CN112374911B - Surface treatment method of graphite substrate and preparation method of TaC coating - Google Patents
Surface treatment method of graphite substrate and preparation method of TaC coating Download PDFInfo
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
Abstract
The invention discloses a surface treatment method of a graphite substrate and a preparation method of a TaC coating, wherein the surface treatment method comprises the following steps: cleaning and drying the graphite substrate, placing the graphite substrate into a reaction chamber of plasma modification equipment, closing an air inlet valve, vacuumizing the reaction chamber, filling the reaction chamber with oxygen or argon, adjusting the air inlet valve to stabilize the vacuum degree of the reaction chamber at 10-100Pa, starting radio frequency power supply discharge, bombarding the surface of the graphite substrate by using the oxygen plasma or the argon plasma, and increasing the roughness and the activity of the surface of the graphite substrate; after the treatment by the method, the TaC coating is deposited, so that the formed TaC coating is tightly combined with the graphite substrate, is not easy to fall off, and the thermal shock resistance is greatly improved; and the process is simple and efficient, the energy consumption is low, the production cost is low, and the production period is short.
Description
Technical Field
The invention relates to the technical field of graphite substrate surface treatment, in particular to a surface treatment method of a graphite substrate and a preparation method of a TaC coating; and more particularly, to a surface treatment method for improving the bonding strength of a graphite substrate and a TaC coating, and a method for high-strength bonding of a graphite substrate and a TaC coating.
Background
Graphite is a light high-melting-point material, is suitable for high-temperature environments, but is easy to react with other substances at high temperature, so that a layer of compact protective coating needs to be prepared on the surface of the graphite. In the face of increasingly severe use environments, the requirements on coatings are higher and higher, and the tantalum carbide (TaC) can well protect the graphite substrate as a high-temperature ceramic material with ultrahigh melting point, excellent chemical stability and good chemical compatibility with carbon materials. However, one of the most important problems faced at present is that the thermal expansion coefficients of TaC and graphite are too different, the interface between the two is prone to too much thermal stress and cracks, and therefore, some methods must be adopted to improve the interface bonding between the two.
The methods for surface modification of graphite substrates mainly include the following: 1. chemical etching method; 2. a pre-oxidation method; 3. machining, and the like. The chemical corrosion method is mainly characterized in that graphite is soaked in a chemical solution containing concentrated nitric acid and concentrated sulfuric acid for oxidation treatment, the method is long in time, and complicated cleaning and drying steps are needed for removing a liquid oxidant and water; the pre-oxidation method is to put graphite in an oxidizing atmosphere at 400-1000 ℃ for surface oxidation, the method is easy to damage the graphite substrate and is different from a composite structure of a C/C composite material, the graphite material has consistent chemical properties at all places, uniform oxidation is easy to occur during oxidation, the pre-oxidized graphite surface is relatively smooth, and the improvement effect on the surface roughness and the surface area is small; the mechanical processing method is a method of recognizing a manufacturing defect on the surface of a graphite substrate by a mechanical method, which easily leaves stress on the surface of the graphite substrate and may damage the structure of the surface of the graphite substrate. The method is mainly used for increasing the fineness of the surface of the graphite substrate, and the problem of interface bonding strength still cannot be solved after the fineness of the surface of the graphite substrate is increased by the oxygen plasma bombardment method and then a coating is deposited.
Therefore, some methods are needed to improve the interfacial bonding between the graphite substrate and the TaC coating and increase the interfacial bonding strength of the two.
Disclosure of Invention
Based on the technical problems in the prior art, the method adopts an oxygen plasma or argon plasma bombardment method to simultaneously improve the roughness and the activity of the surface of the graphite substrate so as to solve the problem of the interface bonding strength between the graphite substrate and the TaC coating, and the process is simple and efficient, low in energy consumption, low in production cost and short in production period.
