CN111763924A - Silicon carbide-silicon dioxide/diamond multilayer composite self-supporting film and preparation method thereof - Google Patents

Silicon carbide-silicon dioxide/diamond multilayer composite self-supporting film and preparation method thereof Download PDF

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CN111763924A
CN111763924A CN202010561137.XA CN202010561137A CN111763924A CN 111763924 A CN111763924 A CN 111763924A CN 202010561137 A CN202010561137 A CN 202010561137A CN 111763924 A CN111763924 A CN 111763924A
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sic
sio
diamond
multilayer composite
graphite
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CN111763924B (en
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高洁
马丹丹
吴玉程
郑可
申艳艳
吴艳霞
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Taiyuan University of Technology
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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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • C23C16/325—Silicon carbide
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/401—Oxides containing silicon
    • C23C16/402—Silicon dioxide
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/517—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using a combination of discharges covered by two or more of groups C23C16/503 - C23C16/515

Abstract

The invention relates to a high-transmittance antioxidant silicon carbide-silicon dioxide/diamond multilayer composite self-supporting film, belonging to the technical field of chemical vapor deposition. The multilayer composite self-supporting film is made of SiC-SiO2The composite layer and the diamond film are alternately overlapped in sequence, and the upper surface, the lower surface and the side surfaces of the composite layer are all SiC-SiO2And (4) compounding layers. When the multilayer composite self-supporting film is prepared, firstly, a plasma-assisted chemical vapor deposition method is adopted to prepare SiC-SiO on the surface of a graphite substrate2Composite layer of SiC-SiO2Depositing diamond film on the composite layer, repeating the above steps, and removing the graphite matrix by oxidation. The invention does not adopt the traditional diamond surface coating process, and the corrosion resistance of the diamond and the SiC-SiO by preparing the multilayer composite self-supporting film2The antioxidant capacity of the diamond is combined, and the problem of poor antioxidant capacity when the diamond is used as an infrared optical material at present is solved.

Description

Silicon carbide-silicon dioxide/diamond multilayer composite self-supporting film and preparation method thereof
Technical Field
The invention relates to the technical field of chemical vapor deposition, in particular to a high-transmittance antioxidant silicon carbide-silicon dioxide/diamond multilayer composite self-supporting film and a preparation method thereof.
Background
The infrared system, especially the infrared guidance system, has a very harsh working environment, and has strict requirements on the infrared optical elements exposed outside in the optical system, such as a fairing, an optical window and the like, the material has excellent characteristics of high infrared transmittance, low absorption coefficient and the like, and also has the performances of high mechanical strength, good heat dissipation, wear resistance, sand corrosion resistance, rain corrosion resistance, chemical corrosion resistance and the like, and common infrared optical materials with the requirements, such as silicon (Si), germanium (Ge), zinc sulfide (ZnS) and zinc selenide (ZnSe), cannot meet the requirements. And the Chemical Vapor Deposition (CVD) diamond has excellent performances of high infrared transmittance, low absorption coefficient, good thermal shock resistance, high thermal conductivity and the like, and the characteristics just meet the requirements on the infrared optical window material. Thus, diamond is an ideal material for long wavelength infrared (8-12 μm) window and hood applications in high speed aircraft.
However, the thermal stability of diamond is poor, and during the high-speed flight of an aircraft, the surface temperature of a window or a head cover of the aircraft is sharply increased due to aerodynamic heating, when the temperature reaches about 650 ℃, the diamond coating starts to be oxidized in the atmosphere, and the diamond coating starts to be converted into graphite at about 1500 ℃ under the vacuum or inert atmosphere. These problems have severely limited the use of diamond as an infrared window in high temperature oxidizing environments. At present, researchers mostly improve the oxidation resistance of the alloy through ion implantation or plating double-layer or multi-layer high-temperature resistant films. However, any coating is also inferior to diamond in corrosion resistance, and once the outer oxidation protection film is etched, the diamond is exposed to the atmosphere and is again subject to oxidation.
Disclosure of Invention
The inventionAiming at solving the problem that the current infrared optical window material can not meet the use requirement in a severe environment, the invention provides the oxidation-resistant SiC-SiO with high transmittance2The diamond multilayer composite self-supporting film.
The invention is realized by the following technical scheme:
a high-permeability antioxidizing silicon carbide-silicon dioxide/diamond multi-layer composite self-supporting film is prepared from SiC-SiO2The composite layers and the diamond films are sequentially and alternately superposed, and the upper surface, the lower surface and the side surfaces of the composite layers are SiC-SiO2 composite layers.
As a preferred technical scheme, SiC-SiO2The composite layer and the diamond film are prepared by adopting a plasma-assisted chemical vapor deposition method.
As a preferred technical scheme, SiC-SiO2The thickness of the composite layer is 0.1-20 μm, and the thickness of the diamond film is 10-100 μm.
Further, the invention also provides a preparation method of the high-transmittance antioxidant silicon carbide-silicon dioxide/diamond multilayer composite self-supporting film, which comprises the following steps:
1) preparing SiC and SiO on the surface of the graphite matrix by adopting a plasma-assisted chemical vapor deposition method and taking mixed gas containing silicon-carbon gas, hydrogen and oxygen as reaction gas2Phase SiC-SiO2Compounding layers;
2) introducing methane, and increasing the flow of methane while decreasing the flow of oxygen and the flow of a gas containing silicon and carbon in SiC-SiO2Depositing a diamond film on the composite layer;
3) repeated preparation of SiC-SiO2The operation processes of compounding layers and depositing diamond films are sequentially and alternately carried out, and finally SiC-SiO with the thickness of 0.2-5mm is formed on the graphite substrate2A diamond multilayer composite layer;
4) repeating the step 1) on the SiC-SiO2Preparing a layer of SiC-SiO on the upper surface and the side surface of the diamond multilayer composite layer2Compounding layers;
5) inverting the test piece to expose the graphite matrix in oxygen atmosphere, oxidizing and removing the graphite matrix, and finally removing the graphite matrixObtaining complete high-transmittance antioxidant SiC-SiO2The diamond multilayer composite self-supporting film.
