KR101261356B1 - stainless steel coated by polyphenylcarbosilane with silicon carbide powder and method of producing the same - Google Patents
stainless steel coated by polyphenylcarbosilane with silicon carbide powder and method of producing the same Download PDFInfo
- Publication number
- KR101261356B1 KR101261356B1 KR1020100073083A KR20100073083A KR101261356B1 KR 101261356 B1 KR101261356 B1 KR 101261356B1 KR 1020100073083 A KR1020100073083 A KR 1020100073083A KR 20100073083 A KR20100073083 A KR 20100073083A KR 101261356 B1 KR101261356 B1 KR 101261356B1
- Authority
- KR
- South Korea
- Prior art keywords
- stainless steel
- polyphenylcarbosilane
- silicon carbide
- carbide powder
- coating
- Prior art date
Links
Images
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
Abstract
The present invention relates to a stainless steel coated with polyphenylcarbosilane to which silicon carbide powder is added and a method for producing the same. More specifically, a polyphenylcarbosilane solution in which silicon carbide (SiC) powder is dispersed is coated on a stainless steel surface And heat-treated to provide a high-temperature resistant corrosion-resistant stainless steel and a method for producing the same. Stainless steel coated with polyphenylcarbosilane dispersed with silicon carbide powder produced by the present invention has a high surface strength at high temperature and is stable in an acidic solution and can be used in a high temperature such as a gas turbine, an automobile engine, a heat exchanger tube, Can be used as a corrosive material.
Description
The present invention relates to stainless steel coated with polyphenylcarbosilane to which silicon carbide powder is added and a method for producing the same.
Along with the recent development of industrial technology, the use of metal materials has been diversified, and in particular, the use environment of metals used as mechanical materials has become harsh, and the performance and durability of metallic materials have been demanded. Among them, multilayer structure coating materials have been developed for the metal used in cutting tools and precision element machines for protection against abrasion and corrosion.
In general, when a metal is exposed to an oxidizing atmosphere at a high temperature, oxygen is adsorbed to precipitate the oxide on the surface or inside. Therefore, in the case of gas turbine engines used in aircrafts and generators, the development of technology related to high temperature internal edible surface treatment is becoming important in order to prevent deterioration due to oxidation in high temperature materials.
Diffusion coating, vapor deposition, spraying, composite coating, and nanocomposite plating are known to be the most common surface treatments for high temperature treatment to date.
With respect to the corrosion resistant material technology, a mixed metal oxide (Korean Patent Laid-Open No. 10-2005-0117111) and a ceramic particle are coated or coated on the surface of a metal in powder form (Korean Patent Laid-Open No. 2005-0089250, There is known a technique of forming a zirconium oxide film on the surface of a cladding tube of a zirconium alloy material in an oxidizing atmosphere (Korean Patent Laid-Open Publication No. 2004-0077162) and using the same in a nuclear fuel rod of a nuclear reactor. However, these methods mainly use metal oxide or oxide ceramic powder, which can partially improve the thermal vulnerability of the metal, but has a problem that the physical properties such as adhesion strength and strength development between the metal and the coating layer are weak.
In recent years, metal is mainly used as a membrane material in the field of fuel cell, which is used at a temperature of 650 ° C before and after, so that corrosion of a metal member due to an electrolyte medium occurs and the efficiency and lifetime of the battery are lowered. Therefore, it is necessary to develop ceramic coating materials and methods for preventing oxidation of metal surfaces.
In particular, stainless steel in metallic materials is resistant to rust and corrosion due to the fact that a large amount of chromium controls the oxidation of the surface, and is superior in fatigue strength and corrosion resistance compared to general steel. Therefore, it can be used for pipes, heat exchangers, It is widely used for heat resistant equipment and so on.
However, stainless steel also has a high corrosion rate in extreme environments and can not prevent corrosion if the chromium oxidation protective film on the surface is lost during processing. Accordingly, stainless steel materials are also required to be improved in heat resistance and corrosion resistance even in extreme environments and surface treatment technology.
