CN115627459B - SiO grows on carbon steel surface2Method of coating - Google Patents
SiO grows on carbon steel surface2Method of coating Download PDFInfo
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- CN115627459B CN115627459B CN202211205703.9A CN202211205703A CN115627459B CN 115627459 B CN115627459 B CN 115627459B CN 202211205703 A CN202211205703 A CN 202211205703A CN 115627459 B CN115627459 B CN 115627459B
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- 239000011248 coating agent Substances 0.000 title claims abstract description 65
- 238000000576 coating method Methods 0.000 title claims abstract description 65
- 229910000975 Carbon steel Inorganic materials 0.000 title claims abstract description 62
- 239000010962 carbon steel Substances 0.000 title claims abstract description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 180
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 90
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 90
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 90
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 90
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 90
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 90
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 85
- 239000000758 substrate Substances 0.000 claims abstract description 80
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 35
- 239000010959 steel Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000001035 drying Methods 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 238000001704 evaporation Methods 0.000 claims abstract description 16
- 230000008020 evaporation Effects 0.000 claims abstract description 9
- 238000010304 firing Methods 0.000 claims abstract description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 63
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 59
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 42
- 239000002245 particle Substances 0.000 claims description 26
- 239000000725 suspension Substances 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 7
- 238000007654 immersion Methods 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 14
- 230000007797 corrosion Effects 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 6
- 238000007598 dipping method Methods 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 description 6
- 238000005536 corrosion prevention Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 108010025899 gelatin film Proteins 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1241—Metallic substrates
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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- Materials Engineering (AREA)
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Abstract
本发明公开一种碳素钢表面生长SiO2涂层的方法,包括:步骤一、配制SiO2溶胶;步骤二、将基板平放于装有正硅酸乙酯的烧杯上,将放置有基板的烧杯置于加热台上,得到组装系统,将组装系统负压处理,烘干,完成一面蒸镀正硅酸乙酯,将基板翻转,重复操作,完成另一面蒸镀正硅酸乙酯;步骤三、将蒸镀有正硅酸乙酯的基板浸没干燥处理后进行烧制,完成碳素钢表面生长SiO2涂层。本发明在碳素钢表面生长SiO2涂层的方法,利用提拉浸渍法在蒸镀有正硅酸乙酯的碳素钢钢表面生长SiO2涂层,一次实现钢板双面涂覆均匀涂层,SiO2涂层与钢板结合性强,具有良好铺展性,可充分利用SiO2涂层化学稳定性高和防腐性好的性能实现钢板防腐。The invention discloses a method for growing SiO2 coating on the surface of carbon steel, comprising: step 1, preparing SiO2 sol; step 2, placing a substrate flat on a beaker containing ethyl orthosilicate, placing the beaker containing the substrate on a heating table to obtain an assembly system, subjecting the assembly system to negative pressure treatment, drying, completing evaporation of ethyl orthosilicate on one side, flipping the substrate, repeating the operation, completing evaporation of ethyl orthosilicate on the other side; step 3, immersing and drying the substrate evaporated with ethyl orthosilicate and then firing, completing the growth of SiO2 coating on the surface of carbon steel. The method for growing SiO2 coating on the surface of carbon steel of the invention uses a pulling and dipping method to grow SiO2 coating on the surface of carbon steel evaporated with ethyl orthosilicate, achieving uniform coating on both sides of the steel plate at one time, the SiO2 coating has strong bonding with the steel plate, has good spreadability, and can fully utilize the high chemical stability and good corrosion resistance of the SiO2 coating to achieve corrosion protection of the steel plate.
Description
技术领域Technical Field
本发明属于防腐技术领域,具体涉及一种碳素钢表面生长SiO2涂层的方法。The invention belongs to the technical field of corrosion prevention, and in particular relates to a method for growing a SiO2 coating on the surface of carbon steel.
背景技术Background technique
近年来,碳素钢(20钢材)在热力管道建设中占有重要地位。然而,由于20钢材普遍处于暴露空气比如潮湿土壤环境中,其表面极易与氧气、水分等发生反应,导致生锈,极大影响热力管道的使用寿命。In recent years, carbon steel (20 steel) has played an important role in the construction of thermal pipelines. However, since 20 steel is generally exposed to air, such as in moist soil environments, its surface is very easy to react with oxygen, moisture, etc., resulting in rust, which greatly affects the service life of thermal pipelines.
为解决热力管道的防腐难题,当前主要采用增加有机保护层的方法,通过将20钢与外界空气或水隔绝,达到钢管外层防腐蚀的目的。然而有机材料存在强度较低的缺陷,在管道建设和维护过程中常因划伤而出现防护缺口型腐蚀点,进一步加速钢材寿命的降低。此外,管道接口、阀门等位置结构较为复杂,难以有效包覆有机层,致使接口和阀门等位置成为热力管道系统防腐中的薄弱环节。此外,由于热力管道运行过程导致的钢管内壁腐蚀往往难以得到有效重视。提供一种有效针对20钢管的全面防腐的方法,是解决当前热力管道腐蚀的主要途径之一。In order to solve the problem of corrosion prevention of thermal pipelines, the current method of adding an organic protective layer is mainly used to achieve the purpose of corrosion prevention of the outer layer of the steel pipe by isolating 20 steel from the outside air or water. However, organic materials have the defect of low strength. During the construction and maintenance of pipelines, protective notch-type corrosion points often appear due to scratches, further accelerating the reduction of steel life. In addition, the structure of pipeline interfaces, valves and other locations is relatively complex, and it is difficult to effectively cover the organic layer, making interfaces and valves and other locations the weak links in the corrosion prevention of thermal pipeline systems. In addition, the corrosion of the inner wall of the steel pipe caused by the operation of the thermal pipeline is often difficult to be effectively taken seriously. Providing an effective method for comprehensive corrosion prevention of 20 steel pipes is one of the main ways to solve the current corrosion of thermal pipelines.