As a preferred technical scheme, SiC-SiO2The preparation method of the composite layer comprises respectively ultrasonic cleaning graphite with deionized water and anhydrous ethanol, hot air drying, placing cleaned graphite in a titanium mold with a groove, wherein the height of the upper surface of the graphite is 0-3mm lower than that of a boss at the edge of the titanium mold, placing the graphite and the titanium mold into a microwave plasma assisted chemical vapor deposition experimental device, and vacuumizing to 9 × 10 in a furnace-4Introducing silicon-carbon-containing gas, hydrogen and oxygen as reaction gases after the pressure is less than Pa, and preparing SiC-SiO on the surface of the graphite matrix2Compounding layers; wherein the technological parameters are as follows: the temperature of the graphite substrate is 750-1200 ℃, the hydrogen flow is 200-1000sccm, the silicon-carbon-containing gas accounts for 0.1-10% of the volume of the hydrogen, the oxygen accounts for 0.1-10% of the volume of the hydrogen, the gas pressure is 2-20kPa, the power is 1-10kW, and the deposition time is 10min-5 h;
as a preferred technical scheme, the specific preparation method of the diamond film comprises the following steps: SiC-SiO2After the preparation of the composite layer is finished, introducing methane into the experimental device, gradually stopping introducing oxygen and silicon-carbon-containing gas while increasing the flow of methane, controlling the flow of hydrogen to be 1000sccm, controlling the volume percentage of methane to be 1-10% of hydrogen, controlling the gas pressure to be 5-30 kPa, controlling the power to be 1-10kW, controlling the temperature of the base material to be 800-1250 ℃ during deposition, and controlling the deposition time to be 2-100 h;
as a preferable technical proposal, SiC-SiO of the outermost layer2The specific preparation method of the composite layer comprises the following steps: after the final layer of diamond film is deposited, the titanium mold is replaced to make the upper surface of the graphite substrate higher than the height of the lug boss at the edge of the titanium mold, and then the graphite substrate is placed in a microwave plasma-assisted chemical vapor deposition experimental device to prepare SiC-SiO2Exposing the diamond multilayer composite layer in plasma, and performing SiC-SiO on the upper surface and the side surface of the diamond multilayer composite layer2Preparing a composite layer, wherein the process parameters are as follows: the temperature of the graphite substrate is 850-1200 ℃, the hydrogen flow is 200-1000sccm, the silicon-carbon-containing gas accounts for 0.1-10% of the volume of the hydrogen, the oxygen accounts for 0.1-10% of the volume of the hydrogen, the gas pressure is 2-20kPa, and the power is high1-10kW, and deposition time is 10min-5 h.
Preferably, the method for removing the graphite substrate by oxidation is a thermal oxidation method or a microwave plasma oxidation method.
As a preferred technical scheme, the silicon-carbon containing gas is tetramethylsilane (Si (CH)3)4TMS), trichloromethylsilane (CH)3SiCl3) Or tetraethoxysilane (Si (OC)2H5)4）。
The invention discloses high-transmittance antioxidant SiC-SiO2The diamond multilayer composite self-supporting film does not adopt the traditional diamond surface coating process, but passes through the diamond film and SiC-SiO2The composite layers are formed by repeating and alternating in sequence, and the corrosion resistance of the diamond is improved by the SiC-SiO2The antioxidant capacity of the diamond is combined, and the problem of poor antioxidant capacity when the diamond is used as an infrared optical material at present is solved.
The diamond has excellent performance, is an ideal material for a long-wave infrared (8-12 mu m) window and a head cover of a high-speed aircraft, but has the problem of poor oxidation resistance when being applied as an optical window and head cover material, and SiC and SiO2Has good oxidation resistance, wherein the oxidation resistance of SiC is realized by forming compact SiO2The protective film is realized, so the outermost layer of the multilayer composite self-supporting film is designed to be SiC-SiO2Composite layer of outermost SiC-SiO in use as an optical window or head cap2The SiC in the composite layer is oxidized and converted into SiO2So that dense SiO is formed2A membrane providing oxidation protection to the multilayer composite self-supporting membrane. In addition, the multilayer film can also provide multiple layers of protection, the next layer of SiC — SiO once the outermost oxide and diamond films are consumed2The composite layer is converted into a new outer oxidation resistant layer, again providing oxidation protection for the multilayer composite self-supporting film as a whole.
Diamond, SiC and SiO2The three materials have different Coefficients of Thermal Expansion (CTE), wherein CTESiC>CTEDiamond>CTESiO2The invention prepares SiC-SiO2Laminating it with goldThe diamonds have similar thermal expansion coefficients, which is beneficial to reducing the interface stress generated by the difference of the thermal expansion coefficients and improving the bonding performance between layers. In addition, the multilayer film is also beneficial to reducing the film thickness of each layer of film and reducing the stress of an interlayer interface by increasing the number of layers. The combined effect of these two aspects ensures that the stresses in the composite as a whole are at a low level and do not fail during use due to spalling or cracking of the coating.
