CN103773236A - Method for preparing waterproof and oilproof ceramic coating on surface of base material - Google Patents
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Abstract
The invention discloses a method for preparing a waterproof and oilproof ceramic coating on the surface of a base material. The method comprises the following steps of uniformly mixing a tetraethyl orthosilicate ingredient A, a silica sol ingredient B, a fluorocarbon chain substituted silane coupling agent ingredient C and a long-carbon-chain substituted silane coupling agent ingredient D under the protection of nitrogen gas, adding a catalyst E, carrying out hydrolytic condensation reaction for 1-5 hours at the temperature of 40-80 DEG C, so as to prepare a fluorosilicone modified ceramic coating material, coating the surface of the base material, which is soaked for 3-7 days with alkaline anhydrous ethanol with the pH value of 9-11, with the ceramic coating material in a spin coating manner, and carrying out heat treatment, thereby obtaining the base material surface with excellent waterproof and oilproof properties. The ceramic coating material can be applied to the fields of cooking utensils, metallurgy, the corrosion and pollution prevention of oceans, and the like. The method has the advantages that the process is simple, the operation is easy, the repeatability is good, and the coating material is good in caking property, is transparent and is convenient in application.
Description
Technical field
The present invention relates to a kind of method of preparing waterproof and oilproof type ceramic coating at substrate surface, belong to super two thin material technologies field.
Background technology
The method of the super two thin material surfaces of preparation has a lot, has two kinds of different approach according to the difference of principle: the one, at low-surface-energy material surface structure nano-micro structure; The 2nd, modify low surface energy at the material surface of having constructed nano-micro structure.Therefore the structured surface that focuses on of, preparing waterproof and oilproof type surface is received micro-coarse structured and modifies on low surface energy.
For the good super two thin materials of processability, investigators have spent many time and efforts to carry out a large amount of research.CN103290418A proposes a kind of by the standby micron of electrochemical etching legal system coarse structure, then by the dual coarse structure of hydrothermal synthesis method synthesizing zinc oxide micro-nano, is then modified and obtained super two thin surface by the material of low surface energy.CN102965720A proposes to obtain super two thin surface by Perfluorocaprylic Acid aqueous solution soaking again after a kind of one-step electrochemistry processing, a step chemical process.
CN103408705A discloses a kind of method of synthetic water epoxy resin and then the super two open coats of preparation.CN102432742A discloses a kind of surface that utilizes fluorine silicon contained polymer and silicon-dioxide to carry out modifying at active group after blend and has assembled film forming, thereby prepares the method for super-double-hydrophobic surface.
The preparation technology of super two thin coating of just current bibliographical information, needs multistep mostly, and some is also quite complicated, industrial applications difficulty.Along with the development of super two thin materials, the technique of the super two thin materials of preparation is more and more pursued simplification, has simplification processing step only, reduces process costs, the industrialization of super two thin materials could be pushed ahead.
Summary of the invention
In order to overcome the deficiencies in the prior art and shortcoming, the object of the present invention is to provide a kind of preparation technology simple, easy handling, reproducible, paint adhesion is good, transparent, and the method for waterproof and oilproof type ceramic coating is prepared in application easily at substrate surface.
The method of preparing waterproof and oilproof type ceramic coating at substrate surface of the present invention, comprises the following steps:
(1) under nitrogen protection, by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain, at 10 ℃～20 ℃, mix, add catalyzer E, the mass ratio of said components A, B, C, D and E is 1:0.20～0.83:0.15～0.31:0.05～0.1:0.1～0.5, hydrolysis-condensation reaction 1-5 hour at 40-80 ℃, obtains fluorinated silicone modified ceramic coating;
(2) the alkaline soaked in absolute ethyl alcohol substrate surface of 3～7 days that it is 9～11 that ceramic coating step (1) being made is spun to through pH, the rotating speed of spin coating is 1000～3000rpm, the spin coating time is 30～60s, then thermal treatment 3～5 hours at 80～120 ℃.
In the present invention, described silicon sol B component is take alcohols as solvent, the acidic silicasol that silicon-dioxide is solute, and colloidal sol pH is 2～6, and solid content is 5%～30%, and the particle diameter of silica dioxide granule is 10～100nm.