发明内容Summary of the invention
本发明所要解决的技术问题在于针对上述现有技术的不足,提供一种碳素钢表面生长SiO2涂层的方法。该方法利用提拉浸渍法将蒸镀有正硅酸乙酯的碳素钢钢表面生长SiO2涂层,一次实现钢板双面涂覆均匀涂层,SiO2涂层与钢板结合性强,具有良好铺展性,可充分利用SiO2涂层化学稳定性高和防腐性好的性能,实现钢板防腐。The technical problem to be solved by the present invention is to provide a method for growing SiO2 coating on the surface of carbon steel in view of the shortcomings of the above-mentioned prior art. The method uses a pulling and dipping method to grow SiO2 coating on the surface of carbon steel evaporated with ethyl orthosilicate, so as to achieve a uniform coating on both sides of the steel plate at one time. The SiO2 coating has strong bonding with the steel plate and good spreadability, and can fully utilize the high chemical stability and good corrosion resistance of the SiO2 coating to achieve corrosion protection of the steel plate.
为解决上述技术问题,本发明采用的技术方案是:一种碳素钢表面生长SiO2涂层的方法,其特征在于,包括:In order to solve the above technical problems, the technical solution adopted by the present invention is: a method for growing SiO2 coating on the surface of carbon steel, characterized by comprising:
步骤一、提供SiO2溶胶,具体包括:Step 1: providing SiO2 sol, specifically comprising:
步骤101、将正硅酸乙酯和无水乙醇混合,于25℃~40℃搅拌1h~2h,加入去离子水,继续搅拌1h~2h,得到溶液A;Step 101, mix tetraethyl orthosilicate and anhydrous ethanol, stir at 25° C. to 40° C. for 1 h to 2 h, add deionized water, and continue stirring for 1 h to 2 h to obtain solution A;
步骤102、向所述溶液A中加入氨水,至pH为10~11,得到悬浊液;Step 102, adding ammonia water to the solution A until the pH value is 10-11 to obtain a suspension;
步骤103、将所述悬浊液离心分离,得到颗粒物,用乙醇清洗所述颗粒物后于室温下放置;Step 103, centrifuging the suspension to obtain particles, washing the particles with ethanol and placing them at room temperature;
步骤104、将室温放置后颗粒物置于乙酰丙酮、无水乙醇和己烷的混合溶液中,于室温下超声30min~40min后搅拌1h~2h,得到SiO2溶胶;Step 104, placing the particles after standing at room temperature in a mixed solution of acetylacetone, anhydrous ethanol and hexane, ultrasonicating at room temperature for 30 minutes to 40 minutes and then stirring for 1 hour to 2 hours to obtain SiO2 sol;
步骤二、在基板上蒸镀正硅酸乙酯,具体包括:Step 2: evaporating tetraethyl orthosilicate on the substrate, specifically comprising:
步骤201、将原料钢打磨,抛光,清洗,得到基板;所述原料钢为碳素钢;Step 201, grinding, polishing and cleaning the raw steel to obtain a substrate; the raw steel is carbon steel;
步骤202、将5mL~15mL正硅酸乙酯置于干净的烧杯中,将步骤201所述基板平放于烧杯上,将放置有基板的烧杯置于加热台上,得到组装系统;Step 202, placing 5 mL to 15 mL of tetraethyl orthosilicate in a clean beaker, placing the substrate described in step 201 flat on the beaker, and placing the beaker with the substrate on a heating table to obtain an assembly system;
步骤203、将上述组装系统在-0.28bar~-0.2bar负压条件下保持30min~40min,取出,在60℃~65℃烘箱中烘1h~2h;Step 203, maintaining the above-mentioned assembly system under a negative pressure condition of -0.28 bar to -0.2 bar for 30 min to 40 min, taking it out, and drying it in an oven at 60° C. to 65° C. for 1 h to 2 h;
步骤204、将基板翻转,重复步骤202和203,完成另一面蒸镀正硅酸乙酯;Step 204, turning over the substrate, repeating steps 202 and 203, and completing the evaporation of tetraethyl orthosilicate on the other side;
步骤三、在蒸镀有正硅酸乙酯的基板上生长SiO2涂层,具体包括:Step 3: growing a SiO2 coating on the substrate on which tetraethyl orthosilicate is evaporated, specifically comprising:
步骤301、将步骤二蒸镀有正硅酸乙酯的基板浸没干燥处理5次~10次;Step 301, immersing and drying the substrate on which tetraethyl orthosilicate is deposited in step 2 for 5 to 10 times;
步骤302、将浸没干燥后料件进行烧制,完成碳素钢表面生长SiO2涂层。Step 302: sinter the immersed and dried material to grow a SiO2 coating on the surface of the carbon steel.
上述的一种碳素钢表面生长SiO2涂层的方法,其特征在于,步骤101中,所述无水乙醇的物质的量为正硅酸乙酯物质的量的5倍~10倍。The above-mentioned method for growing SiO2 coating on the surface of carbon steel is characterized in that, in step 101, the amount of anhydrous ethanol is 5 to 10 times the amount of tetraethyl orthosilicate.
上述的一种碳素钢表面生长SiO2涂层的方法,其特征在于,步骤101中,所述去离子水的物质的量为正硅酸乙酯物质的量的1倍~2倍。The above-mentioned method for growing SiO2 coating on the surface of carbon steel is characterized in that, in step 101, the amount of deionized water is 1 to 2 times the amount of tetraethyl orthosilicate.
上述的一种碳素钢表面生长SiO2涂层的方法,其特征在于,步骤102中,所述氨水的质量百分含量为10%~25%。The above-mentioned method for growing SiO2 coating on the surface of carbon steel is characterized in that, in step 102, the mass percentage of the ammonia water is 10% to 25%.
上述的一种碳素钢表面生长SiO2涂层的方法,其特征在于,步骤104中,所述乙酰丙酮、无水乙醇和己烷的混合溶液中,乙酰丙酮的物质的量为步骤101所述正硅酸乙酯物质的量的6倍~10倍,无水乙醇的物质的量为步骤101所述正硅酸乙酯物质的量的5倍~10倍;己烷的物质的量为步骤101所述正硅酸乙酯物质的量的5倍~10倍。The above-mentioned method for growing SiO2 coating on the surface of carbon steel is characterized in that, in step 104, in the mixed solution of acetylacetone, anhydrous ethanol and hexane, the amount of acetylacetone is 6 to 10 times the amount of the tetraethyl orthosilicate substance in step 101, the amount of anhydrous ethanol is 5 to 10 times the amount of the tetraethyl orthosilicate substance in step 101; the amount of hexane is 5 to 10 times the amount of the tetraethyl orthosilicate substance in step 101.