The composite film belongs to a self-supporting film, and can comprehensively utilize diamond, SiC and SiO2High permeability of (2), wherein SiO2The permeability of the composite self-supporting film is superior to that of diamond, the permeability of SiC is lower than that of diamond, and the multilayer composite self-supporting film with different permeabilities can be obtained by controlling the process, so that the application requirements of different occasions are met.
The chemical vapor deposition diamond generally grows in a columnar crystal mode, the columnar crystal of the diamond grows continuously along with the increase of the film thickness, and the breaking strength of the diamond film is reduced continuously2The composite layer is used as an anti-oxidation layer and also becomes a nucleation substrate of each diamond film, the diamond is blocked from continuously growing along the diamond grains on the previous layer, and the re-nucleation and growth of the diamond are promoted, so that the diamond grains are ensured to be finer, and the fracture strength of the diamond and the toughness of the material are enhanced through a fine grain strengthening effect.
The invention has the following beneficial effects:
1) the invention adopts the plasma-assisted chemical vapor deposition technology to repeatedly and repeatedly carry out SiC-SiO on the graphite surface in sequence2The preparation of composite layer and the growth of diamond film are alternated, and the bottommost layer, the topmost layer and the side surface are all SiC-SiO2And a composite layer, which makes the diamond film completely wrapped in the antioxidation layer. By multilayer SiC-SiO2The diamond film is circularly and alternately compounded, and SiC-SiO can be effectively compounded2The oxidation resistance is combined with the corrosion resistance and heat dissipation performance of the diamond.
2) The SiC-SiO prepared by the invention2The composite layer is used as high temperature oxidation resisting layer, in which the SiC thermal expansion coefficient is slightly higher than that of diamond and SiO2Coefficient of thermal expansion ofSlightly lower than diamond, by preparing a mixture of the two2The composite layer has similar thermal expansion coefficient with diamond, which is favorable for reducing the interface stress generated by the difference of thermal expansion coefficient and improving the bonding performance between layers.
3) The invention is used for preparing SiC-SiO2When the diamond multilayer composite self-supporting film is adopted, the same microwave plasma assisted chemical vapor deposition device is adopted, so that the reaction gas flow for preparing the composite layer and the diamond layer can be controlled to slowly change, and the SiC-SiO2The gradient distribution of the components at the interface of the composite layer/the diamond film can also improve the bonding performance between layers.
4) SiO selected by the invention2Has excellent oxidation resistance, and SiC can be oxidized to form SiO in oxygen2Therefore, the combination of the two is beneficial to providing effective antioxidant protection for diamond, and both have good transmittance, so that the formed SiC-SiO2The diamond multilayer composite self-supporting film has high transmittance and good oxidation resistance. Meanwhile, the composite self-supporting film also has excellent performances such as high thermal conductivity and high hardness, and can better meet the use requirement of an infrared optical window.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the embodiments or the prior art descriptions will be briefly introduced, wherein the drawings are used for providing further explanation of the present invention and form a part of the present application, and the exemplary embodiments and the explanation of the present invention are used for explaining the present invention and do not form a limitation to the present invention.
FIG. 1 shows the preparation of SiC-SiO on the surface of the graphite substrate according to the invention2Schematic cross-sectional view of the composite layer.
FIG. 2 shows a SiC-SiO crystal composition of the present invention2The cross-sectional view of the diamond film deposited on the surface of the graphite substrate of the composite layer is shown.
FIG. 3 shows SiC-SiO of the present invention2Schematic cross-sectional view of the diamond multilayer composite film after preparation.
FIG. 4 shows an outermost SiC-SiO layer of the present invention2Schematic cross-sectional view of the composite layer after preparation.
FIG. 5 shows SiC-SiO obtained by removing graphite matrix according to the present invention2The finished product of the diamond multilayer composite self-supporting film.
In the figure: 1-graphite matrix, 2-SiC-SiO2Composite layer, 3-diamond film and 4-titanium film.
Detailed Description
In order that those skilled in the art will better understand the present invention, a more complete and complete description of the present invention is provided below in conjunction with the accompanying drawings and embodiments. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
A high-permeability antioxidizing silicon carbide-silicon dioxide/diamond multi-layer composite self-supporting film is prepared from SiC-SiO2The composite layers and the diamond films are sequentially and alternately superposed, and the upper surface, the lower surface and the side surfaces of the composite layers are SiC-SiO2 composite layers. Wherein, SiC-SiO2The composite layer and the diamond film are prepared by adopting a plasma-assisted chemical vapor deposition method, and the SiC-SiO2The thickness of the composite layer is 0.1-20 μm, and the thickness of the diamond film is 10-100 μm.
The preparation method of the high-transmittance antioxidant silicon carbide-silicon dioxide/diamond multilayer composite self-supporting film comprises the following steps:
1) preparing SiC and SiO on the surface of the graphite matrix by adopting a plasma-assisted chemical vapor deposition method and taking mixed gas containing silicon-carbon gas, hydrogen and oxygen as reaction gas2Phase SiC-SiO2The preparation method of the composite layer comprises respectively performing ultrasonic cleaning on graphite with deionized water and anhydrous ethanol, drying with hot air, placing the cleaned graphite in a titanium mold with a groove, wherein the height of the upper surface of the graphite is 0-3mm lower than that of a boss at the edge of the titanium mold, placing the graphite and the titanium mold into a microwave plasma assisted chemical vapor deposition experimental device, and vacuumizing to 9 × 10 in a furnace-4Introducing silicon-carbon-containing gas, hydrogen and oxygen as reaction gases after the pressure is less than Pa, and preparing SiC-SiO on the surface of the graphite matrix2Compounding layers; wherein the processThe parameters are as follows: the graphite matrix temperature is 750-.
