CN103773236B - A kind of method preparing waterproof and oilproof type ceramic coating at substrate surface - Google Patents
A kind of method preparing waterproof and oilproof type ceramic coating at substrate surface Download PDFInfo
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Abstract
The invention discloses a kind of method preparing waterproof and oilproof type ceramic coating at substrate surface, step is as follows: under nitrogen protection, by tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C that fluorocarbon chain replaces, the silane coupling agent component D of Long carbon chain mixes, add catalyzer E, hydrolysis-condensation reaction 1-5 hour at 40-80 DEG C, obtained fluorinated silicone modified ceramic coating, this ceramic coating is spun to through pH be 9 ~ 11 the alkaline soaked in absolute ethyl alcohol substrate surface of 3 ~ 7 days, again through Overheating Treatment, obtain the substrate surface with excellent waterproof and oilproof performance, can be used for cooker, metallurgical, the fields such as marine anticorrosion is antifouling.The invention has the advantages that technique is simple, easy handling, reproducible, paint adhesion is good, transparent, and application is convenient.
Description
Technical field
The present invention relates to a kind of method preparing waterproof and oilproof type ceramic coating at substrate surface, belong to super two thin field of material technology.
Background technology
The method preparing super two thin material surface has a lot, has two kinds of different approach: one is at low-surface-energy material surface structure nano-micro structure according to the difference of principle; Two is modify low surface energy at the material surface constructing nano-micro structure.Therefore, the structured surface that focuses on preparing waterproof and oilproof type surface is received micro-coarse structured and modifies on low surface energy.
In order to super two thin materials that processability is good, investigators have spent many time and efforts to carry out large quantifier elimination.CN103290418A proposes a kind of electrochemical etching legal system of passing through for micron coarse structure, then by the dual coarse structure of hydrothermal synthesis method synthesizing zinc oxide micro-nano, is then modified by the material of low surface energy and obtain super two surface of dredging.CN102965720A obtains super two surface of dredging by Perfluorocaprylic Acid aqueous solution soaking after proposing a kind of one-step electrochemistry processing, a step chemical process again.
CN103408705A discloses a kind of method of synthesizing aqueous epoxy resins and then the super two open coat of preparation.CN102432742A disclose a kind of utilize fluorine silicon contained polymer and silicon-dioxide carry out blended after carry out assembling film forming on the surface that active group is modified, thus prepare the method for super-double-hydrophobic surface.
With regard to the preparation technology of super two thin coating of current bibliographical information, mostly need multistep, some is also quite complicated, industrial applications difficulty.Along with the development of super two thin material, the technique preparing super two thin material more and more pursues simplification, has Simplified flowsheet step only, reduces process costs, the industrialization of super two thin material 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 preparing waterproof and oilproof type ceramic coating at substrate surface of the present invention, comprises the following steps:
(1) under nitrogen protection, by tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 10 DEG C ~ 20 DEG C, 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 DEG C, obtains fluorinated silicone modified ceramic coating;
(2) ceramic coating obtained for step (1) is spun to through pH be 9 ~ 11 the alkaline soaked in absolute ethyl alcohol substrate surface of 3 ~ 7 days, the rotating speed of spin coating is 1000 ~ 3000rpm, spin-coating time is 30 ~ 60s, then thermal treatment 3 ~ 5 hours at 80 ~ 120 DEG C.
In the present invention, described silicon sol B component take alcohols as solvent, and silicon-dioxide is the acidic silicasol of 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 described general structure with the silane coupling agent component C that fluorocarbon chain replaces is:
Wherein, n is the integer of 1 ~ 4; M is the integer of 0 ~ 11; X is one in the alkylidene group of chain or ring dress, arylidene, sulfoamido, alkylsulfonyl, sulfonyloxy, carbonamido and carbon oxygen base or its combination.
In the present invention, the general structure of the silane coupling agent component D of described Long carbon chain is:
Wherein, l is the integer between 1 ~ 4, and s is the integer of 8 ~ 18.
In the present invention, described catalyzer is the hydrochloric acid of concentration 0.1mol/L ~ 1mol/L, sulfuric acid, nitric acid or acetic acid.
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, thus realizes super two performance of dredging.Specifically: by tetraethyl orthosilicate, silicon sol, there is the silane coupling agent that fluorocarbon chain replaces, the silane coupling agent of Long carbon chain, mix at 10 DEG C ~ 20 DEG C, add catalyzer, hydrolytic condensation under katalysis, generate the long gel having the silica dioxide granule of the coreshell type structure of fluoro-containing group and Long carbon chain in the surface with different size, then this gel is spin-coated to substrate surface, the rotating speed of control spin coating instrument and spin-coating time can ensure the transparency and the homogeneity of film, the silicon-dioxide of variable grain size can be assembled at substrate surface simultaneously, its surface is made to have certain coarse structure, process under high temperature, the fluoro-containing group of silica sphere and carbochain can be made to arrange more neat, increase the crystallizing power of polymkeric substance, thus the performance of its waterproof and oilproof outstanding, simultaneously, through the hydroxyl of the substrate surface of parlkaline soaked in absolute ethyl alcohol process or carboxyl can with partial hydrolysis-condensation, tetraethyl orthosilicate-fluorine containing silane-long chain silane generation the condensation reaction of surface containing hydroxyl, form interfacial bond, thus 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 relative to existing technology:
1. the ceramic coating that sol-gel method synthesis waterproof and oilproof type provided by the invention is fluorinated silicone modified, technique is simple, easy to operate, reproducible, has good practicality.