上述的一种碳素钢表面生长SiO2涂层的方法,其特征在于,步骤202中,所述加热台的温度为185℃~190℃。The above-mentioned method for growing SiO2 coating on the surface of carbon steel is characterized in that, in step 202, the temperature of the heating platform is 185°C to 190°C.
上述的一种碳素钢表面生长SiO2涂层的方法,其特征在于,步骤301中,所述浸没干燥处理包括:常温条件下,将步骤二蒸镀有正硅酸乙酯的基板浸没于步骤一所述SiO2溶胶中,保持1s~5s,以4mm/s~5mm/s提拉速度拉离SiO2溶胶,将拉离后料件置于80℃~100℃干燥。The above-mentioned method for growing SiO2 coating on the surface of carbon steel is characterized in that in step 301, the immersion drying treatment includes: under room temperature conditions, immersing the substrate on which tetraethyl orthosilicate is vapor-deposited in step 2 in the SiO2 sol described in step 1, maintaining it for 1s to 5s, pulling it away from the SiO2 sol at a pulling speed of 4mm/s to 5mm/s, and placing the pulled material at 80℃ to 100℃ for drying.
上述的一种碳素钢表面生长SiO2涂层的方法,其特征在于,步骤302中,所述烧制的温度为400℃~450℃。The above-mentioned method for growing SiO2 coating on the surface of carbon steel is characterized in that, in step 302, the firing temperature is 400°C to 450°C.
本发明与现有技术相比具有以下优点:Compared with the prior art, the present invention has the following advantages:
1、本发明在碳素钢表面生长SiO2涂层的方法,利用提拉浸渍法在蒸镀有正硅酸乙酯的碳素钢钢表面生长SiO2涂层,一次实现钢板双面涂覆均匀涂层,SiO2涂层与钢板结合性强,具有良好铺展性,可充分利用SiO2涂层化学稳定性高和防腐性好的性能,实现钢板防腐。1. The method for growing SiO2 coating on the surface of carbon steel of the present invention utilizes the pulling and dipping method to grow SiO2 coating on the surface of carbon steel evaporated with ethyl orthosilicate, so as to realize double-sided uniform coating of the steel plate at one time. The SiO2 coating has strong bonding with the steel plate and good spreadability, and can fully utilize the high chemical stability and good corrosion resistance of the SiO2 coating to realize corrosion protection of the steel plate.
2、本发明的方法中,包括在生长SiO2涂层之前采用正硅酸乙酯对碳素钢蒸镀,可有效改善碳素钢表面张力,避免生长SiO2涂层缩膜。2. The method of the present invention includes using ethyl orthosilicate to evaporate carbon steel before growing the SiO2 coating, which can effectively improve the surface tension of the carbon steel and avoid shrinkage of the growing SiO2 coating.
3、本发明方法简单,易于操作,适于推广应用。3. The method of the present invention is simple, easy to operate and suitable for popularization and application.
下面结合实施例,对本发明的技术方案做进一步的详细描述。The technical solution of the present invention is further described in detail below in conjunction with embodiments.
具体实施方式Detailed ways
本发明的碳素钢表面生长SiO2涂层通过在蒸镀有正硅酸乙酯的基板上生长SiO2涂层,其中蒸镀正硅酸乙酯温度为185℃~190℃,负压为-0.28bar~-0.2bar,烧制SiO2溶胶温度为400℃~450℃,获得适宜凝结量的蒸镀有正硅酸乙酯的基板,进而获得具有有效防腐效果的SiO2凝胶膜。The SiO2 coating grown on the surface of carbon steel of the present invention is achieved by growing the SiO2 coating on a substrate on which tetraethyl orthosilicate is vapor-deposited, wherein the temperature for vapor-depositing the tetraethyl orthosilicate is 185°C to 190°C, the negative pressure is -0.28 bar to -0.2 bar, and the temperature for sintering the SiO2 sol is 400°C to 450°C, so as to obtain a substrate on which tetraethyl orthosilicate is vapor-deposited with a suitable condensation amount, thereby obtaining a SiO2 gel film with an effective anti-corrosion effect.