In the present invention, the general structure of the described silane coupling agent component C with fluorocarbon chain replacement is:
Wherein, the integer that n is 1～4; M is 0～11 integer; X is a kind of or its combination in chain or alkylidene group, arylidene, sulfoamido, alkylsulfonyl, sulfonyloxy, carbonamido and the carbon oxygen base that encircles dress.
In the present invention, the general structure of the silane coupling agent component D of described long carbochain is:
Wherein, l is the integer between 1～4, the integer that s is 8～18.
In the present invention, described catalyzer is hydrochloric acid, sulfuric acid, nitric acid or the acetic acid of concentration 0.1mol/L～1mol/L.
In the present invention, described base material is slide glass, silicon chip, iron plate or aluminium flake.
Principle of the present invention:
The present invention mainly utilizes silica dioxide granule to increase the roughness of substrate surface, utilizes fluoro-containing group to reduce low surface energy, thereby realizes super two thin performances.Specifically: by tetraethyl orthosilicate, silicon sol, there is the silane coupling agent that fluorocarbon chain replaces, the silane coupling agent of long carbochain, at 10 ℃～20 ℃, mix, add catalyzer, hydrolytic condensation under katalysis, generation has different big or small surface length the gel of the silica dioxide granule of the hud typed structure of fluoro-containing group and long carbochain, then this gel is spin-coated to substrate surface, the rotating speed of control spin coating instrument and spin coating time can guarantee the transparency and the homogeneity of film, the silicon-dioxide of variable grain size can be assembled at substrate surface simultaneously, make its surface there is certain coarse structure, under high temperature, process, can make fluoro-containing group and the carbochain of silica sphere arrange more neat, increase the crystallizing power of polymkeric substance, thereby the performance of outstanding its waterproof and oilproof, simultaneously, through the hydroxyl of the substrate surface of parlkaline soaked in absolute ethyl alcohol processing or carboxyl can with partial hydrolysis-condensation, tetraethyl orthosilicate-fluorine containing silane-long chain silane generation condensation reaction that hydroxyl is contained on surface, form interfacial bond, thereby make coating show good cohesiveness to substrate surface.Therefore, fluorinated silicone modified ceramic coating prepared by the present invention, can realize the performance of waterproof and oilproof, and the transparency and cohesiveness all better.
The present invention has following advantage and effect with respect to existing technology:
1. the synthetic fluorinated silicone modified ceramic coating of waterproof and oilproof type of sol-gel method provided by the invention, technique is simple, easy to operate, reproducible, has good practicality.
2. the present invention adopts tetraethyl orthosilicate (TEOS) hydrolysis to generate the silicon-dioxide of variable grain size, add that in raw silicon colloidal sol, original silicon-dioxide with certain granules size removes to construct different coarse structures, thereby increase surperficial roughness, make substrate surface there is more excellent waterproof and oilproof performance.
3. the hydroxyl of the substrate surface through parlkaline soaked in absolute ethyl alcohol in the present invention or carboxyl can with partial hydrolysis-condensation, tetraethyl orthosilicate-fluorine containing silane-long chain silane generation condensation reaction that hydroxyl is contained on surface, form interfacial bond, there is good cohesiveness.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
Under nitrogen protection, by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain, at 10 ℃, mix, add catalyzer E, hydrolysis-condensation reaction 1 hour at 40 ℃, make fluorinated silicone modified ceramic coating, wherein the mass ratio of component A, B, C, D, E is 1:0.20:0.15:0.05:0.1;
It is the slide surface that 9 alkaline soaked in absolute ethyl alcohol is processed for 3 days that the above-mentioned fluorinated silicone modified ceramic coating making is spun to pH, the rotating speed of controlling spin coating is 1000rpm, the time of spin coating is 30s, and then thermal treatment 3 hours at 80 ℃, can obtain waterproof and oilproof type slide surface.
In this example, silicon sol B component is pH=2, solid content is 5%, particle diameter is the silicon-dioxide ethanol colloidal sol of 10～100nm, the silane coupling agent component C with fluorocarbon chain replacement is perfluoro butyl ethyl trimethoxy silane, the silane coupling agent component D of long carbochain is n-octyl Trimethoxy silane, and catalyzer E is the hydrochloric acid of concentration 0.1mol/L.The hydrophobic oleophobic performance of the present embodiment gained waterproof and oilproof type ceramic coating detects data and is shown in Table 1.
