CN115627459B - SiO grows on carbon steel surface2Method of coating - Google Patents

SiO grows on carbon steel surface2Method of coating Download PDF

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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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sio
coating
carbon steel
substrate
growing
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CN115627459A (en
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贠柯
张澄
陈梦诗
王博
王若虹
刘金娥
毕成
杨旭
任洋
刘萍
鲁元
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Xian University of Technology
Xian Special Equipment Inspection and Testing Institute
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Xian Special Equipment Inspection and Testing Institute
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/02Chemical 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
    • C23C18/12Chemical 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
    • C23C18/1204Chemical 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
    • C23C18/1208Oxides, e.g. ceramics
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/12Organic material
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/02Chemical 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
    • C23C18/12Chemical 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
    • C23C18/1229Composition of the substrate
    • C23C18/1241Metallic substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/02Chemical 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
    • C23C18/12Chemical 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
    • C23C18/125Process of deposition of the inorganic material
    • C23C18/1254Sol or sol-gel processing

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Abstract

The invention discloses a method for growing a SiO 2 coating on the surface of carbon steel, which comprises the following steps: step one, preparing SiO 2 sol; placing the substrate on a beaker filled with tetraethoxysilane, placing the beaker with the substrate on a heating table to obtain an assembly system, carrying out negative pressure treatment on the assembly system, drying to finish evaporation of tetraethoxysilane on one side, turning the substrate over, repeating the operation, and finishing evaporation of tetraethoxysilane on the other side; and thirdly, immersing and drying the substrate evaporated with the tetraethoxysilane, and then firing to complete the growth of the SiO 2 coating on the surface of the carbon steel. According to the method for growing the SiO 2 coating on the carbon steel surface, the SiO 2 coating is grown on the carbon steel surface evaporated with tetraethoxysilane by using a lifting dipping method, so that the uniform coating on the two surfaces of the steel plate is coated at one time, the SiO 2 coating has strong bonding property with the steel plate, good spreadability is achieved, and the performances of high chemical stability and good corrosion resistance of the SiO 2 coating can be fully utilized to realize corrosion resistance of the steel plate.

Description

Method for growing SiO 2 coating on carbon steel surface
Technical Field
The invention belongs to the technical field of corrosion prevention, and particularly relates to a method for growing a SiO 2 coating on the surface of carbon steel.
Background
In recent years, carbon steel (20 steel) has been an important part in the construction of thermal pipelines. However, since 20 steel is commonly exposed to air such as humid soil, the surface of the 20 steel is extremely susceptible to react with oxygen, moisture and the like, which results in rust and greatly affects the service life of the heat distribution pipeline.
In order to solve the corrosion-resistant problem of the heating power pipeline, a method of adding an organic protective layer is mainly adopted at present, and the aim of corrosion resistance of the outer layer of the steel pipe is achieved by isolating 20 steel from outside air or water. However, the organic material has the defect of lower strength, and a protection notch corrosion point is often generated due to scratch in the process of pipeline construction and maintenance, so that the reduction of the service life of steel is further accelerated. In addition, the pipeline interfaces, valves and other position structures are complex, and organic layers are difficult to effectively coat, so that the interfaces, the valves and the like become weak links in corrosion prevention of a heating power pipeline system. In addition, corrosion of the inner wall of the steel pipe caused by the operation process of the heating power pipeline is often difficult to pay effective attention. The method for effectively preventing corrosion of the 20 steel pipes is one of main ways for solving the corrosion of the current thermal pipelines.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for growing SiO 2 coating on the surface of carbon steel aiming at the defects in the prior art. According to the method, the SiO 2 coating is grown on the surface of the carbon steel evaporated with the tetraethoxysilane by using a lifting dipping method, so that the uniform coating is coated on the two surfaces of the steel plate at one time, the SiO 2 coating has strong bonding property with the steel plate, good spreadability is achieved, the performances of high chemical stability and good corrosion resistance of the SiO 2 coating can be fully utilized, and the corrosion resistance of the steel plate is realized.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for growing a SiO 2 coating on the surface of carbon steel, which is characterized by comprising the following steps:
step one, providing SiO 2 sol, which specifically comprises the following steps:
step 101, mixing tetraethoxysilane and absolute ethyl alcohol, stirring for 1-2 hours at 25-40 ℃, adding deionized water, and continuously stirring for 1-2 hours to obtain a solution A;
102, adding ammonia water into the solution A until the pH value is 10-11 to obtain a suspension;
Step 103, centrifugally separating the suspension to obtain particles, washing the particles with ethanol, and then standing at room temperature;
104, placing the particles after being placed at room temperature into a mixed solution of acetylacetone, absolute ethyl alcohol and hexane, and stirring for 1-2 h after ultrasonic treatment for 30-40 min at room temperature to obtain SiO 2 sol;
evaporating tetraethoxysilane on a substrate, which specifically comprises the following steps:
Step 201, grinding, polishing and cleaning raw steel to obtain a substrate; the raw steel is carbon steel;
Step 202, placing 5-15 mL of ethyl orthosilicate in a clean beaker, placing the substrate in the step 201 on the beaker, and placing the beaker with the substrate on a heating table to obtain an assembly system;
203, maintaining the assembly system at negative pressure of-0.28 bar to-0.2 bar for 30min to 40min, taking out, and drying in a drying oven at 60 ℃ to 65 ℃ for 1h to 2h;
step 204, turning over the substrate, repeating the steps 202 and 203, and completing evaporation of ethyl orthosilicate on the other side;
Step three, growing a SiO 2 coating on the substrate evaporated with the tetraethoxysilane, which specifically comprises the following steps:
Step 301, immersing and drying the substrate evaporated with the tetraethoxysilane in the step two for 5 to 10 times;
and 302, firing the immersed and dried material piece to complete the growth of the SiO 2 coating on the surface of the carbon steel.
The method for growing the SiO 2 coating on the surface of the carbon steel is characterized in that in the step 101, the amount of the absolute ethyl alcohol is 5-10 times that of the tetraethoxysilane.
The method for growing the SiO 2 coating on the surface of the carbon steel is characterized in that in the step 101, the amount of the deionized water is 1-2 times of the amount of the tetraethoxysilane.
The method for growing the SiO 2 coating on the surface of the carbon steel is characterized in that in the step 102, the mass percentage of the ammonia water is 10% -25%.
In the above method for growing a SiO 2 coating on the surface of carbon steel, in step 104, the amount of acetylacetone substance in the mixed solution of acetylacetone, absolute ethyl alcohol and hexane is 6-10 times that of ethyl orthosilicate substance in step 101, and the amount of absolute ethyl alcohol substance is 5-10 times that of ethyl orthosilicate substance in step 101; the amount of hexane is 5 to 10 times the amount of ethyl orthosilicate material described in step 101.
The method for growing the SiO 2 coating on the surface of the carbon steel is characterized in that in the step 202, the temperature of the heating table is 185-190 ℃.
The method for growing the SiO 2 coating on the surface of the carbon steel is characterized in that in step 301, the immersion drying treatment comprises the following steps: under the normal temperature condition, the substrate which is evaporated with tetraethoxysilane in the second step is immersed in the SiO 2 sol in the first step, the SiO 2 sol is pulled away at the pulling speed of 4-5 mm/s, and the pulled-away material piece is dried at the temperature of 80-100 ℃.
The method for growing the SiO 2 coating on the surface of the carbon steel is characterized in that in the step 302, the firing temperature is 400-450 ℃.
Compared with the prior art, the invention has the following advantages:
1. According to the method for growing the SiO 2 coating on the carbon steel surface, the SiO 2 coating is grown on the carbon steel surface evaporated with tetraethoxysilane by using a lifting dipping method, so that the uniform coating on the two surfaces of the steel plate is coated once, the SiO 2 coating has strong bonding property with the steel plate, good spreadability is achieved, the performances of high chemical stability and good corrosion resistance of the SiO 2 coating can be fully utilized, and the corrosion resistance of the steel plate is realized.
2. The method of the invention comprises vapor plating carbon steel by adopting tetraethoxysilane before growing SiO 2 coating, which can effectively improve the surface tension of carbon steel and avoid the shrinkage film of SiO 2 coating.
3. The method is simple, easy to operate and suitable for popularization and application.
The technical scheme of the invention is further described in detail below with reference to the examples.