实施例1Example 1
本实施例提供一种碳素钢表面生长SiO2涂层的方法,包括:This embodiment provides a method for growing a SiO2 coating on a carbon steel surface, comprising:
步骤一、提供SiO2溶胶,具体包括:Step 1: providing SiO2 sol, specifically comprising:
步骤101、将1mol正硅酸乙酯和5mol无水乙醇混合,于25℃搅拌1h,加入1mol去离子水,继续搅拌1h,得到溶液A;Step 101, 1 mol of ethyl orthosilicate and 5 mol of anhydrous ethanol were mixed, stirred at 25° C. for 1 h, 1 mol of deionized water was added, and stirring was continued for 1 h to obtain a solution A;
步骤102、向所述溶液A中加入氨水,至pH为10,得到悬浊液,所述悬浊液呈白色絮凝状;所述氨水的质量百分含量为10%;Step 102, adding ammonia water to the solution A until the pH value is 10, to obtain a suspension, wherein the suspension is white and flocculated; the mass percentage of the ammonia water is 10%;
步骤103、将所述悬浊液离心分离,得到颗粒物,用乙醇清洗所述颗粒物2次,将清洗后颗粒物于室温下放置2小时,使乙醇挥发;Step 103, centrifuging the suspension to obtain particles, washing the particles twice with ethanol, and placing the washed particles at room temperature for 2 hours to allow the ethanol to evaporate;
步骤104、将室温放置后颗粒物置于乙酰丙酮、无水乙醇和己烷的混合溶液中,于室温下超声30min后搅拌1h,得到SiO2溶胶;所述乙酰丙酮、无水乙醇和己烷的混合溶液中,乙酰丙酮的物质的量为步骤101所述正硅酸乙酯物质的量的6倍,无水乙醇的物质的量为步骤101所述正硅酸乙酯物质的量的5倍;己烷的物质的量为步骤101所述正硅酸乙酯物质的量的5倍;Step 104, placing the particles after standing at room temperature in a mixed solution of acetylacetone, anhydrous ethanol and hexane, ultrasonicating for 30 minutes at room temperature and then stirring for 1 hour to obtain SiO2 sol; in the mixed solution of acetylacetone, anhydrous ethanol and hexane, the amount of acetylacetone is 6 times the amount of the tetraethyl orthosilicate in step 101, the amount of anhydrous ethanol is 5 times the amount of the tetraethyl orthosilicate in step 101; the amount of hexane is 5 times the amount of the tetraethyl orthosilicate in step 101;
步骤二、在基板上蒸镀正硅酸乙酯,所述基板为钢材质基板,具体包括:Step 2: Evaporating tetraethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, specifically comprising:
步骤201、将尺寸为40mm×40mm的碳素钢依次用400#、1500#和3000#的砂纸进行打磨,抛光,清洗,得到基板;所述清洗为用无水乙醇进行清洗;所述碳素钢为20钢,所述20钢购买自天津中泰华营钢铁;Step 201, grinding, polishing and cleaning a carbon steel having a size of 40 mm×40 mm with 400#, 1500# and 3000# sandpaper in sequence to obtain a substrate; the cleaning is performed with anhydrous ethanol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Zhongtai Huaying Steel;
步骤202、将5ml正硅酸乙酯置于干净的烧杯中,将步骤201所述基板平放于烧杯上,将放置有基板的烧杯置于加热台上,加热台的温度为185℃,得到组装系统;所述烧杯的容量为25mL;所述加热台为JFTOOIS金锋平板加热台;Step 202, place 5 ml of tetraethyl orthosilicate in a clean beaker, place the substrate described in step 201 flat on the beaker, place the beaker with the substrate on a heating table at a temperature of 185° C., and obtain an assembled system; the capacity of the beaker is 25 ml; the heating table is a JFTOOIS flat heating table;
步骤203、将上述组装系统在-0.26bar负压条件下保持30min,取出,在60℃烘箱中烘1h;所述负压条件下可以为将所述组装系统置于不锈钢容器中,抽真空至负压,密闭,所述抽真空所用泵功率为15w;Step 203, keeping the above-mentioned assembly system under negative pressure of -0.26 bar for 30 minutes, taking it out, and drying it in a 60° C. oven for 1 hour; the negative pressure condition may be placing the assembly system in a stainless steel container, evacuating to negative pressure, and sealing it, and the pump power used for the evacuation is 15W;
步骤204、将基板翻转,重复步骤202和203,完成另一面蒸镀正硅酸乙酯;Step 204, turning over the substrate, repeating steps 202 and 203, and completing the evaporation of tetraethyl orthosilicate on the other side;
步骤三、在蒸镀有正硅酸乙酯的基板上生长SiO2涂层,具体包括:Step 3: growing a SiO2 coating on the substrate on which tetraethyl orthosilicate is evaporated, specifically comprising:
步骤301、将步骤二蒸镀有正硅酸乙酯的基板浸没干燥处理5次;所述浸没干燥处理包括:常温条件下,将步骤二蒸镀有正硅酸乙酯的基板浸没于步骤一所述SiO2溶胶中,保持3s,以4mm/s提拉速度拉离SiO2溶胶,将拉离后料件置于80℃马弗炉中干燥10min;所述常温为20℃~25℃;Step 301, immersing and drying the substrate on which the tetraethyl orthosilicate is deposited in step 2 for 5 times; the immersion drying process comprises: immersing the substrate on which the tetraethyl orthosilicate is deposited in step 2 in the SiO2 sol in step 1 at room temperature for 3 seconds, pulling the substrate away from the SiO2 sol at a pulling speed of 4 mm/s, and placing the pulled substrate in a muffle furnace at 80°C for drying for 10 minutes; the room temperature is 20°C to 25°C;
步骤302、将浸没干燥后料件置于400℃的快速热处理炉中烧制10min,完成碳素钢表面生长SiO2涂层;所述烧制的升温速率为120℃/min。Step 302: Place the immersed dried material in a rapid heat treatment furnace at 400°C and sinter for 10 minutes to grow a SiO2 coating on the surface of the carbon steel; the sintering heating rate is 120°C/min.
将本实施例完成表面生长SiO2涂层的碳素钢表面废料部分切除后进行盐酸腐蚀性能测试,测试方法包括:将上述碳素钢浸没于0.1mol/L的稀盐酸中浸泡4小时,观察表面腐蚀痕迹。结果表明表面无腐蚀痕迹,采用本发明的方法获得的表面生长有SiO2涂层的碳素钢,涂层均匀致密,可将碳素钢板有效包裹,具有较好的防腐效果。After the waste material of the carbon steel surface with SiO2 coating grown on the surface of the present embodiment was removed, a hydrochloric acid corrosion performance test was conducted. The test method includes: immersing the carbon steel in 0.1 mol/L dilute hydrochloric acid for 4 hours and observing the surface corrosion marks. The results show that there are no corrosion marks on the surface. The carbon steel with SiO2 coating grown on the surface obtained by the method of the present invention has a uniform and dense coating, which can effectively wrap the carbon steel plate and has a good anti-corrosion effect.