In order to achieve the above object, one of the objects of the present invention is to provide a method for treating a surface of a graphite substrate, which can increase the roughness and the surface activity of the graphite substrate to improve the bonding strength between the graphite substrate and a TaC coating, and can also increase the surface activity of the graphite substrate to further improve the bonding strength between the graphite substrate and the TaC coating, and the specific technical scheme is as follows:
a surface treatment method of a graphite substrate comprises the following steps:
cleaning and drying the graphite substrate, placing the graphite substrate into a reaction chamber of plasma modification equipment, closing an air inlet valve, vacuumizing the reaction chamber, filling the reaction chamber with oxygen or argon, adjusting the air inlet valve to enable the vacuum degree of the reaction chamber to be stabilized at 10-100Pa, starting radio frequency power supply discharge, carrying out oxygen plasma or argon plasma bombardment on the surface of the graphite substrate, and increasing the roughness of the surface of the graphite substrate, wherein the roughness is 1-5 mu m.
In some embodiments, the surface treatment method comprises the steps of:
cleaning the graphite substrate, putting the graphite substrate into a reaction chamber of plasma modification equipment, closing an air inlet valve, vacuumizing the reaction chamber, filling the reaction chamber with oxygen or argon, vacuumizing again, repeating the operations of gas filling and vacuumizing for 2-5 times, finally adjusting the air inlet valve to stabilize the vacuum degree of the reaction chamber at 10-100Pa, starting radio frequency power supply discharge, carrying out oxygen plasma or argon plasma bombardment on the surface of the graphite substrate, increasing the roughness of the surface of the graphite substrate and improving the activity of the surface of the graphite substrate.
In some embodiments, the plasma bombardment of the surface of the graphite substrate is performed for a time period of 1-30min; the treatment time is preferably 1-10min.
The invention also aims to provide a method for preparing a TaC coating with high bonding strength on the surface of a graphite substrate, which can ensure that the graphite substrate and the TaC coating have higher bonding strength, and the specific technical scheme is as follows:
a preparation method of a TaC coating comprises the following steps:
s1, treating the graphite substrate by using the surface treatment method of any one of claims 1 to 3, and increasing the roughness and the activity of the surface of the graphite substrate;
s2, placing the graphite substrate treated by the S1 into a chemical vapor deposition furnace, vacuumizing to below 50Pa, opening circulating cooling water, heating the chemical vapor deposition furnace to 1000-1400 ℃, and introducing carbon source gas and TaCl 5 、H 2 And carrying gas Ar gas, keeping the furnace pressure at 0-8000Pa, and depositing TaC coating with thickness of 20-300 μm.
In some embodiments, the TaCl is a metal halide 5 Is prepared from TaCl 5 The powder is carried by Ar gas after being heated and gasified.
In some embodiments, the TaCl is a metal halide 5 The heating temperature is 180-240 ℃.
In some embodiments, the Ar flow rate is 300 to 2000ml/min, H 2 The flow rate is 10-8000ml/min, and the flow rate of carbon source gas is 10-300ml/min.
In some embodiments, the carbon source is selected from the group consisting of, but not limited to, C 3 H 6 、CH 4 、C 2 H 6 、C 2 H 2 A gaseous hydrocarbon of at least one of; preferably, the carbon source is C 3 H 6 、CH 4 、C 2 H 6 、C 2 H 2 At least one of (a).
In some embodiments, the electroless deposition furnace ramp rate is from 2 to 10 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
the surface of the graphite substrate is modified by an oxygen plasma or argon plasma bombardment method, so that the roughness of the surface of the graphite substrate is increased, the surface activity is increased, the interface combination of the graphite substrate and the TaC coating is improved, the surface roughness of the graphite substrate bombarded by the oxygen plasma or the argon plasma is improved, and the graphite substrate is hardly damaged. The contact area of the treated graphite substrate and the TaC coating is greatly improved, the TaC coating can be embedded into the graphite substrate, the mechanical biting force between the graphite substrate and the TaC coating is enhanced, the activity of the surface of the graphite substrate is increased after treatment, and a two-phase region of the graphite substrate and the TaC coating is formed in the surface region of the graphite substrate, so that the gradient generated from the graphite substrate to the surface of the TaC coating on the material composition is favorably reduced, the mismatch of thermal stress and thermal expansion coefficient is relieved, the formed TaC coating is tightly combined with the graphite substrate and is not easy to fall off, the thermal stress and the thermal expansion coefficient between the graphite substrate and the TaC coating are relieved, and the thermal shock resistance is greatly improved. The graphite substrate treated by the oxygen plasma can be immediately put into a vapor deposition furnace for TaC coating deposition, the interface combination of the graphite substrate and the TaC coating can be improved with less time and cost, the process is simple and efficient, and the production period is short.