On the other hand, typical polycarbosilane among the carbosilane-based polymers has been used as a precursor for producing silicon carbide mainly in an inert atmosphere. Polycarbosilane has also been developed as a coating agent, and a technique for improving the vulnerability of a metal by forming a ceramic film on a metal surface has been developed.
According to Japanese Laid-Open Patent Application No. 1995-304958, polycarbosilane is used to form a heat-resistant insulating film on a metal surface. However, silica powder is used as an additive and the heat treatment temperature is also lowered to about 200 to 250 ° C, It has limitations that can not be achieved.
Japanese Patent Application Laid-Open No. 1999-0050136 discloses a technique for forming a coating film on a metal surface by using polycarbosilane to prevent carburization on a metal surface. Thereby forming a constituted ceramic film. However, in the above invention, the polycarbosilane coating layer is used as an interlayer in a structure composed of an iron core and a carbon sleeve, and is limited in that it is used as a protective film for protecting an iron core from a carbon sleeve rather than improving physical vulnerability of the metal.
In addition, polycarbosilane has been developed as an insulating film in semiconductor materials (Korean Patent Application No. 10-2010-0012326, Japanese Patent Application Laid-Open No. 2008-210929, Japanese Patent Application Laid-Open No. 2005-183697) It is not suitable for use as a high-temperature material of metal or an oxidation-preventive film.
The present invention seeks to provide a method of coating a ceramic film with a silicon carbide powder added to a stainless steel surface through a safe and effective method.
In addition, the stainless steel having the ceramic film according to the present invention shows stability in surface hardness and high temperature, is stable in strong acidic conditions and can be used as a metal material used at high temperatures of gas turbines, automobile engines, etc., And a method of providing a method that can be used as a component material requiring a corrosion-resistant stainless steel material such as a reaction vessel.
One embodiment of the present invention is a method of manufacturing a semiconductor device, comprising: (S1) preparing a coating solution by adding polyphenylcarbosilane and silicon carbide powder to an organic solvent; (S2) coating the coating solution on the surface of an oxide film-formed stainless steel; And (S3) curing the coated stainless steel after the step (S2) and then performing heat treatment (S3).
Another embodiment of the present invention is a method for manufacturing a stainless steel having a ceramic film, wherein the coating solution is a silicon carbide powder dispersed in a solution in which polyphenylcarbosilane is dissolved in an organic solvent.
In another embodiment of the present invention, the weight ratio of the polyphenylcarbosilane to the silicon carbide powder is 1: 0.1 to 1: 2 in the step S1.
In another embodiment of the present invention, the polyphenylcarbosilane is a compound represented by the following general formula (1) in the step (S1).
≪ Formula 1 >
(1? X? 2, 0? Y? 1, and 1? X + y?
In another embodiment of the present invention, the polyphenylcarbosilane has a polystyrene-reduced weight average molecular weight (Mw) of 2000 to 6000 measured by gel permeation chromatography (GPC) A method for producing a stainless steel film.
Another embodiment of the present invention is a method for manufacturing a stainless steel having a ceramic film, wherein the silicon carbide powder has an average particle size of 10 nm to 10 m in the step S1.
In another embodiment of the present invention, the stainless steel in which the oxide film is formed in step S2 is manufactured by forming an oxide film on stainless steel by any one method selected from a heat treatment method, an atomic layer deposition method, CVD or RF sputtering. A method for producing a stainless steel film.
Another embodiment of the present invention is a method for manufacturing a stainless steel having a ceramic film, wherein the heat treatment is performed at a temperature of 500 to 800 DEG C under an oxygen atmosphere or an atmosphere.
In another embodiment of the present invention, the curing step is performed at a temperature of 150 to 350 DEG C in step S3.
According to an embodiment of the present invention, in the step S3, the heat treatment is performed at a temperature of 600 to 1500 ° C.
One embodiment of the present invention is a stainless steel having a ceramic film formed according to the above-described manufacturing method.
