 | 2022-05-13 | 江苏埃梯恩膜过滤技术有限公司 | Inorganic binder for ceramic or glass ceramic |
| CN115279717A (en) * | 2019-12-12 | 2022-11-01 | 尼蓝宝股份有限公司 | Ceramic surface modification material |
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| EP1095089A1 (en) * | 1998-07-07 | 2001-05-02 | Cognis Deutschland GmbH | Hardener for epoxy resins |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115279717A (en) * | 2019-12-12 | 2022-11-01 | 尼蓝宝股份有限公司 | Ceramic surface modification material |
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Application publication date: 20190517 |