Furthermore, in the surface treatment method, the steps of gas introduction and vacuum pumping are repeated for 2-5 times, so that the purity of gas in the reaction chamber is higher, the effect is better when the surface of the graphite substrate is modified, and the interface strength between the graphite substrate and the TaC coating is enhanced; in addition, the roughness of the graphite substrate surface can be determined by controlling the gas bombardment treatment time.
After the surface treatment method provided by the invention is used, the graphite substrate is placed in a vapor deposition furnace for deposition of the TaC coating, the prepared TaC coating is tightly combined with the graphite substrate and is not easy to fall off, the thermal stress and the thermal expansion coefficient between the TaC coating and the graphite substrate are relieved, and the thermal shock resistance is greatly improved.
In addition, the thickness of the TaC coating on the surface of the graphite substrate can be controlled by controlling the deposition time so as to produce products according to actual requirements.
Drawings
FIG. 1 is a process flow diagram of example 2 of the present invention.
FIG. 2 is an interface diagram of the TaC coating prepared by the present invention bonded to a graphite substrate.
Fig. 3 is a graph showing the relationship between the oxygen plasma treatment time and the roughness.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms than those specifically described herein, and it will be apparent to those skilled in the art that many more modifications are possible without departing from the spirit and scope of the invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
The embodiment provides a surface treatment method for improving the bonding strength of a graphite substrate and a TaC coating, which comprises the following specific steps:
cleaning and drying a graphite substrate, placing the graphite substrate into a reaction chamber of oxygen plasma modification equipment, closing an air inlet valve of the reaction chamber, vacuumizing the reaction chamber, then introducing oxygen to fill the reaction chamber, vacuumizing again, refilling with oxygen, repeating the steps of inflating and vacuumizing for 2 times, finally adjusting the air inlet valve to ensure that the vacuum degree in the reaction chamber is stabilized below 50Pa, starting radio frequency power supply discharge, wherein the frequency is 13.56Mhz, the power is 1kW, and performing oxygen plasma bombardment on the surface of the graphite substrate for 7min; and turning off the radio frequency power supply to finish the surface treatment of the graphite substrate.
In this embodiment, argon plasma may be used to bombard the surface of the graphite substrate to modify the surface of the graphite substrate.
The roughness of the surface of the graphite base is changed along with the different bombardment time of the oxygen plasma or the argon plasma, as shown in fig. 3, the longer the treatment time, the higher the surface roughness, and multiple experiments of the inventor find that the roughness of the surface of the graphite base is suitable for embedding TaC into the graphite base and enhancing the mechanical biting force between the TaC and the graphite base when the treatment time is 1-30min, so that the TaC is tightly combined with the graphite base, the TaC is not easy to fall off, and the thermal shock resistance of the coating is improved. When the treatment time is less, the roughness of the graphite substrate surface is too low to allow TaC intercalation, so that the mechanical gripping force between the coating and the graphite substrate cannot be enhanced; when the treatment time is too long and the roughness is too large, the TaC is not favorably deposited on the surface of the graphite substrate; and when the treatment time is 7min, the roughness (about 3 mu m) of the graphite substrate surface can greatly enhance the bonding strength between the graphite substrate surface and the graphite substrate surface, and the deposited TaC coating has excellent compactness and good thermal shock resistance.