实施例2Example 2
本实施例提供一种碳素钢表面生长SiO2涂层的方法,包括:This embodiment provides a method for growing a SiO2 coating on a carbon steel surface, comprising:
步骤一、提供SiO2溶胶,具体包括:Step 1: providing SiO2 sol, specifically comprising:
步骤101、将1mol正硅酸乙酯和10mol无水乙醇混合,于40℃搅拌2h,加入2mol去离子水,继续搅拌2h,得到溶液A;Step 101, 1 mol of ethyl orthosilicate and 10 mol of anhydrous ethanol are mixed, stirred at 40° C. for 2 h, 2 mol of deionized water is added, and stirring is continued for 2 h to obtain a solution A;
步骤102、向所述溶液A中加入氨水,至pH为11,得到悬浊液,所述悬浊液呈白色絮凝状;所述氨水的质量百分含量为25%;Step 102, adding ammonia water to the solution A until the pH value is 11, to obtain a suspension, wherein the suspension is white and flocculated; the mass percentage of the ammonia water is 25%;
步骤103、将所述悬浊液离心分离,得到颗粒物,用乙醇清洗所述颗粒物4次,将清洗后颗粒物于室温下放置2小时,使乙醇挥发;Step 103, centrifuging the suspension to obtain particles, washing the particles with ethanol for 4 times, and placing the washed particles at room temperature for 2 hours to allow the ethanol to evaporate;
步骤104、将室温放置后颗粒物置于乙酰丙酮、无水乙醇和己烷的混合溶液中,于室温下超声40min后搅拌2h,得到SiO2溶胶;所述乙酰丙酮、无水乙醇和己烷的混合溶液中,乙酰丙酮的物质的量为步骤101所述正硅酸乙酯物质的量的10倍,无水乙醇的物质的量为步骤101所述正硅酸乙酯物质的量的10倍;己烷的物质的量为步骤101所述正硅酸乙酯物质的量的10倍;Step 104, placing the particles after standing at room temperature in a mixed solution of acetylacetone, anhydrous ethanol and hexane, ultrasonicating for 40 minutes at room temperature and then stirring for 2 hours to obtain SiO2 sol; in the mixed solution of acetylacetone, anhydrous ethanol and hexane, the amount of acetylacetone is 10 times the amount of the tetraethyl orthosilicate in step 101, the amount of anhydrous ethanol is 10 times the amount of the tetraethyl orthosilicate in step 101; the amount of hexane is 10 times the amount of the tetraethyl orthosilicate in step 101;
步骤二、在基板上蒸镀正硅酸乙酯,所述基板为钢材质基板,具体包括:Step 2: Evaporating tetraethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, specifically comprising:
步骤201、将尺寸为40mm×40mm的碳素钢依次用400#、1500#和3000#的砂纸进行打磨,抛光,清洗,得到基板;所述清洗为用无水乙醇进行清洗;所述碳素钢为20钢,所述20钢购买自天津中泰华营钢铁;Step 201, grinding, polishing and cleaning a carbon steel having a size of 40 mm×40 mm with 400#, 1500# and 3000# sandpaper in sequence to obtain a substrate; the cleaning is performed with anhydrous ethanol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Zhongtai Huaying Steel;
步骤202、将10ml正硅酸乙酯置于干净的烧杯中,将步骤201所述基板平放于烧杯上,将放置有基板的烧杯置于加热台上,加热台的温度为190℃,得到组装系统;所述烧杯的容量为25mL;所述加热台为JFTOOIS金锋平板加热台;Step 202, place 10 ml of tetraethyl orthosilicate in a clean beaker, place the substrate described in step 201 flat on the beaker, place the beaker with the substrate on a heating table at a temperature of 190° C., and obtain an assembly system; the capacity of the beaker is 25 ml; the heating table is a JFTOOIS flat heating table;
步骤203、将上述组装系统在-0.23bar负压条件下保持40min,取出,在65℃烘箱中烘2h;所述负压条件下可以为将所述组装系统置于不锈钢容器中,抽真空至负压,密闭,所述抽真空所用泵功率为15w;Step 203, keeping the above-mentioned assembly system under negative pressure of -0.23 bar for 40 minutes, taking it out, and drying it in a 65° C. oven for 2 hours; the negative pressure condition may be placing the assembly system in a stainless steel container, evacuating to negative pressure, and sealing it, and the pump power used for the evacuation is 15W;
步骤204、将基板翻转,重复步骤202和203,完成另一面蒸镀正硅酸乙酯;Step 204, turning over the substrate, repeating steps 202 and 203, and completing the evaporation of tetraethyl orthosilicate on the other side;
步骤三、在蒸镀有正硅酸乙酯的基板上生长SiO2涂层,具体包括:Step 3: growing a SiO2 coating on the substrate on which tetraethyl orthosilicate is evaporated, specifically comprising:
步骤301、将步骤二蒸镀有正硅酸乙酯的基板浸没干燥处理10次;所述浸没干燥处理包括:常温条件下,将步骤二蒸镀有正硅酸乙酯的基板浸没于步骤一所述SiO2溶胶中,保持2s,以5mm/s提拉速度拉离SiO2溶胶,将拉离后料件置于100℃马弗炉中干燥10min;Step 301, immersing and drying the substrate on which the tetraethyl orthosilicate is deposited in step 2 for 10 times; the immersion drying process comprises: immersing the substrate on which the tetraethyl orthosilicate is deposited in step 2 in the SiO2 sol in step 1 at room temperature, holding for 2 seconds, pulling the substrate away from the SiO2 sol at a pulling speed of 5 mm/s, and placing the pulled substrate in a muffle furnace at 100°C for drying for 10 minutes;
步骤302、将浸没干燥后料件置于450℃的马弗炉中烧制10min,完成碳素钢表面生长SiO2涂层;所述烧制的升温速率为120℃/min。Step 302: Place the immersed dried material in a muffle furnace at 450° C. and sinter for 10 minutes to grow a SiO 2 coating on the surface of the carbon steel; the heating rate of the sintering is 120° C./min.
本实施例的完成表面生长SiO2涂层的碳素钢性能与实施例1基本一致。The performance of the carbon steel with SiO2 coating grown on the surface in this embodiment is basically the same as that in embodiment 1.