In one embodiment of the present invention, the ceramic film is stainless steel having a thickness of 0.5 to 100 占 퐉.
The stainless steel coated with polyphenylcarbosilane coated with silicon carbide powder according to the present invention and its manufacturing method have high surface strength and stability at high temperature, are stable in an acidic solution, and can simplify a manufacturing process.
Stainless steel coated with polyphenylcarbosilane dispersed with silicon carbide powder produced by the present invention has a high surface strength at high temperature and is stable in an acidic solution and can be used in a high temperature such as a gas turbine, an automobile engine, a heat exchanger tube, Can be used as a corrosive material.
FIG. 1 is an electron microscope (SEM) photograph of a section of stainless steel on which a ceramic film having a silicon carbide powder dispersed therein is taken from Example 5 of the present invention.
Fig. 2 is a photograph showing the color change of the hydrochloric acid solution after 7 days of the corrosion resistance test conducted in Example 9 and Comparative Example 1 of the present invention (Fig. 2 (a) (B) a stainless steel substrate not subjected to the surface treatment according to Comparative Example 1 was immersed in a hydrochloric acid solution).
3 is an electron microscope (SEM) photograph of the surface of a ceramic film after a corrosion resistance test is performed on a stainless steel substrate on which a ceramic film having a silicon carbide powder dispersed therein is formed in Example 9 of the present invention.
4 is an electron micrograph (SEM) photograph of the surface of stainless steel after the corrosion resistance test is performed on a stainless steel substrate not subjected to the surface treatment in Comparative Example 1 of the present invention.
5 is a graph showing a change in weight loss caused by a corrosion resistance test on a stainless steel substrate on which a ceramic film having a silicon carbide powder dispersed therein and a stainless steel substrate not subjected to a surface treatment in Example 9 and Comparative Example 1 (B) a stainless steel substrate on which a ceramic film with a silicon carbide powder dispersed therein produced by Example 5 is formed, (c) a stainless steel substrate on which a silicon carbide powder is dispersed, A stainless steel substrate on which a ceramic film in which silicon carbide powder is dispersed).
According to an embodiment of the present invention, there is provided a method for manufacturing a semiconductor device, comprising: (S1) preparing a coating solution by adding polyphenylcarbosilane and silicon carbide powder to an organic solvent; (S2) coating the coating solution on the surface of an oxide film-formed stainless steel; And a step (S3) of curing the coated stainless steel after the step (S2) and heat treating the coated stainless steel (S3).
First, polyphenylcarbosilane and silicon carbide powder are added to an organic solvent to prepare a coating solution (S1).
The coating solution is obtained by dispersing silicon carbide powder in a solution in which polyphenylcarbosilane is dissolved in an organic solvent. When the silicon carbide powder is dispersed in a solution obtained by dissolving the polyphenylcarbosilane in an organic solvent, that is, a polyphenylcarbosilane solution, it is possible to increase the thickness of the coating layer and to prevent cracking occurring during the heat treatment, And high temperature stability can be improved.
The coating solution is prepared by adding the polyphenylcarbosilane to the silicon carbide powder in an organic solvent such that the weight ratio of the polyphenylcarbosilane to the silicon carbide powder is 1: 0.1 to 1: 2.
When the weight ratio of the polyphenylcarbosilane to the silicon carbide powder is within the above range, the silicon carbide powder is well dispersed in the polyphenylcarbosilane solution, and the polyphenylcarbosilane solution is coated on the surface of the stainless steel, And the surface of the stainless steel can be improved.
When the polyphenylcarbosilane is contained in an organic solvent outside the weight ratio range, there is a problem that the thickness of the ceramic film formed on the surface of the stainless steel becomes thin or the viscosity becomes high, so that a uniform ceramic film can not be obtained.
Generally, when coating is performed using a powder-dispersed solution, a sol-gel, or a polymer precursor, there is a problem that a coating film is cracked due to a shrinkage of the coating layer during a heat treatment process .
