CN113637958B - SiO with high bonding strength 2 /α-Al 2 O 3 Ceramic composite coating and low-temperature preparation method thereof - Google Patents
SiO with high bonding strength 2 /α-Al 2 O 3 Ceramic composite coating and low-temperature preparation method thereof Download PDFInfo
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- 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
- 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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- 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
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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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
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
- C23C18/127—Preformed particles
Abstract
The invention discloses SiO with high bonding strength 2 /α‑Al 2 O 3 And (3) a ceramic composite coating. The invention discloses the SiO with high bonding strength 2 /α‑Al 2 O 3 The low-temperature preparation method of the ceramic composite coating comprises the following steps: step 1, polishing a substrate, then ultrasonically cleaning, and drying to obtain a pretreated substrate; step 2, mixing alpha-Al 2 O 3 Mixing the powder with alkaline silica sol and polyethylene glycol, performing ultrasonic treatment, and uniformly stirring to obtain slurry; step 3, spin-coating the slurry on the surface of the pre-processed substrate to obtain a pre-processed ceramic coating substrate; step 4, sintering the pretreated ceramic coating substrate, heating to 500-700 ℃ at the speed of 0.5-2 ℃/min, preserving heat for 0.5-1.5h, and cooling to room temperature at the speed of 0.5-2 ℃/min to obtain SiO 2 /α‑Al 2 O 3 A ceramic composite coating. The ceramic composite coating obtained by the invention has uniform and compact coating, small thickness and high bonding strength with a matrix.
Description
Technical Field
The invention relates to the technical field of tritium-resistant coatings, in particular to SiO with high bonding strength 2 /α-Al 2 O 3 A ceramic composite coating and a low-temperature preparation method thereof.
Background
One key problem in the implementation of fusion reactors is the prevention of tritium permeation in structural materials, and a common approach to this problem is to prepare tritium-resistant coatings on the surface of the structural materials.
The ceramic is the first choice of the tritium-resistant coating material due to the advantages of high strength, high temperature resistance, low tritium permeability and the like. The tritium-resistant ceramic coating can be divided into an oxide coating, a non-oxide coating and a composite coating thereof. The oxide ceramic coating has the advantages of high melting point, stable chemical property, relatively simple preparation process, good tritium resistance and the like, and mainly comprises Cr 2 O 3 、Y 2 O 3 、Er 2 O 3 、Al 2 O 3 、 SiO 2 And the like. Wherein SiO is 2 The coating has the advantages of high strength, high melting point, stable physicochemical properties and the like, and is widely applied to the substrate material of the ceramic coating on the surface of the metal matrix. But SiO 2 Coatings still suffer from a number of problems, such as SiO prepared by sol-gel processes 2 After the coating is formed into a film, holes and cracks are easily generated on the surface, and the bonding strength of the coating is seriously influenced. Through a series of researches, the doping of the metal oxide can effectively improve the bonding strength of the silicon-based coating. For example: to SiO 2 Adding Al into 2 O 3 、Y 2 O 3 And Er 2 O 3 And the bonding strength of the intermolecular chemical bonds and the occlusion strength of the coating and the substrate can be enhanced, and the bonding strength of the coating and the substrate can be obviously improved.
The preparation technology of the ceramic coating mainly comprises a matrix surface coating deposition technology, such as magnetron sputtering, plasma spraying, hot dip aluminum plating, fused salt electroplating, embedding infiltration, a metal organic decomposition method and the like. However, magnetron sputtering has serious limitations for preparing coatings on the inner surfaces of special-shaped parts such as the inner wall of a pipeline and the like; the coating prepared by the plasma spraying technology has cracks and holes, and the preparation temperature is high, so that the heat influence is generated on the matrix; the application range of the hot dip aluminum plating and molten salt electroplating technology is small and is only limited to preparing an aluminide coating; the chloride ions in the chloride used as an activator in pack cementation lead to severe stress corrosion of the structural material. In addition, the preparation techniques all have the defects of complex process, higher cost, high production technical requirement and the like.
Compared with the preparation technology, the slurry method is a reliable method for preparing the ceramic coating at low temperature, but because the uniformity and thickness of the coating are difficult to control by the traditional slurry brushing and dipping methods, the prepared ceramic coating has the problems of uneven structure, large thickness and the like, and the bonding strength between the coating and a substrate is influenced.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides SiO with high bonding strength 2 /α-Al 2 O 3 A ceramic composite coating and a low-temperature preparation method thereof.