Detailed Description
According to the invention, the SiO 2 coating grows on the surface of the carbon steel, and the SiO 2 coating grows on the substrate on which the tetraethoxysilane is evaporated, wherein the temperature of the tetraethoxysilane is 185-190 ℃, the negative pressure is minus 0.28bar to minus 0.2bar, the temperature of the fired SiO 2 sol is 400-450 ℃, so that the substrate on which the tetraethoxysilane is evaporated with proper condensation quantity is obtained, and further the SiO 2 gel film with an effective anti-corrosion effect is obtained.
Example 1
The embodiment provides a method for growing a SiO 2 coating on the surface of carbon steel, which comprises the following steps:
step one, providing SiO 2 sol, which specifically comprises the following steps:
step 101, mixing 1mol of ethyl orthosilicate with 5mol of absolute ethyl alcohol, stirring for 1h at 25 ℃, adding 1mol of deionized water, and continuing stirring for 1h to obtain a solution A;
102, adding ammonia water into the solution A until the pH value is 10 to obtain a suspension, wherein the suspension is in a white flocculent shape; the mass percentage of the ammonia water is 10%;
step 103, centrifugally separating the suspension to obtain particles, washing the particles with ethanol for 2 times, and standing the washed particles at room temperature for 2 hours to volatilize the ethanol;
104, placing the particles after being placed at room temperature into a mixed solution of acetylacetone, absolute ethyl alcohol and hexane, and stirring for 1h after ultrasonic treatment for 30min at room temperature to obtain SiO 2 sol; in the mixed solution of the acetylacetone, the absolute ethyl alcohol and the hexane, the amount of the acetylacetone is 6 times of the amount of the ethyl orthosilicate in the step 101, and the amount of the absolute ethyl alcohol is 5 times of the amount of the ethyl orthosilicate in the step 101; the amount of hexane is 5 times the amount of ethyl orthosilicate material described in step 101;
Evaporating ethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, and specifically comprises the following steps:
step 201, grinding, polishing and cleaning carbon steel with the size of 40mm multiplied by 40mm by using 400# abrasive paper, 1500# abrasive paper and 3000# abrasive paper in sequence to obtain a substrate; the cleaning is carried out by using absolute ethyl alcohol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Heaihua Ying iron and steel;
Step 202, placing 5ml of ethyl orthosilicate in a clean beaker, placing the substrate in the step 201 on the beaker, placing the beaker with the substrate on a heating table, wherein the temperature of the heating table is 185 ℃, and obtaining an assembly system; the capacity of the beaker is 25mL; the heating table is JFTOOIS golden front flat plate heating table;
Step 203, keeping the assembly system under negative pressure of-0.26 bar for 30min, taking out, and drying in a 60 ℃ oven for 1h; the assembly system is placed in a stainless steel container under the negative pressure condition, and is vacuumized to be negative pressure and sealed, and the pump power for vacuumizing is 15w;
step 204, turning over the substrate, repeating the steps 202 and 203, and completing evaporation of ethyl orthosilicate on the other side;
Step three, growing a SiO 2 coating on the substrate evaporated with the tetraethoxysilane, which specifically comprises the following steps:
Step 301, immersing and drying the substrate evaporated with the tetraethoxysilane in the step two for 5 times; the immersion drying treatment includes: under the normal temperature condition, immersing the substrate evaporated with the tetraethoxysilane in the step II in the SiO 2 sol in the step I, keeping for 3s, pulling the SiO 2 sol at a pulling speed of 4mm/s, and placing the pulled material piece in a muffle furnace at 80 ℃ for drying for 10min; the normal temperature is 20-25 ℃;
Step 302, placing the immersed and dried material piece in a rapid heat treatment furnace at 400 ℃ for firing for 10min, and finishing the growth of SiO 2 coating on the carbon steel surface; the firing temperature rising rate is 120 ℃/min.
The hydrochloric acid corrosion performance test is carried out after the carbon steel surface waste part with the SiO 2 coating growing on the surface is partially cut off, and the test method comprises the following steps: immersing the carbon steel in 0.1mol/L dilute hydrochloric acid for 4 hours, and observing the surface corrosion trace. The result shows that the surface of the carbon steel has no corrosion trace, and the carbon steel with the SiO 2 coating on the surface obtained by the method has even and compact coating, can effectively wrap the carbon steel plate and has better anti-corrosion effect.