The silicon carbide powder according to the present invention not only enhances the strength of the coating layer but also prevents the coating layer due to the polyphenylcarbosilane solution from being formed due to shrinkage during the heat treatment process.
At this time, the polyphenylcarbosilane and the silicon carbide powder may be prepared by first dissolving the polyphenylcarbosilane in the organic solvent and adding the silicon carbide powder to the organic solvent within the above range, The order of dissolving in the solvent is not limited thereto.
The organic solvent is not particularly limited, and one of organic solvents such as toluene, n-hexane, cyclohexane, tetrahydrofuran, benzene, chloroform, Or a mixture of two or more of them may be used.
The polyphenylcarbosilane is a compound represented by the following general formula (1).
≪ Formula 1 >
(1? X? 2, 0? Y? 1, and 1? X + y?
In the present invention, the polyphenylcarbosilane represented by the above formula (1) is advantageous in simplifying the corrosion-resistant surface treatment process and advantageous in large-scale surface treatment.
More specifically, conventional corrosion resistant surface treatment methods such as diffusion coating, vapor deposition, spray coating, composite coating and nanocomposite plating require expensive equipment and require several steps to form a stable coating film. Therefore, It is not only economical because of its complexity, but also difficult to apply to large-scale.
The polyphenylcarbosilane according to the present invention is not only soluble in an organic solvent but also has a high melting temperature and is stable in the air and can be used as a solution process such as dip coating, spray coating, and spin coating It is advantageous in that the process is relatively simple and large in size. The polyphenylcarbosilane is advantageous in terms of processability because it has high adhesion to surfaces of various materials such as ceramic, metal, graphite, and wafer surface, unlike other polymers or ceramic precursors such as a sol-gel process.
Particularly, among the carbosilane-based polymers, polyphenylcarbosilane contains a phenyl functional group, which corresponds to a carbon-rich ceramic precursor. In the case of heat treatment in an inert atmosphere, it is a silicon carbide. In an oxidizing atmosphere, a silicon- It can be converted into silicon oxicarbide and has advantages as a high temperature oxidation resistant coating of various structures. Particularly, the fact that the carbon is abundant is higher than the ordinary polycarbosilane, but the high-temperature stability of the polymer itself is high. However, since the content ratio of carbon and oxygen in the Si-C / Si-O formation can be effectively controlled, And the like can be used as the heat treatment atmosphere.
The polyphenylcarbosilane according to the present invention preferably satisfies the conditions of 1? X? 2, 0? Y? 1 and 1? X + y? 3 in the above formula (1) The effect of dispersing the added silicon carbide nano powder is enhanced, and after the coating, the adhesion of the powder and the polyphenylcarbosilane is increased to form a dense ceramic film.
The precursor of the polyphenylcarbosilane is not particularly limited, and for example, it can be produced using phenyltrichlorosilane, diphenyldichlorosilane, polydimethylsilane, polymethylphenylsilane, or the like. Among them, preferably, polymethylphenylsilane can be used. The method for producing polyphenylcarbosilane can be selected from among well-known methods in the field of the present invention, and Korean Patent No. 10-2006- 17755 as follows.
First, polymethylphenylsilane is prepared by condensation reaction of phenylmethyldichlorosilane with an alkali metal, preferably sodium metal, in an inert atmosphere such as nitrogen.
Specifically, sodium metal is finely sliced into a solvent such as xylene, tetrahydrofuran (THF), and toluene under an inert atmosphere, and the mixture is heated and stirred to completely disperse the sodium metal. Then, phenylmethyl Dichlorosilane may be injected and heated to form a polymer, followed by removal of the residual metal sodium and the solvent.
The produced polymethylphenylsilane can be converted into polyphenylcarbosilane by using a high-temperature autoclave. The conversion reaction temperature is preferably 300 to 350 占 폚, and it is possible to produce polyphenylcarbosilane having a molecular weight suitable for coating by polymerization at 400 to 450 占 폚.