SiO with high bonding strength 2 /α-Al 2 O 3 The low-temperature preparation method of the ceramic composite coating comprises the following steps:
step 4, putting the pretreated ceramic coating substrate into a burning boat and putting the burning boat into a muffle furnace for sintering, heating to 500-700 ℃ at the speed of 0.5-2 ℃/min, preserving heat for 0.5-1.5h, and cooling to room temperature at the speed of 0.5-2 ℃/min to obtain SiO 2 /α-Al 2 O 3 A ceramic composite coating.
Preferably, the specific operation of step 3 is as follows: and spin-coating the slurry on the surface of the pre-treated substrate by a spin coater, drying in the shade at room temperature, and then spin-coating again for 2-4 times.
Preferably, in the step 3, the rotation speed of the spin coater is 1000-2000 rpm, and the spin coating time is 10-30 seconds.
Preferably, in the step 2, the mass fraction of the alkaline silica sol is 30 +/-5%, and the alpha-Al content is 2 O 3 The mass of the powder is 40-60% of that of the alkaline silica sol.
Preferably, in the step 2, the mass of the polyethylene glycol is alpha-Al 2 O 3 Of powder quality1-3％。
Preferably, in step 2, α -Al 2 O 3 The particle size of the powder is 30-200nm.
Preferably, in step 2, the rotation speed of the magnetic stirrer is 500-2000 rpm, and the stirring time is 5-15 hours.
Preferably, in step 1, a plate-shaped sample of 25mm × 25mm × 2mm is prepared by wire-cut electrical discharge machining using a 316L stainless steel plate as a base.
Preferably, in step 1, the matrix is sequentially polished by using 120# and 240# metallographic sandpaper.
Preferably, in step 1, ultrasonic cleaning is performed using alcohol.
The invention adopts a slurry-spin coating method to prepare 316L stainless steel surface SiO 2 /α-Al 2 O 3 The ceramic composite coating has small thickness and uniform structure, has no obvious defects of particle agglomeration, holes, cracks and the like, and obviously improves the SiO 2 /α-Al 2 O 3 The bonding strength between the ceramic composite coating and the substrate.
SiO with high bonding strength 2 /α-Al 2 O 3 Ceramic composite coating using the above high bond strength SiO 2 /α-Al 2 O 3 The ceramic composite coating is prepared by a low-temperature preparation method.
The invention has the beneficial effects that:
the invention adopts a slurry-spin coating method to prepare SiO on the surface of 316L stainless steel 2 /α-Al 2 O 3 The ceramic composite coating realizes rapid film formation at low temperature. The invention adopts polyethylene glycol to promote alpha-Al 2 O 3 The powder is uniformly dispersed in the slurry, the cracking of the coating can be effectively inhibited in the subsequent sintering process, and meanwhile, when the sintering temperature exceeds 400 ℃, the polyethylene glycol is decomposed, and the adverse effect on the coating components is avoided. According to the invention, the coating sample is sintered and cured at a slow heating rate of 0.5-2 ℃/min, so that on one hand, stress unevenness caused by too fast heating can be prevented, and cracking and holes of the coating are generated; on the other hand, only free water and partial substances in the coating can be removed due to low-temperature dryingPhysically bound water and chemically bound water cannot be completely removed, but free water and physically and chemically bound water adsorbed in the coating can be completely evaporated through sintering and curing, so that the silica sol forms Si-O bonds, and the adhesion is improved.
SiO obtained by the invention 2 /α-Al 2 O 3 The surface of the ceramic composite coating is uniform and compact, has no defects of large particle agglomeration, holes, cracks and the like, has the thickness of about 15-30 mu m, and is made of SiO 2 /α-Al 2 O 3 The binding force of the ceramic composite coating and the substrate (316L stainless steel) is up to 70N, which is superior to that of ceramic coatings prepared by other methods such as brush coating, dip coating, drying and the like (the coating thickness is 80-120 μm, the binding force is 30-40N), and the sintering temperature of the invention is only 500-700 ℃, which is far lower than the heat-resisting temperature (1200 ℃) of the 316L stainless steel substrate, so that the property of the 316L stainless steel substrate can not be influenced.
Drawings
FIG. 1 shows SiO obtained in example 2 of the present invention 2 /α-Al 2 O 3 Scanning an electron microscope of the ceramic composite coating; wherein FIG. 1 (a) shows the SiO obtained 2 /α-Al 2 O 3 Surface morphology of the ceramic composite coating, FIG. 1 (b) is the SiO obtained 2 /α-Al 2 O 3 The cross section appearance of the ceramic composite coating.
FIG. 2 shows SiO obtained in example 2 of the present invention 2 /α-Al 2 O 3 X-ray diffraction pattern of the ceramic composite coating.