2) Introducing methane, and increasing the flow of methane while decreasing the flow of oxygen and the flow of a gas containing silicon and carbon in SiC-SiO2The diamond film is deposited on the composite layer, and the specific preparation method comprises the following steps: SiC-SiO2After the preparation of the composite layer is finished, introducing methane into the experimental device, gradually stopping introducing oxygen and silicon-carbon-containing gas while increasing the flow of methane, controlling the flow of hydrogen to be 200-1250 sccm, controlling the volume percentage of methane in the hydrogen to be 1-10%, controlling the gas pressure to be 5-30 kPa, controlling the power to be 1-10kW, and controlling the temperature of the base material to be 800-1250 ℃ during deposition and the deposition time to be 2-100 h.
3) Repeated preparation of SiC-SiO2The operation processes of compounding layers and depositing diamond films are sequentially and alternately carried out, and finally SiC-SiO with the thickness of 0.2-5mm is formed on the graphite substrate2A diamond multilayer composite layer;
4) repeating the step 1) on the SiC-SiO2Preparing a layer of SiC-SiO on the upper surface and the side surface of the diamond multilayer composite layer2The composite layer is prepared by the following specific preparation method: after the final layer of diamond film is deposited, the titanium mold is replaced to make the upper surface of the graphite substrate higher than the height of the lug boss at the edge of the titanium mold, and then the graphite substrate is placed in a microwave plasma-assisted chemical vapor deposition experimental device to prepare SiC-SiO2Exposing the diamond multilayer composite layer in plasma, and performing SiC-SiO on the upper surface and the side surface of the diamond multilayer composite layer2Preparing a composite layer, wherein the process parameters are as follows: the temperature of the graphite substrate is 850-1200 ℃, the hydrogen flow is 200-1000sccm, the silicon-carbon-containing gas accounts for 0.1-10% of the volume of the hydrogen, the oxygen accounts for 0.1-10% of the volume of the hydrogen, the gas pressure is 2-20kPa, the power is 1-10kW, and the deposition time is 10min-5 h.
5) Inverting the test piece to expose the graphite matrix in oxygen atmosphere, and oxidizing the graphite matrix by thermal oxidation or microwave plasma oxidationRemoving the oxide to obtain the complete high-transmittance antioxidant SiC-SiO2The diamond multilayer composite self-supporting film.
It is noted that the repeated preparation of SiC-SiO2In the operation process of composite layer and diamond film deposition, SiC-SiO is required to be expected2The thickness of the diamond multilayer composite self-supporting film is adjusted, and the depth of the groove of the titanium die is adjusted to ensure that the SiC-SiO2The height of the diamond multilayer composite self-supporting film does not exceed the height of the edge boss of the titanium die.
The technical scheme of the invention is further explained by combining a plurality of specific embodiments as follows:
example 1
1) Preparation of SiC-SiO2Composite layer 2
Cleaning the surface of a graphite matrix, putting the graphite matrix 1 with the diameter of 60mm and the thickness of 3mm as a substrate into absolute ethyl alcohol for ultrasonic cleaning for 10min, and drying by hot air;
putting the cleaned graphite substrate 1 into a titanium mold 4 with the outer diameter of 65mm, the height of 10mm, the diameter of a groove of 60.1mm and the depth of 3.1mm, then putting the graphite substrate in the central position of a base table in a reaction cavity of a microwave plasma assisted chemical vapor deposition experimental device, closing the cavity and vacuumizing;
pumping the vacuum degree of the cavity to 9 × 10-4After Pa is less, H is introduced2The flow is controlled to be 220sccm, when the air pressure of the cavity is increased to 8kPa, the microwave power is set to be 1kW, the microwave power supply is started, the microwave plasma is excited, and TMS and O are introduced2Controlling the flow rate to be 3sccm, simultaneously increasing the air pressure and the power, stabilizing the parameters when the temperature of the substrate is increased to 800 ℃, and performing SiC-SiO2Depositing the composite layer 2 for 30min to obtain SiC-SiO with thickness of about 0.5 μm2And (6) a composite layer 2.
As shown in FIG. 1, the preparation of SiC-SiO on the surface of the graphite substrate 1 is shown2Schematic cross-sectional view of the composite layer 2.
2) Preparation of the Diamond film 3
SiC-SiO2After the preparation of the composite layer 2 is finished, CH is slowly introduced into the experimental device4Increase CH4And H2Gradually stopping introducing O at the same time of the flow2And TMS, control H2The flow rate is 400sccm and CH4The flow is 16sccm, the gas pressure is kept at about 8kPa, the deposition of the diamond film 3 is carried out when the temperature of the substrate is raised to 900 ℃ and the parameters are stabilized, the time is controlled to be 20h, and the thickness of the diamond film 3 is ensured to be 30 +/-5 mu m.
As shown in FIG. 2, it is shown in SiC-SiO2The composite layer 2 has a schematic cross-sectional view of the diamond film 3 deposited on the surface.
3) Preparation of SiC-SiO again2 Layer 2
After the deposition of the diamond film 3 is finished, TMS and O are slowly introduced2And gradually stop the introduction of CH4，TMS、O2The flow rates are controlled to be 3sccm and H2The flow is adjusted to 220sccm, the air pressure and power are adjusted to maintain the substrate temperature at 800 ℃, the parameters are stabilized, and SiC-SiO is carried out2Deposition of the composite layer 2 for 30min to obtain SiC-SiO with a thickness of about 0.5 μm2Layer 2.