The polyphenylcarbosilane preferably has a polystyrene reduced weight average molecular weight (Mw) of from 2000 to 6000, more preferably from 2500 to 4000, as measured by Gel Permeation Chromatography (GPC). When the weight average molecular weight of the polyphenylcarbosilane is larger, a thick coating film can be obtained after the heat treatment. However, if the weight average molecular weight exceeds 6000, the polyphenylcarbosilane is not completely dissolved in an organic solvent such as a nucleic acid. When the weight average molecular weight of the polyphenylcarbosilane is less than 2000, the melting point of the polyphenylcarbosilane is lowered, and the coating layer is not retained in the heat treatment step, and the yield of the ceramic is low, which is not easy to coat.
Generally, pyrolysis occurs in the vicinity of 300 to 400 ° C in the organic material. The polyphenylcarbosilane is called an organometallic polymer or an inorganic polymer. The phenyl or ethyl functional groups except for the Si-C backbone are pyrolyzed near the above temperature. Therefore, when the temperature exceeds 600 ° C., the pyrolysis is completed, and only the inorganic material is left except for the loss part which is gasified during the pyrolysis process. It is converted into the inorganic substance compared to the polymer, and the yield of the ceramic (= residual amount after heat treatment / × 100 (%)) can be obtained. In the case of such an inorganic polymer, the melting point and the yield of ceramics vary depending on the molecular weight, and therefore, the polyphenylcarbosilane according to the present invention preferably has a weight average molecular weight of 2,000 to 6,000.
The silicon carbide powder preferably has an average particle size of 10 nm to 10 mu m. When the average particle size of the silicon carbide powder is within the above range, it is not only advantageous in dispersing in the formation of a coating layer but also in an excellent adhesion state with a mother liquor.
Next, the coating solution is coated on the surface of the stainless steel on which the oxide film is formed (S2).
The coating process can be generally carried out by employing a coating method widely known in the field of the present invention, for example, dip coating, spray coating, spin coating, or the like , But is not limited thereto.
The coating solution is coated on the surface of the stainless steel having the oxide film. Examples of the method of forming the oxide film on the stainless steel include a heat treatment method, an atomic layer deposition method, CVD or RF sputtering. In the present invention, Is not limited to the above method, and a thin chromium oxide layer already formed naturally on a stainless steel surface may be used.
Preferably, the stainless steel having the oxide film formed thereon is heat-treated at a temperature of 500 to 800 DEG C under an oxygen atmosphere or an atmosphere for a certain period of time to form an oxide film, because the process is relatively simple and economical.
After the step S2, the coated stainless steel is cured and then heat-treated (S3).
The curing process is carried out at a temperature of 150 to 350 ° C. When curing under the above conditions, there is an advantage that the phenomenon that the polyphenylcarbosilane is melted in the heat treatment step and the coating film is collapsed can be prevented.
The heat treatment process is performed at a temperature of 600 to 1500 ° C. When the heat treatment is performed under the above conditions, the polyphenylcarbosilane in the polymer state is converted into the ceramic state, and the bonding strength of the silicon carbide powder dispersed in the coating layer is enhanced, which is advantageous for high temperature use.
The polyphenylcarbosilane or generally known polycarbosilane used in the present invention has a melting point of 300 ° C or higher. The temperature at which the ceramic is formed should be 500 ° C or higher in the case of glassy material, but the temperature for forming the crystalline ceramic should be at least 800 ° C or higher. In other words, when the heat treatment temperature is in the range of 200 to 250 ° C., although some oxidation phenomenon occurs in the atmospheric environment, it is possible to maintain the properties of the polymer itself, and in order to exhibit the high- Should be. In this regard, it is preferable that the temperature of the heat treatment process according to the present invention is in the range of 600 to 1500 ° C.
At this time, the curing process or the heat treatment process can be performed within the temperature range by appropriately adjusting the time according to any purpose, as long as a person skilled in the art is familiar with the process.
Generally, in order to form a ceramic film on a metal surface, a bond coat layer is formed between the metal surface and the interface of the ceramic film to improve the bonding strength.