Example 2
The embodiment provides a method for growing a SiO 2 coating on the surface of carbon steel, which comprises the following steps:
step one, providing SiO 2 sol, which specifically comprises the following steps:
Step 101, mixing 1mol of ethyl orthosilicate with 10mol of absolute ethyl alcohol, stirring for 2 hours at 40 ℃, adding 2mol of deionized water, and continuing stirring for 2 hours to obtain a solution A;
102, adding ammonia water into the solution A until the pH value is 11 to obtain a suspension, wherein the suspension is in a white flocculent shape; the mass percentage of the ammonia water is 25%;
Step 103, centrifugally separating the suspension to obtain particles, washing the particles with ethanol for 4 times, and standing the washed particles at room temperature for 2 hours to volatilize the ethanol;
104, placing the particles after being placed at room temperature into a mixed solution of acetylacetone, absolute ethyl alcohol and hexane, and stirring for 2 hours after ultrasonic treatment at room temperature for 40 minutes to obtain SiO 2 sol; in the mixed solution of the acetylacetone, the absolute ethyl alcohol and the hexane, the amount of the acetylacetone is 10 times of the amount of the ethyl orthosilicate in the step 101, and the amount of the absolute ethyl alcohol is 10 times of the amount of the ethyl orthosilicate in the step 101; the amount of hexane is 10 times the amount of ethyl orthosilicate material described in step 101;
Evaporating ethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, and specifically comprises the following steps:
step 201, grinding, polishing and cleaning carbon steel with the size of 40mm multiplied by 40mm by using 400# abrasive paper, 1500# abrasive paper and 3000# abrasive paper in sequence to obtain a substrate; the cleaning is carried out by using absolute ethyl alcohol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Heaihua Ying iron and steel;
step 202, placing 10ml of ethyl orthosilicate in a clean beaker, placing the substrate in the step 201 on the beaker, placing the beaker with the substrate on a heating table, wherein the temperature of the heating table is 190 ℃, and obtaining an assembly system; the capacity of the beaker is 25mL; the heating table is JFTOOIS golden front flat plate heating table;
Step 203, keeping the assembly system under negative pressure of-0.23 bar for 40min, taking out, and drying in a 65 ℃ oven for 2h; the assembly system is placed in a stainless steel container under the negative pressure condition, and is vacuumized to be negative pressure and sealed, and the pump power for vacuumizing is 15w;
step 204, turning over the substrate, repeating the steps 202 and 203, and completing evaporation of ethyl orthosilicate on the other side;
Step three, growing a SiO 2 coating on the substrate evaporated with the tetraethoxysilane, which specifically comprises the following steps:
Step 301, immersing and drying the substrate evaporated with the tetraethoxysilane in the step two for 10 times; the immersion drying treatment includes: under the normal temperature condition, immersing the substrate evaporated with the tetraethoxysilane in the step II in the SiO 2 sol in the step I, keeping for 2s, pulling the SiO 2 sol at a pulling speed of 5mm/s, and placing the pulled material piece in a muffle furnace at 100 ℃ for drying for 10min;
step 302, placing the immersed and dried material piece in a muffle furnace at 450 ℃ for firing for 10min, and finishing the growth of a SiO 2 coating on the surface of the carbon steel; the firing temperature rising rate is 120 ℃/min.
The carbon steel properties of the finished surface grown SiO 2 coating of this example are substantially identical to those of example 1.