实施例3Example 3
本实施例提供一种碳素钢表面生长SiO2涂层的方法,包括:This embodiment provides a method for growing a SiO2 coating on a carbon steel surface, comprising:
步骤一、提供SiO2溶胶,具体包括:Step 1: providing SiO2 sol, specifically comprising:
步骤101、将1mol正硅酸乙酯和7mol无水乙醇混合,于30℃搅拌2h,加入1mol去离子水,继续搅拌1h,得到溶液A;Step 101, 1 mol of ethyl orthosilicate and 7 mol of anhydrous ethanol were mixed, stirred at 30° C. for 2 h, 1 mol of deionized water was added, and stirring was continued for 1 h to obtain a solution A;
步骤102、向所述溶液A中加入氨水,至pH为10,得到悬浊液,所述悬浊液呈白色絮凝状;所述氨水的质量百分含量为20%;Step 102, adding ammonia water to the solution A until the pH value is 10, to obtain a suspension, wherein the suspension is white and flocculated; the mass percentage of the ammonia water is 20%;
步骤103、将所述悬浊液离心分离,得到颗粒物,用乙醇清洗所述颗粒物3次,将清洗后颗粒物于室温下放置2小时,使乙醇挥发;Step 103, centrifuging the suspension to obtain particles, washing the particles with ethanol for 3 times, and placing the washed particles at room temperature for 2 hours to allow the ethanol to evaporate;
步骤104、将室温放置后颗粒物置于乙酰丙酮、无水乙醇和己烷的混合溶液中,于室温下超声35min后搅拌2h,得到SiO2溶胶;所述乙酰丙酮、无水乙醇和己烷的混合溶液中,乙酰丙酮的物质的量为步骤101所述正硅酸乙酯物质的量的8倍,无水乙醇的物质的量为步骤101所述正硅酸乙酯物质的量的7倍;己烷的物质的量为步骤101所述正硅酸乙酯物质的量的10倍;Step 104, placing the particles after standing at room temperature in a mixed solution of acetylacetone, anhydrous ethanol and hexane, ultrasonicating for 35 minutes at room temperature and then stirring for 2 hours to obtain SiO2 sol; in the mixed solution of acetylacetone, anhydrous ethanol and hexane, the amount of acetylacetone is 8 times the amount of the tetraethyl orthosilicate in step 101, the amount of anhydrous ethanol is 7 times the amount of the tetraethyl orthosilicate in step 101; the amount of hexane is 10 times the amount of the tetraethyl orthosilicate in step 101;
步骤二、在基板上蒸镀正硅酸乙酯,所述基板为钢材质基板,具体包括:Step 2: Evaporating tetraethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, specifically comprising:
步骤201、将尺寸为40mm×40mm的碳素钢依次用400#、1500#和3000#的砂纸进行打磨,抛光,清洗,得到基板;所述清洗为用无水乙醇进行清洗;所述碳素钢为20钢,所述20钢购买自天津中泰华营钢铁;Step 201, grinding, polishing and cleaning a carbon steel having a size of 40 mm×40 mm with 400#, 1500# and 3000# sandpaper in sequence to obtain a substrate; the cleaning is performed with anhydrous ethanol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Zhongtai Huaying Steel;
步骤202、将15ml正硅酸乙酯置于干净的烧杯中,将步骤201所述基板平放于烧杯上,将放置有基板的烧杯置于加热台上,加热台的温度为185℃,得到组装系统;所述烧杯的容量为25mL;所述加热台为JFTOOIS金锋平板加热台;Step 202, place 15 ml of tetraethyl orthosilicate in a clean beaker, place the substrate described in step 201 flat on the beaker, place the beaker with the substrate on a heating table at a temperature of 185° C., and obtain an assembled system; the capacity of the beaker is 25 mL; the heating table is a JFTOOIS flat heating table;
步骤203、将上述组装系统在-0.2bar负压条件下保持35min,取出,在60℃烘箱中烘2h;所述负压条件下可以为将所述组装系统置于不锈钢容器中,抽真空至负压,密闭,所述抽真空所用泵功率为15w;Step 203, keeping the above-mentioned assembly system under negative pressure of -0.2 bar for 35 minutes, taking it out, and drying it in a 60° C. oven for 2 hours; the negative pressure condition may be placing the assembly system in a stainless steel container, evacuating to negative pressure, and sealing it, and the pump power used for the evacuation is 15W;
步骤204、将基板翻转,重复步骤202和203,完成另一面蒸镀正硅酸乙酯;Step 204, turning over the substrate, repeating steps 202 and 203, and completing evaporation of tetraethyl orthosilicate on the other side;
步骤三、在蒸镀有正硅酸乙酯的基板上生长SiO2涂层,具体包括:Step 3: growing a SiO2 coating on the substrate on which tetraethyl orthosilicate is evaporated, specifically comprising:
步骤301、将步骤二蒸镀有正硅酸乙酯的基板浸没干燥处理8次;所述浸没干燥处理包括:常温条件下,将步骤二蒸镀有正硅酸乙酯的基板浸没于步骤一所述SiO2溶胶中,保持1s,以4.5mm/s提拉速度拉离SiO2溶胶,将拉离后料件置于90℃马弗炉中干燥10min;Step 301, immersing and drying the substrate on which the tetraethyl orthosilicate is deposited in step 2 for 8 times; the immersion drying process comprises: immersing the substrate on which the tetraethyl orthosilicate is deposited in step 2 in the SiO2 sol in step 1 at room temperature for 1 second, pulling it away from the SiO2 sol at a pulling speed of 4.5 mm/s, and placing the pulled material in a muffle furnace at 90°C for drying for 10 minutes;
步骤302、将浸没干燥后料件置于420℃的快速热处理炉中烧制10min,完成碳素钢表面生长SiO2涂层;所述烧制的升温速率为120℃/min;Step 302, placing the immersed dried material in a rapid heat treatment furnace at 420°C for 10 minutes to complete the growth of SiO2 coating on the surface of the carbon steel; the heating rate of the sintering is 120°C/min;
本实施例的完成表面生长SiO2涂层的碳素钢性能与实施例1基本一致。The performance of the carbon steel with SiO2 coating grown on the surface in this embodiment is basically the same as that in embodiment 1.