2. the present invention adopts tetraethyl orthosilicate (TEOS) to be hydrolyzed the silicon-dioxide generating variable grain size, add that in raw silicon colloidal sol, original silicon-dioxide with certain granules size goes to construct different coarse structures, thus increase the roughness on surface, make substrate surface have more excellent waterproof and oilproof performance.
The hydroxyl of the substrate surface through parlkaline soaked in absolute ethyl alcohol 3. in the present invention or carboxyl can with partial hydrolysis-condensation, tetraethyl orthosilicate-fluorine containing silane-long chain silane generation the condensation reaction of surface containing hydroxyl, 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 thereto.
Embodiment 1
Under nitrogen protection, by tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 10 DEG C, add catalyzer E, hydrolysis-condensation reaction 1 hour at 40 DEG C, obtained 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;
Above-mentioned obtained fluorinated silicone modified ceramic coating is spun to the slide surface that pH is the alkaline soaked in absolute ethyl alcohol process in 3 days of 9, the rotating speed controlling spin coating is 1000rpm, the time of spin coating is 30s, and then thermal treatment 3 hours at 80 DEG C, 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 carbon chain 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 tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 12 DEG C, add catalyzer E, hydrolysis-condensation reaction 1.5 hours at 45 DEG C, obtained 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;
Above-mentioned obtained fluorinated silicone modified ceramic coating is spun to the silicon chip surface that pH is the alkaline soaked in absolute ethyl alcohol process in 3 days of 9, the rotating speed controlling spin coating is 1500rpm, the time of spin coating is 35s, and then thermal treatment 4 hours at 100 DEG C, 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 carbon chain 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 tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 14 DEG C, add catalyzer E, hydrolysis-condensation reaction 2 hours at 50 DEG C, obtained 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;
Above-mentioned obtained fluorinated silicone modified ceramic coating is spun to the iron plate surface that pH is the alkaline soaked in absolute ethyl alcohol process in 3 days of 10, the rotating speed controlling spin coating is 1800rpm, the time of spin coating is 40s, then thermal treatment 5 hours at 120 DEG C, 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 carbon chain is dodecyl three propane TMOS, and catalyzer E is the sulfuric acid of concentration 0.1mol/L.The hydrophobic oleophobic performance detection data of the present embodiment gained waterproof and oilproof type ceramic coating are as shown in table 1.
Embodiment 4
Under nitrogen protection, by tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 15 DEG C, add catalyzer E, hydrolysis-condensation reaction 2.5 hours at 55 DEG C, obtained 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;
Above-mentioned obtained fluorinated silicone modified ceramic coating is spun to the aluminium flake surface that pH is the alkaline soaked in absolute ethyl alcohol process in 5 days of 10, the rotating speed controlling spin coating is 2000rpm, the time of spin coating is 45s, then thermal treatment 5 hours at 120 DEG C, 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 TMOS, the silane coupling agent component D of Long carbon chain is n-tetradecane base three butane TMOS, and catalyzer E is the nitric acid of concentration 1mol/L.The hydrophobic oleophobic performance detection data of the present embodiment gained waterproof and oilproof type ceramic coating are as shown in table 1.
Embodiment 5
Under nitrogen protection, by tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 16 DEG C, add catalyzer E, hydrolysis-condensation reaction 3 hours at 65 DEG C, can obtain 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;
Above-mentioned obtained fluorinated silicone modified ceramic coating is spun to the slide surface that pH is the alkaline soaked in absolute ethyl alcohol process in 3 days of 11, the rotating speed controlling spin coating is 2200rpm, the time of spin coating is 50s, and then thermal treatment 3 hours at 120 DEG C, 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 carbon chain is n-hexadecyl Trimethoxy silane, and catalyzer E is the hydrochloric acid of concentration 0.1mol/L.The hydrophobic oleophobic performance detection data of the present embodiment gained waterproof and oilproof type ceramic coating are as shown in table 1.