Example 3
The embodiment provides a method for growing a SiO 2 coating on the surface of carbon steel, which comprises the following steps:
step one, providing SiO 2 sol, which specifically comprises the following steps:
step 101, mixing 1mol of ethyl orthosilicate with 7mol of absolute ethyl alcohol, stirring for 2 hours at 30 ℃, adding 1mol of deionized water, and continuing stirring for 1 hour to obtain a solution A;
102, adding ammonia water into the solution A until the pH value is 10 to obtain a suspension, wherein the suspension is in a white flocculent shape; the mass percentage of the ammonia water is 20%;
step 103, centrifugally separating the suspension to obtain particles, washing the particles with ethanol for 3 times, and standing the washed particles at room temperature for 2 hours to volatilize the ethanol;
104, placing the particles after being placed at room temperature into a mixed solution of acetylacetone, absolute ethyl alcohol and hexane, and stirring for 2 hours after ultrasonic treatment at room temperature for 35min to obtain SiO 2 sol; in the mixed solution of the acetylacetone, the absolute ethyl alcohol and the hexane, the amount of the acetylacetone is 8 times of the amount of the ethyl orthosilicate in the step 101, and the amount of the absolute ethyl alcohol is 7 times of the amount of the ethyl orthosilicate in the step 101; the amount of hexane is 10 times the amount of ethyl orthosilicate material described in step 101;
Evaporating ethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, and specifically comprises the following steps:
step 201, grinding, polishing and cleaning carbon steel with the size of 40mm multiplied by 40mm by using 400# abrasive paper, 1500# abrasive paper and 3000# abrasive paper in sequence to obtain a substrate; the cleaning is carried out by using absolute ethyl alcohol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Heaihua Ying iron and steel;
step 202, placing 15ml of ethyl orthosilicate in a clean beaker, placing the substrate in the step 201 on the beaker, placing the beaker with the substrate on a heating table, wherein the temperature of the heating table is 185 ℃, and obtaining an assembly system; the capacity of the beaker is 25mL; the heating table is JFTOOIS golden front flat plate heating table;
step 203, keeping the assembly system under negative pressure of-0.2 bar for 35min, taking out, and drying in a 60 ℃ oven for 2h; the assembly system is placed in a stainless steel container under the negative pressure condition, and is vacuumized to be negative pressure and sealed, and the pump power for vacuumizing is 15w;
step 204, turning over the substrate, repeating the steps 202 and 203, and completing evaporation of ethyl orthosilicate on the other side;
Step three, growing a SiO 2 coating on the substrate evaporated with the tetraethoxysilane, which specifically comprises the following steps:
Step 301, immersing and drying the substrate evaporated with the tetraethoxysilane in the step two for 8 times; the immersion drying treatment includes: under the normal temperature condition, immersing the substrate evaporated with the tetraethoxysilane in the step II in the SiO 2 sol in the step I, keeping for 1s, pulling the SiO 2 sol at a pulling speed of 4.5mm/s, and drying the pulled material in a muffle furnace at 90 ℃ for 10min;
step 302, placing the immersed and dried material piece in a rapid heat treatment furnace at 420 ℃ for firing for 10min, and finishing the growth of SiO 2 coating on the carbon steel surface; the heating rate of the firing is 120 ℃/min;
the carbon steel properties of the finished surface grown SiO 2 coating of this example are substantially identical to those of example 1.
Example 4
The embodiment provides a method for growing a SiO 2 coating on the surface of carbon steel, which comprises the following steps:
step one, providing SiO 2 sol, which specifically comprises the following steps:
Step 101, mixing 1mol of ethyl orthosilicate with 10mol of absolute ethyl alcohol, stirring for 1h at 35 ℃, adding 1mol of deionized water, and continuously stirring for 2h to obtain a solution A;
102, adding ammonia water into the solution A until the pH value is 11 to obtain a suspension, wherein the suspension is in a white flocculent shape; the mass percentage of the ammonia water is 12%;
step 103, centrifugally separating the suspension to obtain particles, washing the particles with ethanol for 2 times, and standing the washed particles at room temperature for 2 hours to volatilize the ethanol;
104, placing the particles after being placed at room temperature into a mixed solution of acetylacetone, absolute ethyl alcohol and hexane, and stirring for 2 hours after ultrasonic treatment for 30 minutes at room temperature to obtain SiO 2 sol; in the mixed solution of the acetylacetone, the absolute ethyl alcohol and the hexane, the amount of the acetylacetone is 6 times of the amount of the ethyl orthosilicate in the step 101, and the amount of the absolute ethyl alcohol is 10 times of the amount of the ethyl orthosilicate in the step 101; the amount of hexane is 8 times the amount of ethyl orthosilicate material described in step 101;
Evaporating ethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, and specifically comprises the following steps:
step 201, grinding, polishing and cleaning carbon steel with the size of 40mm multiplied by 40mm by using 400# abrasive paper, 1500# abrasive paper and 3000# abrasive paper in sequence to obtain a substrate; the cleaning is carried out by using absolute ethyl alcohol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Heaihua Ying iron and steel;