4）SiC-SiO2Diamond multilayer composite film
Repeating the steps 2) and 3) to prepare SiC-SiO2The diamond multilayer composite film has the total thickness of 3mm and the uppermost layer of diamond film 3; in the process, the titanium die 4 is replaced according to the film thickness, so that SiC-SiO2The upper surface of the diamond multilayer composite film is lower than the height of a lug boss at the edge of the titanium mold 4, and CH is stopped to be introduced after the deposition of the diamond film 3 is finished4Gradually reducing the pressure of the cavity of the microwave power meter to 1kW and 1kPa, closing the microwave power supply, and stopping introducing H2And closing the vacuum system and taking out the graphite sample containing the composite membrane.
As shown in FIG. 3, it represents SiC-SiO2Schematic cross-sectional view of the diamond multilayer composite film after preparation.
5) Preparation of outermost layer of SiC-SiO2Composite layer
Will contain SiC-SiO2Placing the graphite substrate of the diamond composite layer into a titanium die 4 with a groove depth of 3mm to enable the upper surface of the graphite substrate 1 to be higher than the height of a lug boss at the edge of the titanium die 4, then placing the graphite substrate in the central position of a reaction cavity base station, and after the graphite substrate is pumped out of the furnaceVacuum to 9 × 10-4After Pa is less, the silicon carbide powder contains SiC-SiO2SiC-SiO is carried out on the upper surface and the side surface of a graphite matrix of a diamond film exposed in plasma2Preparing a composite layer 2, and the process parameters are the same as those in the step 1).
As shown in FIG. 4, SiC-SiO as the outermost layer2SiC-SiO after the preparation of the composite layer is finished2Schematic cross-sectional view of a diamond multilayer composite membrane.
6) Removal of graphite matrix
The sample was placed upside down in a titanium mold 4 having a groove depth of 3.2mm to make the multilayer SiC-SiO2The diamond multilayer composite film is contained in the groove of the titanium mold 4, the graphite matrix 1 is exposed outside, the graphite matrix 1 is oxidized and removed, and finally the outermost layer is SiC-SiO2A multilayer composite self-supporting film of composite layers.
As shown in FIG. 5, SiC-SiO obtained after removal of the graphite matrix is shown2Schematic cross-sectional view of a diamond multilayer composite self-supporting film.
Example 2
1) Preparation of SiC-SiO2Composite layer 2
Cleaning the surface of the graphite substrate: taking a graphite matrix 1 with the diameter of 60mm and the thickness of 4mm as a substrate, putting the substrate into absolute ethyl alcohol for ultrasonic cleaning for 10min, and drying the substrate by hot air;
putting the cleaned graphite substrate 1 into a titanium mold 4 with the outer diameter of 65mm, the height of 10mm, the diameter of a groove of 60.1mm and the depth of 4.1mm, then putting the graphite substrate in the central position of a base table in a reaction cavity of a microwave plasma assisted chemical vapor deposition experimental device, closing the cavity and vacuumizing;
pumping the vacuum degree of the cavity to 9 × 10-4After Pa is less, H is introduced2The flow is controlled to be 200sccm, when the air pressure of the cavity is increased to 2kPa, the microwave power is set to be 10kW, the microwave power supply is started, the microwave plasma is excited, and TMS and O are introduced2Controlling the flow rate to be 5sccm, simultaneously increasing the air pressure and the power, stabilizing the parameters when the temperature of the substrate is increased to 750 ℃, and performing SiC-SiO2Depositing a composite layer for 10min to obtain SiC-SiO with the thickness of about 0.1 mu m2And (6) a composite layer 2.
As shown in FIG. 1, the preparation of SiC-SiO on the surface of graphite is shown2Schematic cross-sectional view of the composite layer 2.
2) Preparation of the Diamond film 3
SiC-SiO2After the preparation of the composite layer 2 is finished, CH is slowly introduced into the experimental device4Increase CH4And H2Gradually stopping introducing O at the same time of the flow2And TMS, control H2The flow rate is 1000sccm and CH4The flow is 32sccm, the gas pressure is kept at about 30kPa, the deposition of the diamond film 3 is carried out when the temperature of the substrate is raised to 800 ℃ and the parameters are stabilized, the time is controlled to be 2h, and the thickness of the diamond film 3 is ensured to be 100 mu m.
As shown in FIG. 2, it is shown in SiC-SiO2The composite layer 2 has a schematic cross-sectional view of the diamond film 3 deposited on the surface.
3) Preparation of SiC-SiO again2 Layer 2
After the deposition of the diamond film 3 is finished, TMS and O are slowly introduced2And gradually stop the introduction of CH4TMS and oxygen flow are controlled to be 5sccm and H2The flow is adjusted to 300sccm, the air pressure and power are adjusted to maintain the substrate temperature at 750 ℃, the parameters are stabilized, and SiC-SiO is carried out2Depositing the composite layer 2 for 10min to obtain SiC-SiO with thickness of about 0.5 μm2Layer 2.
4）SiC-SiO2Diamond multilayer composite film
Repeating the steps 2) and 3) to prepare SiC-SiO2A diamond multilayer composite film having a total film thickness of 4mm and a diamond film 3 as the uppermost layer, wherein a titanium mold 4 is replaced according to the film thickness to form a SiC-SiO2The upper surface of the diamond multilayer composite film is lower than the height of a lug boss at the edge of the titanium mold 4, and CH is stopped to be introduced after the deposition of the diamond film 3 is finished4Gradually reducing the pressure of the cavity of the microwave power meter to 10kW and 1kPa, closing the microwave power supply, and stopping introducing H2And closing the vacuum system and taking out the graphite sample containing the composite membrane.