实施例4Example 4
本实施例提供一种碳素钢表面生长SiO2涂层的方法,包括:This embodiment provides a method for growing a SiO2 coating on a carbon steel surface, comprising:
步骤一、提供SiO2溶胶,具体包括:Step 1: providing SiO2 sol, specifically comprising:
步骤101、将1mol正硅酸乙酯和10mol无水乙醇混合,于35℃搅拌1h,加入1mol去离子水,继续搅拌2h,得到溶液A;Step 101, 1 mol of tetraethyl orthosilicate and 10 mol of anhydrous ethanol were mixed, stirred at 35° C. for 1 h, 1 mol of deionized water was added, and stirring was continued for 2 h to obtain a solution A;
步骤102、向所述溶液A中加入氨水,至pH为11,得到悬浊液,所述悬浊液呈白色絮凝状;所述氨水的质量百分含量为12%;Step 102, adding ammonia water to the solution A until the pH value is 11, to obtain a suspension, wherein the suspension is white and flocculated; the mass percentage of the ammonia water is 12%;
步骤103、将所述悬浊液离心分离,得到颗粒物,用乙醇清洗所述颗粒物2次,将清洗后颗粒物于室温下放置2小时,使乙醇挥发;Step 103, centrifuging the suspension to obtain particles, washing the particles twice with ethanol, and placing the washed particles at room temperature for 2 hours to allow the ethanol to evaporate;
步骤104、将室温放置后颗粒物置于乙酰丙酮、无水乙醇和己烷的混合溶液中,于室温下超声30min后搅拌2h,得到SiO2溶胶;所述乙酰丙酮、无水乙醇和己烷的混合溶液中,乙酰丙酮的物质的量为步骤101所述正硅酸乙酯物质的量的6倍,无水乙醇的物质的量为步骤101所述正硅酸乙酯物质的量的10倍;己烷的物质的量为步骤101所述正硅酸乙酯物质的量的8倍;Step 104, placing the particles after standing at room temperature in a mixed solution of acetylacetone, anhydrous ethanol and hexane, ultrasonicating for 30 minutes at room temperature and then stirring for 2 hours to obtain SiO2 sol; in the mixed solution of acetylacetone, anhydrous ethanol and hexane, the amount of acetylacetone is 6 times the amount of the tetraethyl orthosilicate in step 101, the amount of anhydrous ethanol is 10 times the amount of the tetraethyl orthosilicate in step 101; the amount of hexane is 8 times the amount of the tetraethyl orthosilicate in step 101;
步骤二、在基板上蒸镀正硅酸乙酯,所述基板为钢材质基板,具体包括:Step 2: Evaporating tetraethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, specifically comprising:
步骤201、将尺寸为40mm×40mm的碳素钢依次用400#、1500#和3000#的砂纸进行打磨,抛光,清洗,得到基板;所述清洗为用无水乙醇进行清洗;所述碳素钢为20钢,所述20钢购买自天津中泰华营钢铁;Step 201, grinding, polishing and cleaning a carbon steel having a size of 40 mm×40 mm with 400#, 1500# and 3000# sandpaper in sequence to obtain a substrate; the cleaning is performed with anhydrous ethanol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Zhongtai Huaying Steel;
步骤202、将10ml正硅酸乙酯置于干净的烧杯中,将步骤201所述基板平放于烧杯上,将放置有基板的烧杯置于加热台上,加热台的温度为188℃,得到组装系统;所述烧杯的容量为25mL;所述加热台为JFTOOIS金锋平板加热台;Step 202, place 10 ml of tetraethyl orthosilicate in a clean beaker, place the substrate in step 201 flat on the beaker, place the beaker with the substrate on a heating table at a temperature of 188° C., and obtain an assembly system; the capacity of the beaker is 25 ml; the heating table is a JFTOOIS flat heating table;
步骤203、将上述组装系统在-0.28bar负压条件下保持40min,取出,在65℃烘箱中烘1h;所述负压条件下可以为将所述组装系统置于不锈钢容器中,抽真空至负压,密闭,所述抽真空所用泵功率为15w;Step 203, keeping the above-mentioned assembly system under negative pressure of -0.28 bar for 40 minutes, taking it out, and drying it in a 65° C. oven for 1 hour; the negative pressure condition may be placing the assembly system in a stainless steel container, evacuating to negative pressure, and sealing it, and the pump power used for evacuation is 15W;
步骤204、将基板翻转,重复步骤202和203,完成另一面蒸镀正硅酸乙酯;Step 204, turning over the substrate, repeating steps 202 and 203, and completing the evaporation of tetraethyl orthosilicate on the other side;
步骤三、在蒸镀有正硅酸乙酯的基板上生长SiO2涂层,具体包括:Step 3: growing a SiO2 coating on the substrate on which tetraethyl orthosilicate is evaporated, specifically comprising:
步骤301、将步骤二蒸镀有正硅酸乙酯的基板浸没干燥处理9次;所述浸没干燥处理包括:常温条件下,将步骤二蒸镀有正硅酸乙酯的基板浸没于步骤一所述SiO2溶胶中,保持5s,以5mm/s提拉速度拉离SiO2溶胶,将拉离后料件置于80℃马弗炉中干燥10min;Step 301, immersing and drying the substrate on which the tetraethyl orthosilicate is deposited in step 2 for 9 times; the immersion drying process comprises: immersing the substrate on which the tetraethyl orthosilicate is deposited in step 2 in the SiO2 sol in step 1 at room temperature for 5 seconds, pulling the substrate away from the SiO2 sol at a pulling speed of 5 mm/s, and placing the pulled substrate in a muffle furnace at 80°C for drying for 10 minutes;
步骤302、将浸没干燥后料件置于410℃的快速热处理炉中烧制10min,完成碳素钢表面生长SiO2涂层;所述烧制的升温速率为120℃/min;Step 302, placing the immersed dried material in a rapid heat treatment furnace at 410°C for 10 minutes to complete the growth of SiO2 coating on the surface of the carbon steel; the heating rate of the sintering is 120°C/min;
本实施例的完成表面生长SiO2涂层的碳素钢性能与实施例1基本一致。The performance of the carbon steel with SiO2 coating grown on the surface in this embodiment is basically the same as that in embodiment 1.