However, in the case of stainless steel, it is known that the chromium component is contained on the surface in order to prevent corrosion on the surface and diffusion of corrosion into the inside of the stainless steel, and a chromium oxide film is formed in a high temperature oxidizing atmosphere to improve oxidation resistance.
Accordingly, in the embodiment of the present invention, the stainless steel base material is heat-treated in an oxidizing atmosphere to form an oxide film thicker on the surface and acts as a bond coat layer, thereby improving the bonding strength between the metal base material and the ceramic film.
According to another embodiment of the present invention, there is provided a stainless steel in which a ceramic film is formed by the manufacturing method described above.
It is preferable that the ceramic film has a ceramic film having a thickness of 0.5 to 100 탆, preferably 1 to 50 탆. When the thickness of the ceramic film is within the above range, it is more effective in enhancing the acid resistance of the metal foil.
Hereinafter, preferred embodiments and comparative examples of the present invention will be described. However, the following embodiments are merely preferred embodiments of the present invention, and the present invention is not limited to the following embodiments.
≪ Example 1 >
20 g of polyphenylcarbosilane having a weight average molecular weight of 4,000 was dissolved in toluene as a solvent to prepare a polyphenylcarbosilane solution having a concentration of 20% by weight. While stirring the polyphenylcarbosilane solution, 10 g of a 130 nm silicon carbide powder was added and maintained in a stirred state to disperse evenly. At this time, the polyphenylcarbosilane is a compound represented by the following general formula (2).
(2)
(Wherein x is 1 and y is 0).
≪ Example 2 >
20 g of polyphenylcarbosilane having a weight average molecular weight of 4,000 was dissolved in toluene as a solvent to prepare a polyphenylcarbosilane solution having a concentration of 20% by weight. 15 g of 130 nm silicon carbide powder was added while stirring the polyphenylcarbosilane solution, and the mixture was stirred to disperse evenly. At this time, the polyphenylcarbosilane is a compound represented by the following general formula (3).
(3)
(Wherein x is 1 and y is 0).
≪ Example 3 >
20 g of polyphenylcarbosilane having a weight average molecular weight of 4,000 was dissolved in toluene as a solvent to prepare a polyphenylcarbosilane solution having a concentration of 20% by weight. 15 g of 130 nm silicon carbide powder was added while stirring the polyphenylcarbosilane solution, and the mixture was stirred to disperse evenly. At this time, the polyphenylcarbosilane is a compound represented by the following general formula (4).
≪
(Wherein x is 1 and y is 1.)
<Example 4>
The stainless steel (STS316) substrate was heat treated at 800 ° C in the atmosphere to form an oxide film on the surface of the stainless steel substrate.
≪ Example 5 >
The stainless steel substrate on which the oxide film was formed in Example 4 was impregnated with the coating solution prepared in Example 1 at a rate of 1 mm / s, cured at 200 ° C for 2 hours, Lt; 0 > C for 1 hour. The cross section of the stainless steel substrate on which the silicon carbide-dispersed ceramic coating thus obtained was photographed by an electron microscope is shown in FIG. FIG. 2 shows that a coating layer of about 5 to 6 μm was formed.
≪ Example 6 >
The stainless steel substrate on which the oxide film was formed in Example 4 was impregnated with the coating solution prepared in Example 2 at a rate of 1 mm / s in the same manner as in Example 5, and cured at 200 ° C for 2 hours Followed by heat treatment at 800 ° C for 1 hour in an argon atmosphere.
≪ Example 7 >
The stainless steel substrate on which the oxide film was formed in Example 4 was impregnated with the coating solution prepared in Example 3 at a rate of 1 mm / s in the same manner as in Example 5, and cured at 200 ° C for 2 hours Followed by heat treatment at 800 ° C for 1 hour in an argon atmosphere.
≪ Example 8 >
An electromechanical pencil tester was used to measure the surface hardness of a stainless steel substrate on which a ceramic coating layer with silicon carbide dispersed according to Example 5, Example 6 and Example 7 was formed, and 9H Using a pencil, the pencil's core was placed at an angle of 45 ° and the load was measured at 800 g.