As shown in FIG. 3, it represents SiC-SiO2Schematic cross-sectional view of the diamond multilayer composite film after preparation.
5) System for makingPreparing SiC-SiO of the outermost layer2Composite layer
Will contain SiC-SiO2Placing the graphite substrate 1 of the diamond composite layer into a titanium die 4 with the groove depth of 4mm to ensure that the upper surface of the graphite substrate 1 is higher than the height of a lug boss at the edge of the titanium die 4, then placing the graphite substrate at the central position of a reaction cavity base station, and vacuumizing the furnace to 9 × 10-4After Pa is less, the silicon carbide powder contains SiC-SiO2SiC-SiO is carried out on the upper surface and the side surface of the graphite matrix 1 of the diamond film exposed in the plasma2Preparing a composite layer 2, and the process parameters are the same as those in the step 1).
As shown in FIG. 4, SiC-SiO as the outermost layer2SiC-SiO after the preparation of the composite layer is finished2Schematic cross-sectional view of a diamond multilayer composite membrane.
6) Removal of graphite matrix
The sample was placed upside down in a titanium mold 4 having a groove depth of 4.2mm to make the multilayer SiC-SiO2The diamond multilayer composite film is contained in the groove of the titanium mold 4, the graphite matrix 1 is exposed outside, the graphite matrix 1 is oxidized and removed, and finally the outermost layer is SiC-SiO2A multilayer composite self-supporting film of composite layers.
As shown in FIG. 5, SiC-SiO obtained after removal of the graphite matrix is shown2Schematic cross-sectional view of a diamond multilayer composite self-supporting film.
Example 3
1) Preparation of SiC-SiO2Composite layer 2
Cleaning the surface of the graphite substrate: taking a graphite matrix 1 with the diameter of 60mm and the thickness of 5mm as a substrate, putting the substrate into absolute ethyl alcohol for ultrasonic cleaning for 10min, and drying the substrate by hot air;
putting the cleaned graphite substrate 1 into a titanium mold 4 with the outer diameter of 65mm, the height of 10mm, the diameter of a groove of 60.1mm and the depth of 5.1mm, then putting the graphite substrate in the central position of a base table in a reaction cavity of a microwave plasma assisted chemical vapor deposition experimental device, closing the cavity and vacuumizing;
pumping the vacuum degree of the cavity to 9 × 10-4After Pa is less, H is introduced2The flow is controlled to be 1000sccm, the microwave power is set to be 5kW when the air pressure of the cavity is increased to 20kPa,starting a microwave power supply, exciting microwave plasma, and introducing TMS and O2Controlling the flow rate to be 5sccm, simultaneously increasing the air pressure and the power, and stabilizing the parameters when the temperature of the substrate is increased to 1200 DEG C2Depositing a composite layer for 10min to obtain SiC-SiO with the thickness of about 20 mu m2And (6) a composite layer 2.
As shown in FIG. 1, the preparation of SiC-SiO on the surface of graphite is shown2Schematic cross-sectional view of the composite layer 2.
2) Preparation of the Diamond film 3
SiC-SiO2After the preparation of the composite layer 2 is finished, CH is slowly introduced into the experimental device4Increase CH4And H2Gradually stopping introducing O at the same time of the flow2And TMS, control H2The flow rate is 200sccm and CH4The flow rate is 40sccm, the gas pressure is kept at about 5kPa, the deposition of the diamond film 3 is carried out when the temperature of the substrate is raised to 1250 ℃ and the parameters are stabilized, the time is controlled to be 100h, and the thickness of the diamond film 3 is ensured to be 10 +/-5 mu m.
As shown in FIG. 2, it is shown in SiC-SiO2The composite layer 2 has a schematic cross-sectional view of the diamond film 3 deposited on the surface.
3) Preparation of SiC-SiO again2 Layer 2
After the deposition of the diamond film 3 is finished, TMS and O are slowly introduced2And gradually stop the introduction of CH4TMS and oxygen flow are controlled to be 5sccm and H2Adjusting the flow rate to 200sccm, adjusting the gas pressure and power to maintain the substrate temperature at 1200 deg.C, stabilizing the parameters, and performing SiC-SiO2Depositing the composite layer 2 for 10min to obtain SiC-SiO with thickness of about 1 μm2Layer 2.
4）SiC-SiO2Diamond multilayer composite film
Repeating the steps 2) and 3) to prepare SiC-SiO2A diamond multilayer composite film having a total film thickness of 5mm and a diamond film 3 as the uppermost layer, wherein a titanium mold 4 is replaced according to the film thickness to form a SiC-SiO2The upper surface of the diamond multilayer composite film is lower than the height of a lug boss at the edge of the titanium mold 4, and CH is stopped to be introduced after the deposition of the diamond film 3 is finished4Gradually decrease the microwave powerThe pressure of a cavity of the rate meter is 5kW and 1kPa, the microwave power supply is closed, and the introduction of H is stopped2And closing the vacuum system and taking out the graphite sample containing the composite membrane.
As shown in FIG. 3, it represents SiC-SiO2Schematic cross-sectional view of the diamond multilayer composite film after preparation.