FIG. 3 shows SiO obtained in example 2 of the present invention 2 /α-Al 2 O 3 Ceramic composite coating and Al obtained in comparative example 2 O 3 /SiO 2 The binding force curve of the tritium-resistant coating is compounded.
FIG. 4 shows SiO obtained in example 2 of the present invention 2 /α-Al 2 O 3 Scratch electron microscopy scan of ceramic composite coatings.
FIG. 5 shows SiO obtained in example 2 of the present invention 2 /α-Al 2 O 3 Electrochemical hydrogen permeation curve of the ceramic composite coating and the substrate.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example 1
High bond strength SiO in this example 2 /α-Al 2 O 3 The preparation method of the ceramic composite coating comprises the following steps:
step 1: pretreatment of substrates
A316L stainless steel plate is used as a substrate, a 25mm multiplied by 2mm plate-shaped sample is prepared by spark wire cutting, then a 120# metallographic abrasive paper and a 240# metallographic abrasive paper are used for grinding the sample in sequence, and then alcohol ultrasonic cleaning and drying are carried out for standby.
Step 2: preparation of the slurry
alpha-Al with the purity of 99.99 percent 2 O 3 The powder and 30% by mass of alkaline silica sol (JN-30) were weighed respectively and placed in a beaker, and polyethylene glycol (PEG) was added. And then, carrying out ultrasonic treatment on the slurry at room temperature, and then uniformly stirring the slurry by using a magnetic stirrer at the rotating speed of 500 revolutions per minute for 5 hours after the ultrasonic treatment is finished.
Wherein, alpha-Al 2 O 3 The powder has a particle size of 30nm and alpha-Al 2 O 3 The addition amount of the powder is 40% of the mass of the alkaline silica sol, and the addition amount of the PEG is alpha-Al 2 O 3 1% of the mass of the powder.
And 3, step 3: spin coating of slurries
And (3) spin-coating the slurry obtained in the step (2) on the 316L stainless steel plate processed in the step (1) by using a spin coater, wherein the rotation speed of the spin coater is 1000 r/min, the spin coating time is 10 seconds, and after each spin coating, the 2 nd spin coating is carried out after the coating is dried in the shade at room temperature.
And 4, step 4: sinter curing of coatings
And (4) loading the coating sample obtained in the step (3) into a burning boat, and then placing the burning boat into a muffle furnace for sintering. Raising the temperature of the muffle furnace to 500 ℃ at the speed of 0.5 ℃/minute, preserving the heat for 1.5 hours, and then cooling to room temperature at the speed of 0.5 ℃/minute to obtain SiO 2 /α-Al 2 O 3 A ceramic composite coating.
SiO obtained in this example 2 /α-Al 2 O 3 The surface of the ceramic composite coating is uniformThe compact coating has the thickness of about 23 mu m, and the bonding force of the coating and the matrix is up to 55N measured by a scratch method, which is superior to that of a comparative example. The steady-state hydrogen permeation current density value of the substrate is 243.3 times that of the coating, and the difference between the steady-state hydrogen permeation current density of the substrate and the hydrogen charging starting point is 160.6 times that of the coating, which is not much different from that of a comparative example.
Example 2
High bond strength SiO in this example 2 /α-Al 2 O 3 The preparation method of the ceramic composite coating comprises the following steps:
step 1: pretreatment of substrates
A316L stainless steel plate is used as a substrate, a 25mm multiplied by 2mm plate-shaped sample is prepared by wire cut electrical discharge machining, then a 120# and a 240# metallographic abrasive paper are used for polishing the sample in sequence, and then the sample is cleaned by alcohol ultrasonic and dried for standby.
And 2, step: preparation of the slurry
alpha-Al with the purity of 99.99 percent 2 O 3 The powder and 30% by mass of alkaline silica sol (JN-30) were weighed separately and placed in a beaker, and polyethylene glycol (PEG) was added. And then, carrying out ultrasonic treatment on the slurry at room temperature, and then uniformly stirring the slurry by using a magnetic stirrer at the rotating speed of 1000 revolutions per minute for 10 hours after the ultrasonic treatment is finished.
Wherein, alpha-Al 2 O 3 The powder has an average particle size of 100nm and alpha-Al 2 O 3 The addition amount of the powder is 50 percent of the mass of the alkaline silica sol, and the addition amount of the PEG is alpha-Al 2 O 3 2% of the mass of the powder.
And step 3: spin coating of slurries
And (3) spin-coating the slurry obtained in the step (2) on the 316L stainless steel plate processed in the step (1) by using a spin coater, wherein the rotation speed of the spin coater is 1500 rpm, the spin-coating time is 20 seconds, and after each spin-coating, the next spin-coating is carried out at room temperature and in the shade, and the spin-coating is carried out for 3 times.