Embodiment 2
Under nitrogen protection, by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain, at 12 ℃, mix, add catalyzer E, hydrolysis-condensation reaction 1.5 hours at 45 ℃, make fluorinated silicone modified ceramic coating, wherein the mass ratio of component A, B, C, D, E is 1:0.31:0.18:0.06:0.2;
It is the silicon chip surface that 9 alkaline soaked in absolute ethyl alcohol is processed for 3 days that the above-mentioned fluorinated silicone modified ceramic coating making is spun to pH, the rotating speed of controlling spin coating is 1500rpm, the time of spin coating is 35s, and then thermal treatment 4 hours at 100 ℃, can obtain waterproof and oilproof type silicon chip surface.
In this example; silicon sol B component is pH=4; solid content is 10%; particle diameter is the silicon dioxde propanol solution of 10～100nm; the silane coupling agent component C with fluorocarbon chain replacement is perfluoro hexyl alkylsulfonyl propyl-triethoxysilicane; the silane coupling agent component D of long carbochain is decane ethyl triethoxy silicane alkane, and catalyzer E is the hydrochloric acid of concentration 1mol/L.The hydrophobic oleophobic performance of the present embodiment gained waterproof and oilproof type ceramic coating detects data and is shown in Table 1.
Embodiment 3
Under nitrogen protection, by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain, at 14 ℃, mix, add catalyzer E, hydrolysis-condensation reaction 2 hours at 50 ℃, make fluorinated silicone modified ceramic coating, wherein the mass ratio of component A, B, C, D, E is 1:0.35:0.22:0.08:0.2;
It is the iron plate surface that 10 alkaline soaked in absolute ethyl alcohol is processed for 3 days that the above-mentioned fluorinated silicone modified ceramic coating making is spun to pH, the rotating speed of controlling spin coating is 1800rpm, the time of spin coating is 40s, and then thermal treatment 5 hours at 120 ℃, can obtain waterproof and oilproof sections sheet surface.
In this example; silicon sol B component is pH=6; solid content is 30%; particle diameter is the silicon-dioxide methanol solution of 10～100nm; the silane coupling agent component C with fluorocarbon chain replacement is the amino three propane TMOSs of perfluorooctyl sulfonyl; the silane coupling agent component D of long carbochain is dodecyl three propane TMOSs, and catalyzer E is the sulfuric acid of concentration 0.1mol/L.It is as shown in table 1 that the hydrophobic oleophobic performance of the present embodiment gained waterproof and oilproof type ceramic coating detects data.
Embodiment 4
Under nitrogen protection, by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain, at 15 ℃, mix, add catalyzer E, hydrolysis-condensation reaction 2.5 hours at 55 ℃, make fluorinated silicone modified ceramic coating, wherein the mass ratio of component A, B, C, D, E is 1:0.44:0.24:0.07:0.3;
It is the aluminium flake surface that 10 alkaline soaked in absolute ethyl alcohol is processed for 5 days that the above-mentioned fluorinated silicone modified ceramic coating making is spun to pH, the rotating speed of controlling spin coating is 2000rpm, the time of spin coating is 45s, and then thermal treatment 5 hours at 120 ℃, can obtain waterproof and oilproof type aluminium flake surface.
In this example, silicon sol B component is pH=6, solid content is 30%, particle diameter is the silicon-dioxide ethanolic soln of 10～100nm, the silane coupling agent component C with fluorocarbon chain replacement is perfluor certain herbaceous plants with big flowers base sulfonyloxy propyl group three butane TMOSs, the silane coupling agent component D of long carbochain is n-tetradecane base three butane TMOSs, and catalyzer E is the nitric acid of concentration 1mol/L.It is as shown in table 1 that the hydrophobic oleophobic performance of the present embodiment gained waterproof and oilproof type ceramic coating detects data.