≪ Example 9 >
A 10% hydrochloric acid solution was prepared to measure the corrosion resistance of the stainless steel substrate on which the ceramic film was formed, and the stainless steel substrate on which the ceramic coating layer having the silicon carbide dispersed therein prepared in each of Examples 5 and 6 was formed was immersed. The immersed stainless steel substrates were taken out after 5, 6, and 7 days, washed and dried, and then weighed and recorded for weight loss by corrosion. For samples with corrosion test 7 days, stainless steel The degree of color change of the hydrochloric acid test solution caused by the corrosion was confirmed, and the surface of each sample was photographed by an electron microscope.
≪ Comparative Example 1 &
To measure the corrosion resistance of the stainless steel substrate, a 10% hydrochloric acid solution was prepared, and a stainless steel substrate on which the surface was not pretreated and coated was immersed. The immersed stainless steel substrates were taken out after 5, 6, and 7 days, washed and dried, and then weighed and recorded for weight loss by corrosion. For samples with corrosion test 7 days, stainless steel The degree of color change of the hydrochloric acid test solution caused by the corrosion was confirmed, and the surface of each sample was photographed by an electron microscope.
As a result of evaluating the hardness of Example 8, it was found that the stainless steel substrate formed with the ceramic film produced in the example of the present invention exhibits excellent surface hardness and does not cause peeling phenomenon from the metal mold.
The color change of each stainless steel substrate and hydrochloric acid solution after 7 days for the corrosion test conducted according to Example 9 and Comparative Example 1 is shown in FIG. 2 (a), in the case of the hydrochloric acid solution immersed in the stainless steel substrate on which the ceramic coating film having the silicon carbide dispersed therein was formed, the colorless transparent solution became green, but it remained clear while maintaining transparency. On the other hand, in the case of a solution immersed in a stainless steel substrate which had not undergone any surface treatment (Fig. 2 (b)), corrosion of the stainless steel substrate surface occurred, and the hydrochloric acid solution lost transparency and discolored to turbid and deep cyan.
3 and 4 show the surface of the stainless steel substrate subjected to the corrosion test, respectively. FIG. 3 is a photograph of the surface of a stainless steel substrate on which a ceramic coating layer having a silicon carbide dispersed therein was formed. According to corrosion test using hydrochloric acid, It can be confirmed that the surface defect caused by the surface defect has not occurred. FIG. 4 is a photograph of a surface of a stainless steel substrate on which surface treatment is not performed. It can be seen that corrosion is much promoted by the hydrochloric acid solution because the surface has many defects.
It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (12)
(S2) coating the coating solution on the surface of an oxide film-formed stainless steel;
(S3) of curing the coated stainless steel after the step S2 and then performing heat treatment;
In the step S1, the polyphenylcarbosilane is a compound represented by the following formula (1)
≪ Formula 1 >
(1? X? 2, 0? Y? 1, and 1? X + y?