And 4, step 4: sintering and curing of coatings
And (4) loading the coating sample obtained in the step (3) into a burning boat, and then placing the burning boat into a muffle furnace for sintering. Firstly, the muffle furnace is raised by 1 ℃/minKeeping the temperature at 600 ℃ for 1h, then cooling the temperature to room temperature according to the speed of 1 ℃/min, and then obtaining SiO 2 /α-Al 2 O 3 And (3) a ceramic composite coating.
SiO obtained in this example 2 /α-Al 2 O 3 The surface of the ceramic composite coating is uniform and compact, the thickness of the coating is about 20 mu m, and the bonding force between the coating and the matrix is up to 70N measured by a scratch method, which is superior to that of a comparative example. The steady-state hydrogen permeation current density value of the substrate is 244.1 times that of the coating, and the difference between the steady-state hydrogen permeation current density of the substrate and the hydrogen charging starting point is 162.5 times that of the coating, which is not much different from that of the comparative example.
The SiO obtained in this example 2 /α-Al 2 O 3 The ceramic composite coating was subjected to electron microscopy scanning as shown in fig. 1. As can be seen from fig. 1 (a): siO obtained in this example 2 /α-Al 2 O 3 The surface structure of the ceramic composite coating is uniform, and the defects such as holes, cracks and the like are avoided; as can be seen from 1 (b): the coating thickness was small, only 20 μm.
The SiO obtained in this example 2 /α-Al 2 O 3 The ceramic composite coating was subjected to X-ray diffraction, as shown in fig. 2. As can be seen from fig. 2: the coating is made of amorphous SiO 2 And crystalline alpha-Al 2 O 3 And (4) forming.
The SiO obtained in this example 2 /α-Al 2 O 3 And (3) testing the binding force of the coating and the substrate of the ceramic composite coating. And (3) carrying out scratch test on the surface of the coating by adopting a scratch tester, wherein the loading force is 0-150N, the loading speed is 100N/min, and the scratch length is 5-10mm. When the first abrupt peak appears on the test acoustic signal graph, it indicates that the coating begins to peel under this load, which is defined as the bond strength of the coating, and the results are shown in fig. 3. As can be seen from fig. 3: the coating has a bonding force with the substrate of up to 70N. In the above bonding force test, the scratch morphology of the coating is subjected to electron microscope scanning, as shown in fig. 4. As can be seen in fig. 4: in the scratch direction, the width and depth of the scratch gradually increase. When the load reaches 70N, the coating begins to fall off, and the sound signal has a sudden change value. The coating damage around the scratch trace was small, indicating that the SiO obtained in this example 2 /α-Al 2 O 3 The adhesive force between the ceramic composite coating and the matrix is better.
The SiO obtained in this example 2 /α-Al 2 O 3 Electrochemical hydrogen permeation tests were performed on the ceramic composite coating and the 316L stainless steel substrate, and the results are shown in fig. 5. As can be seen in fig. 5: the steady-state hydrogen permeation current density value of the substrate is 244.1 times that of the coating, and the difference between the steady-state hydrogen permeation current density of the substrate and the hydrogen charging starting point is 162.5 times that of the coating.
Example 3
High bond strength SiO in this example 2 /α-Al 2 O 3 The preparation method of the ceramic composite coating comprises the following steps:
step 1: pretreatment of substrates
A316L stainless steel plate is used as a substrate, a 25mm multiplied by 2mm plate-shaped sample is prepared by wire cut electrical discharge machining, then a 120# and a 240# metallographic abrasive paper are used for polishing the sample in sequence, and then the sample is cleaned by alcohol ultrasonic and dried for standby.
And 2, step: preparation of the slurry
Respectively weighing alpha-Al 2O3 powder with the purity of 99.99 percent and alkaline silica sol (JN-30) with the mass fraction of 30 percent, placing the weighed materials in a beaker, and then adding polyethylene glycol (PEG). And then, carrying out ultrasonic treatment on the slurry at room temperature, and then uniformly stirring the slurry by using a magnetic stirrer at the rotating speed of 1500 rpm for 15h.
Wherein, alpha-Al 2 O 3 The powder has a particle size of 200nm and alpha-Al 2 O 3 The addition amount of the powder is 60 percent of the mass of the alkaline silica sol, and the addition amount of the PEG is alpha-Al 2 O 3 3% of the mass of the powder.
And step 3: spin coating of slurries
And (3) spin-coating the slurry obtained in the step (2) on the 316L stainless steel plate treated in the step (1) by using a spin coater, wherein the rotation speed of the spin coater is 2000 r/min, the spin-coating time is 30 seconds, and after each spin-coating, the next spin-coating is carried out after the coating is dried in the shade at room temperature, and the total spin-coating is carried out for 3 times.