5) Preparation of outermost layer of SiC-SiO2Composite layer
Will contain SiC-SiO2Placing the graphite substrate 1 of the diamond composite layer into a titanium die 4 with the groove depth of 5mm to ensure that the upper surface of the graphite substrate 1 is higher than the height of a lug boss at the edge of the titanium die 4, then placing the graphite substrate at the central position of a reaction cavity base station, and vacuumizing the furnace to 9 × 10-4After Pa is less, the silicon carbide powder contains SiC-SiO2SiC-SiO is carried out on the upper surface and the side surface of the graphite matrix 1 of the diamond film exposed in the plasma2The preparation 1 of the composite layer 2 has the same technological parameters as the step 1).
As shown in FIG. 4, SiC-SiO as the outermost layer2SiC-SiO after the preparation of the composite layer is finished2Schematic cross-sectional view of a diamond multilayer composite membrane.
6) Removal of graphite matrix
The sample was placed upside down in a titanium mold 4 having a groove depth of 5.2mm to make the multilayer SiC-SiO2The diamond multilayer composite film is contained in the groove of the titanium mold 4, the graphite matrix 1 is exposed outside, the graphite matrix 1 is oxidized and removed, and finally the outermost layer is SiC-SiO2A multilayer composite self-supporting film of composite layers.
As shown in FIG. 5, SiC-SiO obtained after removal of the graphite matrix is shown2Schematic cross-sectional view of a diamond multilayer composite self-supporting film.
The technical solutions in the embodiments of the present invention are clearly and completely described above, and the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (7)

1. A kind ofThe silicon carbide-silicon dioxide/diamond multilayer composite self-supporting film is characterized in that: from SiC-SiO2The composite layers and the diamond films are sequentially and alternately superposed, and the upper surface, the lower surface and the side surfaces of the composite layers are SiC-SiO2 composite layers.
2. The silicon carbide-silica/diamond multilayer composite self-supporting film according to claim 1, wherein: SiC-SiO2The composite layer and the diamond film are prepared by adopting a plasma-assisted chemical vapor deposition method.
3. The silicon carbide-silica/diamond multilayer composite self-supporting film according to claim 2, wherein: SiC-SiO2The thickness of the composite layer is 0.1-20 μm, and the thickness of the diamond film is 10-100 μm.
4. A method for producing a silicon carbide-silica/diamond multilayer composite self-supporting film according to any one of claims 1 to 3, comprising the steps of:
1) preparing SiC and SiO on the surface of the graphite matrix by adopting a plasma-assisted chemical vapor deposition method and taking mixed gas containing silicon-carbon gas, hydrogen and oxygen as reaction gas2Phase SiC-SiO2Compounding layers;
2) introducing methane, and increasing the flow of methane while decreasing the flow of oxygen and the flow of a gas containing silicon and carbon in SiC-SiO2Depositing a diamond film on the composite layer;
3) repeated preparation of SiC-SiO2The operation processes of compounding layers and depositing diamond films are sequentially and alternately carried out, and finally SiC-SiO with the thickness of 0.2-5mm is formed on the graphite substrate2A diamond multilayer composite layer;
4) repeating the step 1) on the SiC-SiO2Preparing a layer of SiC-SiO on the upper surface and the side surface of the diamond multilayer composite layer2Compounding layers;
5) inverting the test piece to expose the graphite matrix in oxygen atmosphere, oxidizing and removing the graphite matrix to obtain the complete high-transmittance antioxidant SiC-SiO2The diamond multilayer composite self-supporting film.
5. The method for producing a silicon carbide-silica/diamond multilayer composite self-supporting film according to claim 4, characterized in that:
SiC-SiO2the preparation method of the composite layer comprises respectively ultrasonic cleaning graphite with deionized water and anhydrous ethanol, hot air drying, placing cleaned graphite in a titanium mold with a groove, wherein the height of the upper surface of the graphite is 0-3mm lower than that of a boss at the edge of the titanium mold, placing the graphite and the titanium mold into a microwave plasma assisted chemical vapor deposition experimental device, and vacuumizing to 9 × 10 in a furnace-4Introducing silicon-carbon-containing gas, hydrogen and oxygen as reaction gases after the pressure is less than Pa, and preparing SiC-SiO on the surface of the graphite matrix2Compounding layers; wherein the technological parameters are as follows: the temperature of the graphite substrate is 750-1200 ℃, the hydrogen flow is 200-1000sccm, the silicon-carbon-containing gas accounts for 0.1-10% of the volume of the hydrogen, the oxygen accounts for 0.1-10% of the volume of the hydrogen, the gas pressure is 2-20kPa, the power is 1-10kW, and the deposition time is 10min-5 h;
the specific preparation method of the diamond film comprises the following steps: SiC-SiO2After the preparation of the composite layer is finished, introducing methane into the experimental device, gradually stopping introducing oxygen and silicon-carbon-containing gas while increasing the flow of methane, controlling the flow of hydrogen to be 1000sccm, controlling the volume percentage of methane to be 1-10% of hydrogen, controlling the gas pressure to be 5-30 kPa, controlling the power to be 1-10kW, controlling the temperature of the base material to be 800-1250 ℃ during deposition, and controlling the deposition time to be 2-100 h;
outermost layer of SiC-SiO2The specific preparation method of the composite layer comprises the following steps: after the final layer of diamond film is deposited, the titanium mold is replaced to make the upper surface of the graphite substrate higher than the height of the lug boss at the edge of the titanium mold, and then the graphite substrate is placed in a microwave plasma-assisted chemical vapor deposition experimental device to prepare SiC-SiO2Exposing the diamond multilayer composite layer in plasma, and performing SiC-SiO on the upper surface and the side surface of the diamond multilayer composite layer2Preparing a composite layer, wherein the process parameters are as follows: the temperature of the graphite substrate is 850-1200 ℃, the hydrogen flow is 200-1000sccm, the silicon-carbon-containing gas accounts for 0.1-10% of the volume of the hydrogen, and the oxygenThe volume percentage of the gas in the hydrogen is 0.1-10%, the gas pressure is 2-20kPa, the power is 1-10kW, and the deposition time is 10min-5 h.