Example 2
The embodiment provides a method for high-strength bonding of a graphite substrate and a TaC coating, which specifically includes the following steps, as shown in fig. 1:
s1, treating a graphite substrate in the manner of example 1;
s2, placing the graphite substrate treated by the oxygen plasma into a chemical vapor deposition furnace, vacuumizing to below 50Pa, opening circulating cooling water to cool a pump set for vacuumizing and a furnace body of the chemical vapor deposition furnace so as to protect the furnace body, heating the deposition furnace to 1300 ℃, wherein the heating rate is 5 ℃/min; when the temperature of the vapor deposition furnace reaches 1300 ℃, introducing C 3 H 6 (or CH) 4 Or C 2 H 6 Or C 2 H 2 )、TaCl 5 、H 2 And a carrier gas Ar gas, and carrying out TaC coating deposition, wherein the deposition thickness is adjusted by controlling the deposition time, and the thickness of the TaC coating prepared by the embodiment is 20-300 mu m; wherein the Ar gas flow is 300-2000ml/min, H 2 The flow rate is 10-800ml/min, C 3 H 6 (or CH) 4 Or C 2 H 6 Or C 2 H 2 ) Flow rate of 10-300ml/min, vapor depositionThe furnace pressure in the furnace is kept between 0 and 8000Pa; wherein, taCl 5 Is TaCl 5 Heating and gasifying the powder at 180-240 deg.c, introducing Ar gas, closing the chemical vapor deposition furnace after deposition reaction, stopping reaction, lowering the temperature inside the furnace to room temperature and taking out the product.
The product prepared in this example (carbon composite material with graphite substrate as base material and TaC as coating) was cut along the direction perpendicular to the surface of TaC coating, and the interfacial bonding between graphite substrate and TaC coating of the product cross section was observed, as shown in fig. 2.
As shown in fig. 2, in the carbon composite material prepared by the present embodiment, the interface between the TaC coating and the graphite substrate surface is combined in an embedded manner, a certain roughness is formed on the surface of the graphite substrate treated by the oxygen plasma, and during the deposition reaction, the TaC deposits the concave position on the graphite substrate surface and is embedded into the graphite substrate, so that the interface combination manner can enhance the mechanical engagement force between the TaC coating and the graphite substrate, is beneficial to reducing the gradient generated on the material composition from the graphite substrate to the TaC coating surface, relieves the mismatch of thermal stress and expansion coefficient, and enhances the interface combination strength between the TaC coating and the graphite substrate, so that the TaC coating and the graphite substrate are combined tightly and are not easy to fall off, and the thermal shock resistance is greatly improved.
Example 3
The embodiment provides a method for high-strength bonding of a graphite substrate and a TaC coating, which specifically comprises the following steps:
s1, treating a graphite substrate in the manner of example 1;
s2, placing the graphite substrate treated by the oxygen plasma into a chemical vapor deposition furnace, vacuumizing to below 50Pa, opening circulating cooling water, heating the deposition furnace to 1000 ℃, wherein the heating rate is 2 ℃/min; when the temperature of the vapor deposition furnace reaches 1000 ℃, introducing C 3 H 6 、TaCl 5 、H 2 And a carrier gas Ar gas, and carrying out TaC coating deposition, wherein the deposition thickness is adjusted by controlling the deposition time, and the thickness of the TaC coating prepared by the embodiment is 100 mu m; wherein the flow rate of Ar is 1000ml/min, H 2 The flow rate is 300ml/min, C 3 H 6 Flow rate of 20ml/min, gas phaseMaintaining the furnace pressure in the deposition furnace at 1000Pa; wherein, taCl 5 Is TaCl 5 Heating and gasifying the powder at 180-240 deg.c, introducing Ar gas, closing the chemical vapor deposition furnace after deposition reaction, stopping reaction, lowering the temperature inside the furnace to room temperature and taking out the product.
Example 4
The embodiment provides a method for high-strength bonding of a graphite substrate and a TaC coating, which specifically comprises the following steps:
s1, treating a graphite substrate in the mode of the embodiment 1;
s2, placing the graphite substrate treated by the oxygen plasma into a chemical vapor deposition furnace, vacuumizing to below 50Pa, opening circulating cooling water, heating the deposition furnace to 1400 ℃, wherein the heating rate is 10 ℃/min; when the temperature of the vapor deposition furnace reaches 1400 ℃, introducing C 2 H 6 、TaCl 5 、H 2 And a carrier gas Ar gas, and carrying out TaC coating deposition, wherein the deposition thickness is adjusted by controlling the deposition time, and the thickness of the TaC coating prepared in the embodiment is 50 μm; wherein the flow rate of Ar is 1000ml/min, H 2 Flow rate of 300ml/min, C 2 H 6 The flow rate is 60ml/min, and the furnace pressure in the vapor deposition furnace is kept at 100Pa; wherein, taCl 5 Is TaCl 5 Heating and gasifying the powder at 180-240 deg.c, introducing Ar gas, closing the chemical vapor deposition furnace after deposition reaction, stopping reaction, lowering the temperature inside the furnace to room temperature and taking out the product.