实施例5Example 5
本实施例提供一种碳素钢表面生长SiO2涂层的方法,包括:This embodiment provides a method for growing a SiO2 coating on a carbon steel surface, comprising:
步骤一、提供SiO2溶胶,具体包括:Step 1: providing SiO2 sol, specifically comprising:
步骤101、将1mol正硅酸乙酯和6mol无水乙醇混合,于40℃搅拌1h,加入2mol去离子水,继续搅拌2h,得到溶液A;Step 101, 1 mol of ethyl orthosilicate and 6 mol of anhydrous ethanol are mixed, stirred at 40° C. for 1 h, 2 mol of deionized water are added, and stirring is continued for 2 h to obtain a solution A;
步骤102、向所述溶液A中加入氨水,至pH为10,得到悬浊液,所述悬浊液呈白色絮凝状;所述氨水的质量百分含量为25%;Step 102, adding ammonia water to the solution A until the pH value is 10, to obtain a suspension, wherein the suspension is white and flocculated; the mass percentage of the ammonia water is 25%;
步骤103、将所述悬浊液离心分离,得到颗粒物,用乙醇清洗所述颗粒物4次,将清洗后颗粒物于室温下放置2小时,使乙醇挥发;Step 103, centrifuging the suspension to obtain particles, washing the particles with ethanol for 4 times, and placing the washed particles at room temperature for 2 hours to allow the ethanol to evaporate;
步骤104、将室温放置后颗粒物置于乙酰丙酮、无水乙醇和己烷的混合溶液中,于室温下超声40min后搅拌1h,得到SiO2溶胶;所述乙酰丙酮、无水乙醇和己烷的混合溶液中,乙酰丙酮的物质的量为步骤101所述正硅酸乙酯物质的量的10倍,无水乙醇的物质的量为步骤101所述正硅酸乙酯物质的量的6倍;己烷的物质的量为步骤101所述正硅酸乙酯物质的量的9倍;Step 104, placing the particles after standing at room temperature in a mixed solution of acetylacetone, anhydrous ethanol and hexane, ultrasonicating for 40 minutes at room temperature and then stirring for 1 hour to obtain SiO2 sol; in the mixed solution of acetylacetone, anhydrous ethanol and hexane, the amount of acetylacetone is 10 times the amount of the tetraethyl orthosilicate in step 101, the amount of anhydrous ethanol is 6 times the amount of the tetraethyl orthosilicate in step 101; the amount of hexane is 9 times the amount of the tetraethyl orthosilicate in step 101;
步骤二、在基板上蒸镀正硅酸乙酯,所述基板为钢材质基板,具体包括:Step 2: Evaporating tetraethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, specifically comprising:
步骤201、将尺寸为40mm×40mm的碳素钢依次用400#、1500#和3000#的砂纸进行打磨,抛光,清洗,得到基板;所述清洗为用无水乙醇进行清洗;所述碳素钢为20钢,所述20钢购买自天津中泰华营钢铁;Step 201, grinding, polishing and cleaning a carbon steel having a size of 40 mm×40 mm with 400#, 1500# and 3000# sandpaper in sequence to obtain a substrate; the cleaning is performed with anhydrous ethanol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Zhongtai Huaying Steel;
步骤202、将5ml正硅酸乙酯置于干净的烧杯中,将步骤201所述基板平放于烧杯上,将放置有基板的烧杯置于加热台上,加热台的温度为187℃,得到组装系统;所述烧杯的容量为25mL;所述加热台为JFTOOIS金锋平板加热台;Step 202, place 5 ml of tetraethyl orthosilicate in a clean beaker, place the substrate described in step 201 flat on the beaker, place the beaker with the substrate on a heating table at a temperature of 187° C., and obtain an assembled system; the capacity of the beaker is 25 ml; the heating table is a JFTOOIS flat heating table;
步骤203、将上述组装系统在-0.25bar负压条件下保持30min,取出,在60℃烘箱中烘2h;所述负压条件下可以为将所述组装系统置于不锈钢容器中,抽真空至负压,密闭,所述抽真空所用泵功率为15w;Step 203, keeping the above-mentioned assembly system under negative pressure of -0.25 bar for 30 minutes, taking it out, and drying it in a 60° C. oven for 2 hours; the negative pressure condition may be placing the assembly system in a stainless steel container, evacuating to negative pressure, and sealing it, and the pump power used for the evacuation is 15W;
步骤204、将基板翻转,重复步骤202和203,完成另一面蒸镀正硅酸乙酯;Step 204, turning over the substrate, repeating steps 202 and 203, and completing the evaporation of tetraethyl orthosilicate on the other side;
步骤三、在蒸镀有正硅酸乙酯的基板上生长SiO2涂层,具体包括:Step 3: growing a SiO2 coating on the substrate on which tetraethyl orthosilicate is evaporated, specifically comprising:
步骤301、将步骤二蒸镀有正硅酸乙酯的基板浸没干燥处理5次;所述浸没干燥处理包括:常温条件下,将步骤二蒸镀有正硅酸乙酯的基板浸没于步骤一所述SiO2溶胶中,保持3s,以4mm/s提拉速度拉离SiO2溶胶,将拉离后料件置于100℃马弗炉中干燥10min;Step 301, immersing and drying the substrate on which the tetraethyl orthosilicate is deposited in step 2 for 5 times; the immersion drying process comprises: immersing the substrate on which the tetraethyl orthosilicate is deposited in step 2 in the SiO2 sol in step 1 at room temperature for 3 seconds, pulling the substrate away from the SiO2 sol at a pulling speed of 4 mm/s, and placing the pulled substrate in a muffle furnace at 100°C for drying for 10 minutes;
步骤302、将浸没干燥后料件置于440℃的快速热处理炉中烧制10min,完成碳素钢表面生长SiO2涂层;所述烧制的升温速率为120℃/min;Step 302, placing the immersed dried material in a rapid heat treatment furnace at 440°C for 10 minutes to complete the growth of SiO2 coating on the surface of the carbon steel; the heating rate of the sintering is 120°C/min;
本实施例的完成表面生长SiO2涂层的碳素钢性能与实施例1基本一致。The performance of the carbon steel with SiO2 coating grown on the surface in this embodiment is basically the same as that in embodiment 1.
以上所述,仅是本发明的较佳实施例,并非对本发明做任何限制,凡是根据发明技术实质对以上实施例所作的任何简单修改、变更以及等效结构变化,均仍属于本发明技术方案的保护范围内。The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent structural change made to the above embodiment according to the technical essence of the invention shall still fall within the protection scope of the technical solution of the present invention.
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