Embodiment 6
Under nitrogen protection, by tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 17 DEG C, add catalyzer E, hydrolysis-condensation reaction 3.5 hours at 70 DEG C, can obtain 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;
Above-mentioned obtained fluorinated silicone modified ceramic coating is spun to the silicon chip surface that pH is the alkaline soaked in absolute ethyl alcohol process in 6 days of 10, the rotating speed controlling spin coating is 2500rpm, the time of spin coating is 50s, and then thermal treatment 4 hours at 110 DEG C, 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 carbon chain is Octadecane ethyl triethoxy silicane alkane, and catalyzer E is the nitric acid of concentration 0.1mol/L.The hydrophobic oleophobic performance detection data of the present embodiment gained waterproof and oilproof type ceramic coating are as shown in table 1.
Embodiment 7
Under nitrogen protection, by tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 18 DEG C, add catalyzer E, hydrolysis-condensation reaction 4 hours at 75 DEG C, can obtain 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;
Above-mentioned obtained fluorinated silicone modified ceramic coating is spun to the iron plate surface that pH is the alkaline soaked in absolute ethyl alcohol process in 7 days of 11, the rotating speed controlling spin coating is 2800rpm, the time of spin coating is 55s, then thermal treatment 4 hours at 120 DEG C, 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 perfluoropentyl propyl group tripropoxy silane, the silane coupling agent component D of Long carbon chain is dodecyl tripropoxy silane, and catalyzer E is the hydrochloric acid of concentration 0.1mol/L.The hydrophobic oleophobic performance detection data of the present embodiment gained waterproof and oilproof type ceramic coating are as shown in table 1.
Embodiment 8
Under nitrogen protection, by tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 20 DEG C, add catalyzer E, hydrolysis-condensation reaction 5 hours at 80 DEG C, can obtain 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;
Above-mentioned obtained fluorinated silicone modified ceramic coating is spun to the aluminium flake surface that pH is the alkaline soaked in absolute ethyl alcohol process in 7 days of 11, the rotating speed controlling spin coating is 3000rpm, the time of spin coating is 60s, then thermal treatment 5 hours at 90 DEG C, 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 silane; the silane coupling agent component D of Long carbon chain is Octadecane base three butoxy silane, and catalyzer E is the hydrochloric acid of concentration 1mol/L.The hydrophobic oleophobic performance detection data of the present embodiment gained waterproof and oilproof type ceramic coating are as shown in table 1.
The performance on the ceramic coating surface of waterproof and oilproof obtained by 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 (DeanXiongandGuojunLiu.Diblock-Coploymer-CoatedWaterandoi l-RepellentCottonFabrics.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 construct good super-double-hydrophobic surface, this sol-gel method is adopted 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 the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under what other were any do not deviate from spirit of the present invention and principle, substitute, combine, simplify; be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (3)
1. prepare a method for waterproof and oilproof type ceramic coating at substrate surface, it is characterized in that comprising the following steps:
(1) under nitrogen protection, by tetraethyl orthosilicate component A, silicon sol B component, there is the silane coupling agent component C of fluorocarbon chain replacement, the silane coupling agent component D of Long carbon chain, mix at 10 DEG C ~ 20 DEG C, 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 DEG C, obtains fluorinated silicone modified ceramic coating;
(2) ceramic coating obtained for step (1) is spun to through pH be 9 ~ 11 the alkaline soaked in absolute ethyl alcohol substrate surface of 3 ~ 7 days, the rotating speed of spin coating is 1000 ~ 3000rpm, and spin-coating time is 30 ~ 60s, then thermal treatment 3 ~ 5 hours at 80 ~ 120 DEG C;
Described silicon sol B component take alcohols as solvent, and silicon-dioxide is the acidic silicasol of 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;
The described general structure with the silane coupling agent component C that fluorocarbon chain replaces is:
Wherein, n is the integer of 1 ~ 4; M is the integer of 0 ~ 11; X is one in the alkylidene group of chain or ring dress, arylidene, sulfoamido, alkylsulfonyl, sulfonyloxy, carbonamido and carbon oxygen base or its combination;
The general structure of the silane coupling agent component D of described Long carbon chain is:
Wherein, l is the integer of 1 ~ 4, and s is the integer of 8 ~ 18.
2. the method preparing waterproof and oilproof type ceramic coating at substrate surface according to claim 1, is characterized in that: described catalyzer is the hydrochloric acid of concentration 0.1mol/L ~ 1mol/L, sulfuric acid, nitric acid or acetic acid.
3. the method 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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| US10593538B2 (en) * | 2017-03-24 | 2020-03-17 | Fujifilm Electronic Materials U.S.A., Inc. | Surface treatment methods and compositions therefor |
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| CN111334136B (en) * | 2020-03-30 | 2021-09-07 | 东南大学 | Long-acting oil-proof coating and preparation method thereof |
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Application publication date: 20140507 Assignee: HANGZHOU NANOGEL NEW MATERIAL Co.,Ltd. Assignor: ZHEJIANG University Contract record no.: X2021330000014 Denomination of invention: A method of preparing waterproof and oil proof ceramic coating on the surface of substrate Granted publication date: 20160203 License type: Common License Record date: 20210204 |