Example 5
The embodiment provides a method for high-strength bonding of a graphite substrate and a TaC coating, which specifically comprises the following steps:
s1, treating a graphite substrate in the manner of example 1;
s2, placing the graphite substrate treated by the oxygen plasma into a chemical vapor deposition furnace, vacuumizing to below 50Pa, opening circulating cooling water, heating the deposition furnace to 1200 ℃, wherein the heating rate is 8 ℃/min; when the temperature of the vapor deposition furnace reaches 1200 ℃, CH is introduced 4 、TaCl 5 、H 2 And a carrier gas Ar gas for TaC coating depositionThe deposition thickness is adjusted by controlling the deposition time, and the thickness of the TaC coating prepared by the embodiment is 300 mu m; wherein the flow rate of Ar is 2000ml/min, H 2 The flow rate is 800ml/min, CH 4 The flow rate is 180ml/min, and the furnace pressure in the vapor deposition furnace is kept at 5000Pa; wherein, taCl 5 Is TaCl 5 Heating and gasifying the powder at 180-240 deg.c, introducing Ar gas, closing the chemical vapor deposition furnace after deposition reaction, stopping reaction, lowering the temperature inside the furnace to room temperature and taking out the product.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (6)
1. A preparation method of a TaC coating is characterized by comprising the following steps:
s1, cleaning and drying a graphite substrate, placing the graphite substrate into a reaction chamber of plasma modification equipment, closing an air inlet valve, vacuumizing the reaction chamber, filling the reaction chamber with oxygen or argon, adjusting the air inlet valve to enable the vacuum degree of the reaction chamber to be stabilized at 10-100Pa, starting radio frequency power supply discharge, bombarding the surface of the graphite substrate by oxygen plasma or argon plasma, increasing the roughness of the surface of the graphite substrate and improving the activity of the surface of the graphite substrate, wherein the roughness is 1-5 mu m;
s2, placing the graphite substrate treated by the S1 into a chemical vapor deposition furnace, vacuumizing to below 50Pa, and opening for circulationCooling water circularly, heating the chemical vapor deposition furnace to 1000-1400 deg.C, and introducing carbon source gas and TaCl 5 、H 2 And a carrier gas Ar gas, wherein the furnace pressure is kept at 100-8000Pa, and TaC coating deposition is carried out, and the thickness of the TaC coating is 20-300 mu m;
wherein the carbon source gas is gaseous hydrocarbon;
the Ar gas flow is 300-2000ml/min, H 2 The flow rate is 10-8000ml/min, and the flow rate of carbon source gas is 10-300ml/min.
2. The process for the preparation of a TaC coating according to claim 1, comprising the following steps:
cleaning the graphite substrate, putting the graphite substrate into a reaction chamber of plasma modification equipment, closing an air inlet valve, vacuumizing the reaction chamber, filling the reaction chamber with oxygen or argon, vacuumizing again, repeating the operations of gas filling and vacuumizing for 2-5 times, finally adjusting the air inlet valve to ensure that the vacuum degree of the reaction chamber is stabilized at 10-100Pa, starting radio frequency power supply discharge, carrying out oxygen plasma or argon plasma bombardment on the surface of the graphite substrate, increasing the roughness of the surface of the graphite substrate and improving the activity of the surface of the graphite substrate.
3. The method for preparing TaC coating according to claim 1, wherein the plasma bombardment of the surface of the graphite substrate is performed for 1-30min.
4. The method of preparing a TaC coating according to claim 1, wherein the TaCl is present in the form of TaCl 5 Is prepared from TaCl 5 The powder is carried in by Ar gas after being heated and gasified.
5. A process for the preparation of a TaC coating according to claim 4, wherein said TaCl is present 5 The heating temperature is 180-240 ℃.
6. The process for the preparation of a TaC coating according to claim 1, wherein,the carbon source gas is C 3 H 6 、CH 4 、C 2 H 6 、C 2 H 2 At least one of (a).
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