Step 202, placing 10ml of ethyl orthosilicate in a clean beaker, placing the substrate in the step 201 on the beaker, placing the beaker with the substrate on a heating table, wherein the temperature of the heating table is 188 ℃, and obtaining an assembly system; the capacity of the beaker is 25mL; the heating table is JFTOOIS golden front flat plate heating table;
Step 203, keeping the assembly system under negative pressure of-0.28 bar for 40min, taking out, and drying in a 65 ℃ oven for 1h; the assembly system is placed in a stainless steel container under the negative pressure condition, and is vacuumized to be negative pressure and sealed, and the pump power for vacuumizing is 15w;
step 204, turning over the substrate, repeating the steps 202 and 203, and completing evaporation of ethyl orthosilicate on the other side;
Step three, growing a SiO 2 coating on the substrate evaporated with the tetraethoxysilane, which specifically comprises the following steps:
Step 301, immersing and drying the substrate evaporated with the tetraethoxysilane in the step two for 9 times; the immersion drying treatment includes: under the normal temperature condition, immersing the substrate evaporated with the tetraethoxysilane in the step II in the SiO 2 sol in the step I, keeping for 5s, pulling the SiO 2 sol at a pulling speed of 5mm/s, and placing the pulled material piece in a muffle furnace at 80 ℃ for drying for 10min;
step 302, placing the immersed and dried material piece in a rapid heat treatment furnace at 410 ℃ for firing for 10min, and finishing the growth of SiO 2 coating on the carbon steel surface; the heating rate of the firing is 120 ℃/min;
the carbon steel properties of the finished surface grown SiO 2 coating of this example are substantially identical to those of example 1.
Example 5
The embodiment provides a method for growing a SiO 2 coating on the surface of carbon steel, which comprises the following steps:
step one, providing SiO 2 sol, which specifically comprises the following steps:
Step 101, mixing 1mol of ethyl orthosilicate with 6mol of absolute ethyl alcohol, stirring for 1h at 40 ℃, adding 2mol of deionized water, and continuously stirring for 2h to obtain a solution A;
102, adding ammonia water into the solution A until the pH value is 10 to obtain a suspension, wherein the suspension is in a white flocculent shape; the mass percentage of the ammonia water is 25%;
Step 103, centrifugally separating the suspension to obtain particles, washing the particles with ethanol for 4 times, and standing the washed particles at room temperature for 2 hours to volatilize the ethanol;
104, placing the particles after being placed at room temperature into a mixed solution of acetylacetone, absolute ethyl alcohol and hexane, and stirring for 1h after ultrasonic treatment at room temperature for 40min to obtain SiO 2 sol; in the mixed solution of the acetylacetone, the absolute ethyl alcohol and the hexane, the amount of the acetylacetone is 10 times of the amount of the ethyl orthosilicate in the step 101, and the amount of the absolute ethyl alcohol is 6 times of the amount of the ethyl orthosilicate in the step 101; the amount of hexane material was 9 times the amount of ethyl orthosilicate material described in step 101;
Evaporating ethyl orthosilicate on a substrate, wherein the substrate is a steel substrate, and specifically comprises the following steps:
step 201, grinding, polishing and cleaning carbon steel with the size of 40mm multiplied by 40mm by using 400# abrasive paper, 1500# abrasive paper and 3000# abrasive paper in sequence to obtain a substrate; the cleaning is carried out by using absolute ethyl alcohol; the carbon steel is 20 steel, and the 20 steel is purchased from Tianjin Heaihua Ying iron and steel;
Step 202, placing 5ml of ethyl orthosilicate in a clean beaker, placing the substrate in the step 201 on the beaker, placing the beaker with the substrate on a heating table, wherein the temperature of the heating table is 187 ℃, and obtaining an assembly system; the capacity of the beaker is 25mL; the heating table is JFTOOIS golden front flat plate heating table;
step 203, keeping the assembly system under negative pressure of-0.25 bar for 30min, taking out, and drying in a 60 ℃ oven for 2h; the assembly system is placed in a stainless steel container under the negative pressure condition, and is vacuumized to be negative pressure and sealed, and the pump power for vacuumizing is 15w;
step 204, turning over the substrate, repeating the steps 202 and 203, and completing evaporation of ethyl orthosilicate on the other side;
Step three, growing a SiO 2 coating on the substrate evaporated with the tetraethoxysilane, which specifically comprises the following steps:
Step 301, immersing and drying the substrate evaporated with the tetraethoxysilane in the step two for 5 times; the immersion drying treatment includes: under the normal temperature condition, immersing the substrate evaporated with the tetraethoxysilane in the step II in the SiO 2 sol in the step I, keeping for 3s, pulling the SiO 2 sol at a pulling speed of 4mm/s, and placing the pulled material piece in a muffle furnace at 100 ℃ for drying for 10min;
Step 302, placing the immersed and dried material piece in a rapid heat treatment furnace at 440 ℃ for firing for 10min, and finishing the growth of SiO 2 coating on the carbon steel surface; the heating rate of the firing is 120 ℃/min;
the carbon steel properties of the finished surface grown SiO 2 coating of this example are substantially identical to those of example 1.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent structural changes of the above embodiment according to the technical matter of the present invention still fall within the scope of the technical solution of the present invention.