6. The method for producing a silicon carbide-silica/diamond multilayer composite self-supporting film according to claim 4, characterized in that: the method for removing the graphite matrix by oxidation is a thermal oxidation or microwave plasma oxidation method.
7. The method for producing a silicon carbide-silica/diamond multilayer composite self-supporting film according to claim 4, characterized in that: the silicon-carbon containing gas is tetramethylsilane (Si (CH)3)4TMS), trichloromethylsilane (CH)3SiCl3) Or tetraethoxysilane (Si (OC)2H5)4）。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114318287A (en) * 2021-12-23 2022-04-12 深圳技术大学 Preparation method of diamond self-supporting film and diamond self-supporting film
CN114834105A (en) * 2022-04-28 2022-08-02 太原理工大学 High-thermal-conductivity diamond carbon fiber composite material and preparation method thereof

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5527559A (en) * 1994-07-18 1996-06-18 Saint Gobain/Norton Industrial Ceramics Corp. Method of depositing a diamond film on a graphite substrate
US5654044A (en) * 1995-08-29 1997-08-05 The United States Of America As Represented By The Secretary Of The Navy Diamond film deposition on graphite
US5674572A (en) * 1993-05-21 1997-10-07 Trustees Of Boston University Enhanced adherence of diamond coatings employing pretreatment process
US5705262A (en) * 1993-11-12 1998-01-06 Le Carbone Lorraine Surface treatment of carbonaceous material for making a subsequent deposit of diamond adherent and diamond-covered pieces obtained
JPH1053871A (en) * 1996-08-06 1998-02-24 Toyo Tanso Kk Diamond-coated carbon member
US20150218694A1 (en) * 2014-01-24 2015-08-06 Ii-Vi Incorporated Substrate Including a Diamond Layer and a Composite Layer of Diamond and Silicon Carbide, and, Optionally, Silicon
CN105039928A (en) * 2015-06-17 2015-11-11 姜辛 Preparation method of diamond/silicon carbide three-dimensional composite structure and prepared product
CN106835064A (en) * 2016-12-16 2017-06-13 中国科学院深圳先进技术研究院 A kind of instrument with diamond/silicon carbide composite coating and preparation method thereof
CN110565065A (en) * 2018-06-06 2019-12-13 深圳先进技术研究院 Silicon carbide-nano diamond composite coating, preparation method and application thereof, cold extrusion die male die and die
CN111593322A (en) * 2020-06-18 2020-08-28 太原理工大学 Silica-diamond composite material and method for producing same

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5674572A (en) * 1993-05-21 1997-10-07 Trustees Of Boston University Enhanced adherence of diamond coatings employing pretreatment process
US5705262A (en) * 1993-11-12 1998-01-06 Le Carbone Lorraine Surface treatment of carbonaceous material for making a subsequent deposit of diamond adherent and diamond-covered pieces obtained
US5527559A (en) * 1994-07-18 1996-06-18 Saint Gobain/Norton Industrial Ceramics Corp. Method of depositing a diamond film on a graphite substrate
US5654044A (en) * 1995-08-29 1997-08-05 The United States Of America As Represented By The Secretary Of The Navy Diamond film deposition on graphite
JPH1053871A (en) * 1996-08-06 1998-02-24 Toyo Tanso Kk Diamond-coated carbon member
US20150218694A1 (en) * 2014-01-24 2015-08-06 Ii-Vi Incorporated Substrate Including a Diamond Layer and a Composite Layer of Diamond and Silicon Carbide, and, Optionally, Silicon
CN105039928A (en) * 2015-06-17 2015-11-11 姜辛 Preparation method of diamond/silicon carbide three-dimensional composite structure and prepared product
CN106835064A (en) * 2016-12-16 2017-06-13 中国科学院深圳先进技术研究院 A kind of instrument with diamond/silicon carbide composite coating and preparation method thereof
CN110565065A (en) * 2018-06-06 2019-12-13 深圳先进技术研究院 Silicon carbide-nano diamond composite coating, preparation method and application thereof, cold extrusion die male die and die
CN111593322A (en) * 2020-06-18 2020-08-28 太原理工大学 Silica-diamond composite material and method for producing same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
梁宝岩等: "热处理在金刚石表面热蒸镀覆SiO2/SiC晶体复合涂层", 《材料热处理学报》 *
郭会斌等: "光学级金刚石自支撑膜及其镀制Y2O3增透膜后的高温抗氧化性", 《材料热处理学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114318287A (en) * 2021-12-23 2022-04-12 深圳技术大学 Preparation method of diamond self-supporting film and diamond self-supporting film
CN114318287B (en) * 2021-12-23 2023-11-03 深圳技术大学 Preparation method of diamond self-supporting film and diamond self-supporting film
CN114834105A (en) * 2022-04-28 2022-08-02 太原理工大学 High-thermal-conductivity diamond carbon fiber composite material and preparation method thereof
CN114834105B (en) * 2022-04-28 2023-06-27 太原理工大学 High-thermal conductivity diamond carbon fiber composite material and preparation method thereof

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