And 4, step 4: sintering and curing of coatings
And (4) loading the coating sample obtained in the step (3) into a burning boat, and then placing the burning boat into a muffle furnace for sintering. Firstly, raising the temperature of a muffle furnace to 700 ℃ according to the speed of 2 ℃/minute, preserving the temperature for 0.5h, then cooling the temperature to room temperature according to the speed of 2 ℃/minute, and then obtaining SiO 2 /α-Al 2 O 3 A ceramic composite coating.
SiO obtained in this example 2 /α-Al 2 O 3 The surface of the ceramic composite coating is uniform and compact, the thickness of the coating is about 18 mu m, and the bonding force between the coating and a matrix is up to 60N measured by a scratch method, which is superior to that of a comparative example. The steady-state hydrogen permeation current density value of the substrate is 240.7 times that of the coating, and the difference between the steady-state hydrogen permeation current density of the substrate and the hydrogen charging starting point is 166.3 times that of the coating, which is not much different from that of the comparative example.
Comparative example
The applicant previously filed an application of 316L stainless steel pipe inner wall Al 2 O 3 /SiO 2 The composite tritium-resistant coating obtained by the preparation method (application date is 2020, 12 and 23 days, application number is 202011538343.5, publication number is CN 112657815A, and publication number is 2021, 04 and 16 days) serves as a comparative example.
Al obtained in this comparative example 2 O 3 /SiO 2 The thickness of the composite tritium-resistant coating is about 80 mu m, and the binding force is 30N.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. SiO with high bonding strength 2 /α-Al 2 O 3 The low-temperature preparation method of the ceramic composite coating is characterized by comprising the following steps of:
step 1, polishing a substrate, then ultrasonically cleaning, and drying to obtain a pretreated substrate;
step 2, mixing alpha-Al 2 O 3 Mixing the powder with alkaline silica sol and polyethylene glycolMixing, performing ultrasonic treatment, and uniformly stirring to obtain slurry;
step 3, spin-coating the slurry on the surface of the pre-processed substrate to obtain a pre-processed ceramic coating substrate;
step 4, sintering the pretreated ceramic coating substrate, heating to 500-700 ℃ at the speed of 0.5-2 ℃/min, preserving heat for 0.5-1.5h, and cooling to room temperature at the speed of 0.5-2 ℃/min to obtain SiO 2 /α-Al 2 O 3 A ceramic composite coating;
in the step 2, the mass fraction of the alkaline silica sol is 30 +/-5 percent, and the alpha-Al 2 O 3 The mass of the powder is 40-60% of that of the alkaline silica sol;
in step 2, the mass of the polyethylene glycol is alpha-Al 2 O 3 1-3% of the powder mass.
2. The high bond strength SiO of claim 1 2 /α-Al 2 O 3 The low-temperature preparation method of the ceramic composite coating is characterized in that the specific operation of the step 3 is as follows: and spin-coating the slurry on the surface of the pre-treated substrate by using a spin coater, and performing spin-coating again after drying in the shade at room temperature, wherein the spin-coating times are 2-4.
3. The high bond strength SiO of claim 2 2 /α-Al 2 O 3 The low-temperature preparation method of the ceramic composite coating is characterized in that in the step 3, the rotating speed of the spin coater is 1000-2000 rpm, and the spin coating time is 10-30 seconds.
4. The high bond strength SiO of claim 1 2 /α-Al 2 O 3 The low-temperature preparation method of the ceramic composite coating is characterized in that in the step 2, alpha-Al 2 O 3 The particle size of the powder is 30-200nm.
5. The high bond strength SiO of claim 1 2 /α-Al 2 O 3 The low-temperature preparation method of the ceramic composite coating is characterized in that in the step 1, 120# and 240# metallographic abrasive paper are sequentially adopted to polish a substrate.
6. The high bond strength SiO of claim 1 2 /α-Al 2 O 3 The low-temperature preparation method of the ceramic composite coating is characterized in that in the step 1, alcohol is adopted for ultrasonic cleaning.
7. SiO with high bonding strength 2 /α-Al 2 O 3 Ceramic composite coating, characterized in that a high bond strength SiO according to any of claims 1 to 6 is used 2 /α-Al 2 O 3 The ceramic composite coating is prepared by a low-temperature preparation method.
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| CN114807854A (en) * | 2022-04-14 | 2022-07-29 | 华南理工大学 | Method for depositing alpha-alumina dielectric film on surface of silicon substrate |
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