Claims (8)

1. A method for growing a SiO 2 coating on the surface of carbon steel, which is characterized by comprising the following steps:
step one, providing SiO 2 sol, which specifically comprises the following steps:
step 101, mixing tetraethoxysilane and absolute ethyl alcohol, stirring for 1-2 hours at 25-40 ℃, adding deionized water, and continuously stirring for 1-2 hours to obtain a solution A;
102, adding ammonia water into the solution A until the pH value is 10-11 to obtain a suspension;
Step 103, centrifugally separating the suspension to obtain particles, washing the particles with ethanol, and then standing at room temperature;
104, placing the particles after being placed at room temperature into a mixed solution of acetylacetone, absolute ethyl alcohol and hexane, and stirring for 1-2 h after ultrasonic treatment for 30-40 min at room temperature to obtain SiO 2 sol;
evaporating tetraethoxysilane on a substrate, which specifically comprises the following steps:
Step 201, grinding, polishing and cleaning raw steel to obtain a substrate; the raw steel is carbon steel;
Step 202, placing 5-15 mL of ethyl orthosilicate in a clean beaker, placing the substrate in the step 201 on the beaker, and placing the beaker with the substrate on a heating table to obtain an assembly system;
203, maintaining the assembly system at negative pressure of-0.28 bar to-0.2 bar for 30min to 40min, taking out, and drying in a drying oven at 60 ℃ to 65 ℃ for 1h to 2h;
step 204, turning over the substrate, repeating the steps 202 and 203, and completing evaporation of ethyl orthosilicate on the other side;
Step three, growing a SiO 2 coating on the substrate evaporated with the tetraethoxysilane, which specifically comprises the following steps:
Step 301, immersing and drying the substrate evaporated with the tetraethoxysilane in the step two for 5 to 10 times;
and 302, firing the immersed and dried material piece to complete the growth of the SiO 2 coating on the surface of the carbon steel.
2. The method for growing a SiO 2 coating on a carbon steel surface according to claim 1, wherein in step 101, the amount of the absolute ethyl alcohol is 5-10 times the amount of the tetraethyl orthosilicate.
3. The method for growing a SiO 2 coating on a carbon steel surface according to claim 1, wherein in step 101, the amount of deionized water is 1 to 2 times the amount of ethyl orthosilicate.
4. The method for growing a SiO 2 coating on the surface of carbon steel according to claim 1, wherein in step 102, the mass percentage of the ammonia water is 10% -25%.
5. The method for growing a SiO 2 coating on the surface of carbon steel according to claim 1, wherein in step 104, the amount of acetylacetone substance in the mixed solution of acetylacetone, absolute ethyl alcohol and hexane is 6-10 times the amount of ethyl orthosilicate substance in step 101, and the amount of absolute ethyl alcohol substance is 5-10 times the amount of ethyl orthosilicate substance in step 101; the amount of hexane is 5 to 10 times the amount of ethyl orthosilicate material described in step 101.
6. A method for growing a SiO 2 coating on a carbon steel surface according to claim 1, wherein in step 202, the temperature of the heating table is 185 ℃ to 190 ℃.
7. A method for growing a SiO 2 coating on a carbon steel surface according to claim 1, wherein in step 301, the submerged drying process comprises: under the normal temperature condition, the substrate which is evaporated with tetraethoxysilane in the second step is immersed in the SiO 2 sol in the first step, the SiO 2 sol is pulled away at the pulling speed of 4-5 mm/s, and the pulled-away material piece is dried at the temperature of 80-100 ℃.
8. A method of growing a SiO 2 coating on a carbon steel surface according to claim 1, wherein in step 302, the firing temperature is from 400 ℃ to 450 ℃.
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