Embodiment 5
Under nitrogen protection, by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain, at 16 ℃, mix, add catalyzer E, hydrolysis-condensation reaction 3 hours at 65 ℃, can make fluorinated silicone modified ceramic coating, wherein the mass ratio of component A, B, C, D, E is 1:0.53:0.28:0.06:0.3;
It is the slide surface that 11 alkaline soaked in absolute ethyl alcohol is processed for 3 days that the above-mentioned fluorinated silicone modified ceramic coating making is spun to pH, the rotating speed of controlling spin coating is 2200rpm, the time of spin coating is 50s, and then thermal treatment 3 hours at 120 ℃, can obtain waterproof and oilproof type slide surface.
In this example, silicon sol B component is pH=5, solid content is 30%, particle diameter is the silicon dioxde propanol solution of 10～100nm, the silane coupling agent component C with fluorocarbon chain replacement is perfluor nonyl carbonamido propyl trimethoxy silicane, the silane coupling agent component D of long carbochain is n-hexadecyl Trimethoxy silane, and catalyzer E is the hydrochloric acid of concentration 0.1mol/L.It is as shown in table 1 that the hydrophobic oleophobic performance of the present embodiment gained waterproof and oilproof type ceramic coating detects data.
Embodiment 6
Under nitrogen protection, by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain, at 17 ℃, mix, add catalyzer E, hydrolysis-condensation reaction 3.5 hours at 70 ℃, can make fluorinated silicone modified ceramic coating, wherein the mass ratio of component A, B, C, D, E is 1:0.67:0.30:0.09:0.4;
It is the silicon chip surface that 10 alkaline soaked in absolute ethyl alcohol is processed for 6 days that the above-mentioned fluorinated silicone modified ceramic coating making is spun to pH, the rotating speed of controlling spin coating is 2500rpm, the time of spin coating is 50s, and then thermal treatment 4 hours at 110 ℃, can obtain waterproof and oilproof type silicon chip surface.
In this example; silicon sol B component is pH=6; solid content is 20%; particle diameter is the silicon-dioxide ethanolic soln of 10～100nm; the silane coupling agent component C with fluorocarbon chain replacement is perfluor certain herbaceous plants with big flowers base carbonic acyl radical triethoxyl silane; the silane coupling agent component D of long carbochain is Octadecane ethyl triethoxy silicane alkane, and catalyzer E is the nitric acid of concentration 0.1mol/L.It is as shown in table 1 that the hydrophobic oleophobic performance of the present embodiment gained waterproof and oilproof type ceramic coating detects data.
Embodiment 7
Under nitrogen protection, by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain, at 18 ℃, mix, add catalyzer E, hydrolysis-condensation reaction 4 hours at 75 ℃, can make fluorinated silicone modified ceramic coating, wherein the mass ratio of component A, B, C, D, E is 1:0.77:0.31:0.10:0.0.5;
It is the iron plate surface that 11 alkaline soaked in absolute ethyl alcohol is processed for 7 days that the above-mentioned fluorinated silicone modified ceramic coating making is spun to pH, the rotating speed of controlling spin coating is 2800rpm, the time of spin coating is 55s, and then thermal treatment 4 hours at 120 ℃, can obtain waterproof and oilproof sections sheet surface.
In this example, silicon sol B component is pH=5, solid content is 15%, particle diameter is the silicon-dioxide ethanolic soln of 10～100nm, the silane coupling agent component C with fluorocarbon chain replacement is perfluor amyl group propyl group tripropoxy silane, the silane coupling agent component D of long carbochain is dodecyl tripropoxy silane, and catalyzer E is the hydrochloric acid of concentration 0.1mol/L.It is as shown in table 1 that the hydrophobic oleophobic performance of the present embodiment gained waterproof and oilproof type ceramic coating detects data.
Embodiment 8
Under nitrogen protection; by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain; at 20 ℃, mix; add catalyzer E; hydrolysis-condensation reaction 5 hours at 80 ℃; can make fluorinated silicone modified ceramic coating, wherein
The mass ratio of component A, B, C, D, E is 1:0.83:0.31:0.1:0.5;
It is the aluminium flake surface that 11 alkaline soaked in absolute ethyl alcohol is processed for 7 days that the above-mentioned fluorinated silicone modified ceramic coating making is spun to pH, the rotating speed of controlling spin coating is 3000rpm, the time of spin coating is 60s, and then thermal treatment 5 hours at 90 ℃, can obtain waterproof and oilproof type aluminium flake surface.