Wherein the weight ratio of the polyphenylcarbosilane to the silicon carbide powder is 1: 0.1 to 1: 2 in the step (S1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020100073083A KR101261356B1 (en) | 2010-07-28 | 2010-07-28 | stainless steel coated by polyphenylcarbosilane with silicon carbide powder and method of producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020100073083A KR101261356B1 (en) | 2010-07-28 | 2010-07-28 | stainless steel coated by polyphenylcarbosilane with silicon carbide powder and method of producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR20120011300A KR20120011300A (en) | 2012-02-07 |
| KR101261356B1 true KR101261356B1 (en) | 2013-05-07 |
Family
ID=45835549
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1020100073083A KR101261356B1 (en) | 2010-07-28 | 2010-07-28 | stainless steel coated by polyphenylcarbosilane with silicon carbide powder and method of producing the same |
Country Status (1)
| Country | Link |
|---|---|
| KR (1) | KR101261356B1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101442559B1 (en) * | 2013-09-12 | 2014-09-22 | 한국세라믹기술원 | Coating composition and method of formation of the high quality ceramic coating layer using the same |
| KR101870733B1 (en) * | 2017-03-16 | 2018-06-26 | 한국과학기술원 | Dual-mode transmission mechanism based on twisted string actuation |
| CN112876258A (en) * | 2021-03-05 | 2021-06-01 | 中国人民解放军国防科技大学 | BCN ceramic precursor containing phenyl and synthesis method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100824275B1 (en) | 2006-11-17 | 2008-04-24 | 주식회사 티씨케이 | Metal coated with graded-ceramic and manufacturing method thereof |
-
2010
- 2010-07-28 KR KR1020100073083A patent/KR101261356B1/en active IP Right Grant
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100824275B1 (en) | 2006-11-17 | 2008-04-24 | 주식회사 티씨케이 | Metal coated with graded-ceramic and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20120011300A (en) | 2012-02-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101503305B (en) | Process for preparing self-sealing silicon carbide ceramic based composite material | |
| JP6865554B2 (en) | Goods with excellent high temperature performance | |
| US20090297718A1 (en) | Methods of fabricating environmental barrier coatings for silicon based substrates | |
| CN110461799B (en) | Component comprising a substrate and an environmental barrier | |
| JP2006327923A (en) | Coating system for silicon based substrate | |
| CN110357632B (en) | ZrC/SiC complex phase ceramic precursor and preparation method thereof | |
| WO2007089666A2 (en) | Aluminosilicate-based oxide composite coating and bond coat for silicon-based ceramic substrates | |
| CN109400168B (en) | SiC fiber containing SiBCN coating and SiC coating which are alternately formed, and preparation method and application thereof | |
| CN109592987B (en) | Preparation method of C/C-SiC composite material containing carbon-rich boron nitride interface phase | |
| US20220055957A1 (en) | Method of making a ceramic matrix composite that exhibits chemical resistance | |
| US20160107940A1 (en) | Ceramic matrix composites and methods for producing ceramic matrix composites | |
| CN112374917B (en) | High-temperature ceramic coating and preparation method thereof | |
| CN108947588A (en) | A kind of C/SiC composite material and the antioxidant coating for the material and preparation method thereof | |
| KR101261356B1 (en) | stainless steel coated by polyphenylcarbosilane with silicon carbide powder and method of producing the same | |
| Packirisamy et al. | Polymer-derived ceramics and their space applications | |
| JPH08225382A (en) | Composite electronics film | |
| Tong et al. | Coating of poly (carborane-carbosilane-phenylacetylene) on carbon fibers with excellent oxidation protection | |
| JP5267729B2 (en) | SiC coated SiC fiber bonded ceramics | |
| KR101331403B1 (en) | Process for silicon carbide coating on graphite | |
| CN108752012B (en) | Preparation method of boron nitride/silicon nitride composite interface layer on fiber surface | |
| KR101204013B1 (en) | Low temperature silicon carbide coating | |
| EP3957620A1 (en) | Method of making a ceramic matrix composite that exhibits moisture and environmental resistance | |
| JP2002104892A (en) | Ceramic composite material | |
| Cinibulk et al. | Constituent Development for Higher-Temperature Capable Ceramic Matrix Composites | |
| KR101110351B1 (en) | Structures of the graphite foam |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A201 | Request for examination | ||
| E902 | Notification of reason for refusal | ||
| E90F | Notification of reason for final refusal | ||
| E701 | Decision to grant or registration of patent right | ||
| GRNT | Written decision to grant | ||
| FPAY | Annual fee payment |
Payment date: 20160404 Year of fee payment: 4 |
|
| FPAY | Annual fee payment |
Payment date: 20170419 Year of fee payment: 5 |
|
| FPAY | Annual fee payment |
Payment date: 20180605 Year of fee payment: 6 |
|
| FPAY | Annual fee payment |
Payment date: 20190423 Year of fee payment: 7 |