In this example; silicon sol B component is pH=6; solid content is 30%; particle diameter is the silicon-dioxide methanol solution of 10～100nm; the silane coupling agent component C with fluorocarbon chain replacement is perfluor heptyl carbonic acyl radical three butoxy silanes; the silane coupling agent component D of long carbochain is Octadecane base three butoxy silanes, and catalyzer E is the hydrochloric acid of concentration 1mol/L.It is as shown in table 1 that the hydrophobic oleophobic performance of the present embodiment gained waterproof and oilproof type ceramic coating detects data.
The performance on the ceramic coating surface of the obtained waterproof and oilproof of the each embodiment of table 1.
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 |
| WCA | 163 | 166 | 165 | 163 | 158 | 169 | 161 | 172 |
| OCA | 115 | 121 | 112 | 115 | 117 | 124 | 122 | 118 |
| SA | 11 | 13 | 13 | 13 | 18 | 15 | 17 | 9 |
In table 1, WCA is water contact angle, OCA is oily contact angle, SA is water roll angle, all according to document (Dean Xiong and Guojun Liu.Diblock-Coploymer-Coated Water and oil-Repellent Cotton Fabrics.Langmuir2012,28,6911-6918) in method test.
Above-mentioned test result shows, fluorinated silicone modified ceramic coating prepared by method provided by the invention can be constructed good super-double-hydrophobic surface, adopt this sol-gel method to prepare waterproof and oilproof type coating at substrate surface, technique is simple, easy handling, reproducible, paint adhesion is good, transparent, practical.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; change, modification that what other were any do not deviate from does under spirit of the present invention and principle, substitute, combination, simplify; be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (6)
1. a method of preparing waterproof and oilproof type ceramic coating at substrate surface, is characterized in that comprising the following steps:
(1) under nitrogen protection, by the silane coupling agent component D of tetraethyl orthosilicate component A, silicon sol B component, the silane coupling agent component C with fluorocarbon chain replacement, length carbochain, at 10 ℃ ~ 20 ℃, mix, add catalyzer E, the mass ratio of said components A, B, C, D and E is 1:0.20 ~ 0.83:0.15 ~ 0.31:0.05 ~ 0.1:0.1 ~ 0.5, hydrolysis-condensation reaction 1-5 hour at 40-80 ℃, obtains fluorinated silicone modified ceramic coating;
(2) the alkaline soaked in absolute ethyl alcohol substrate surface of 3 ~ 7 days that it is 9 ~ 11 that ceramic coating step (1) being made is spun to through pH, the rotating speed of spin coating is 1000 ~ 3000rpm, the spin coating time is 30 ~ 60s, then thermal treatment 3 ~ 5 hours at 80 ~ 120 ℃.
2. the method for preparing waterproof and oilproof type ceramic coating at substrate surface according to claim 1, it is characterized in that: described silicon sol B component is take alcohols as solvent, silicon-dioxide is the acidic silicasol of solute, colloidal sol pH is 2 ~ 6, solid content is 5% ~ 30%, and the particle diameter of silica dioxide granule is 10 ~ 100nm.
3. the method for preparing waterproof and oilproof type ceramic coating at substrate surface according to claim 1, is characterized in that: the general structure of the described silane coupling agent component C with fluorocarbon chain replacement is:
Wherein, the integer that n is 1 ~ 4; M is 0 ~ 11 integer; X is a kind of or its combination in chain or alkylidene group, arylidene, sulfoamido, alkylsulfonyl, sulfonyloxy, carbonamido and the carbon oxygen base that encircles dress.
4. the method for preparing waterproof and oilproof type ceramic coating at substrate surface according to claim 1, is characterized in that: the general structure of the silane coupling agent component D of described long carbochain is:
Wherein, the integer that l is 1 ~ 4, the integer that s is 8 ~ 18.
5. the method for preparing waterproof and oilproof type ceramic coating at substrate surface according to claim 1, is characterized in that: described catalyzer is hydrochloric acid, sulfuric acid, nitric acid or the acetic acid of concentration 0.1mol/L ~ 1mol/L.
6. the method for preparing waterproof and oilproof type ceramic coating at substrate surface according to claim 1, is characterized in that: described base material is slide glass, silicon chip, iron plate or aluminium flake.
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