CN112647043A - High-hardness and high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating and preparation method thereof - Google Patents
High-hardness and high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating and preparation method thereof Download PDFInfo
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- CN112647043A CN112647043A CN202011365829.3A CN202011365829A CN112647043A CN 112647043 A CN112647043 A CN 112647043A CN 202011365829 A CN202011365829 A CN 202011365829A CN 112647043 A CN112647043 A CN 112647043A
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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Abstract
The invention belongs to the technical field of surface protection, and particularly relates to a high-hardness and high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating and a preparation method thereof. The carbide coating consists of the following elements in atomic percentage: 15-45% of tantalum, hafnium: 15% -45%, carbon: 40 to 50 percent. The component range with high hardness and high elastic modulus in the tantalum-hafnium-carbon ternary compound system is screened out by a high-throughput experimental method, and the tantalum-hafnium-carbon ternary compound crystalline coating is prepared by adopting a combined magnetron sputtering method. The coating prepared by the method has ultrahigh hardness and elastic modulus, the indentation hardness is more than 25GPa, the elastic modulus is more than 400GPa, and compared with other methods, the preparation method provided by the invention has the characteristics of simple process, no need of ceramic powder precursor and reaction gas, controllable coating components and microstructure, compact coating and the like.
Description
Technical Field
The invention belongs to the technical field of surface protection, and particularly relates to a high-hardness and high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating and a preparation method thereof.
Background
In the ultra-high temperature ceramic material, TaC and HfC which are binary compounds of metal tantalum and hafnium and carbon have extremely high hardness and thermal stability. TaC and HfC have ultrahigh melting points (3890 ℃ and 3928 ℃ respectively), and are two substances with the highest melting points in the binary metal compound. TaC and HfC have high hardness, high elastic modulus, low resistivity (the resistivity is 42.1 mu omega cm at 25 ℃), excellent chemical stability, corrosion resistance, high-temperature strength, high-temperature corrosion resistance, low diffusion coefficient and oxidation resistance at high temperature, and can be used as thermal protection coatings for tool steel, wear-resistant parts, diffusion barriers, hypersonic aircrafts (such as leading edges and nose caps), propulsion parts (such as rocket nozzles), scramjet engine parts, hypersonic reentry aircrafts and other ultrahigh-temperature environments.
TaC and HfC can stably exist in the range of C/Ta or C/Hf ratio of 0.74-1.00, and can contain 0-20% of carbon crystal lattice vacancy without crystal structure change. The crystal structures of TaC and HfC are typical face-centered cubic NaCl crystal structures, and a continuous single-phase cubic Ta-Hf-C solid solution can be theoretically formed. The phase diagram of the Ta-Hf-C system shows complete miscibility over a wide temperature range above 1200K, Ta4HfC5The melting point of the ternary ceramic phase reaches 3990 ℃, is a compound with the highest melting point discovered so far, and becomes a hot spot in the research field of ultra-high temperature heat-proof materials.
At present, the preparation process of Ta-Hf-C ternary ceramic carbide mainly focuses on powder synthesis and block material preparation, such as preparation of ceramic powder by using self-propagating high-temperature synthesis, precursor calcination or carbothermic reduction and the like, preparation of block materials by using hot-pressing sintering or spark plasma sintering and the like, and the preparation process mainly has the defects of complex process flow, high sintering temperature, low densification degree, easy introduction of free carbon impurities, oxide impurities and the like. The preparation process of the Ta-Hf-C ternary ceramic carbide coating mainly comprises methods such as chemical vapor deposition, plasma spraying and the like, wherein the chemical vapor deposition method is low in speed, long in preparation period, complex in process, high in coating stress and easy to crack, and the plasma spraying method has the problems of high requirement on the quality of ceramic powder, low coating density, difficulty in realizing fine regulation and control of components and tissues and the like.
Disclosure of Invention
The invention aims to provide a high-hardness high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating and a preparation method thereof, wherein the coating has ultrahigh hardness and elastic modulus, and extremely high thermal stability, and can be used for surface thermal protection in various ultrahigh-temperature environments; the preparation method has the advantages of simple process, good repeatability, no need of ceramic powder precursor and reaction gas, uniform and controllable coating components and organization structure, good coating compactness, high binding force with a substrate and good application prospect.
The technical scheme of the invention is as follows:
a high-hardness high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating is characterized in that the carbide coating is a completely-miscible single-phase face-centered cubic solid solution, and the thickness of the carbide coating ranges from 0.1 to 10 micrometers; the atomic percentages of Ta, Hf and C are: 15-45% of tantalum, 15-45% of hafnium and 40-50% of carbon; the concentration range of carbon vacancies in the ternary carbide calculated according to the stoichiometric ratio is 0-10% in atomic percentage; based on nano indentation measurement, the hardness of the carbide coating is more than 25GPa, and the elastic modulus is more than 400 GPa.
The high-hardness high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating is a mixture of TaC and HfC, wherein a single-phase face-centered cubic structure solid solution is adopted.
Preferably, the high-hardness high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating comprises the following components in percentage by atom: 22 to 45 percent of tantalum, 15 to 31 percent of hafnium and 40 to 50 percent of carbon; the concentration of carbon vacancies in the ternary carbide ranges in atomic percent < 5% calculated as a stoichiometric ratio.
The high-hardness high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating is prepared on the surface of a substrate of a silicon wafer, aluminum oxide, a carbon/carbon composite material, stainless steel or a high-temperature alloy.
A preparation method of a high-hardness high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating adopts multi-target co-sputtering of three pure element targets of tantalum, hafnium and carbon: firstly, cleaning and drying the substrate in ethanol or acetone, placing the substrate on a sample table in a vacuum cavity, and pumping the vacuum degree of the back to 5 multiplied by 10-5Below Pa; then introducing high-purity argon with the purity of 99.999 percent into the vacuum chamber to ensure that the air pressure is between 0.2 and 1 Pa, and enabling the sample to be subjected to vacuum evaporationHeating to 400-800 ℃ and keeping for 20-40 minutes to make the surface temperature of the sample uniform; and then respectively applying 200-1000V direct current negative bias on the magnetron sputtering target to enable the target to be in an arc state, starting deposition after sputtering and cleaning for 5-20 minutes, wherein in the deposition process, the potential of the sample table is grounded or 50-100V direct current negative bias is applied, the sample table rotates at the speed of 0-20 revolutions per minute, and the deposition time is 20-5 hours.
The design idea of the invention is as follows:
the tantalum carbide and the hafnium carbide have the same crystal structure, the chemical bonding of the binary carbides is mainly carried out by the hybridization of Hf (Ta) -5d and C-2p orbitals, a strong covalent bonding effect is formed, the tantalum and hafnium elements are cooperatively introduced to form a continuous ternary carbide solid solution, and the tantalum-hafnium-carbon coating with high hardness and high elastic modulus is obtained under the element cooperation effect.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the tantalum-hafnium-carbon ternary ceramic carbide coating prepared by the method has the advantages of uniform structure, consistent thickness, good coverage and bonding force, high density, ultrahigh hardness and ultrahigh elastic modulus.
2. The invention optimizes the components, structure, thickness and density of the tantalum-hafnium-carbon ternary ceramic carbide coating, so that the coating has more excellent physical and mechanical properties.
3. The tantalum-hafnium-carbon ternary ceramic carbide coating is prepared by adopting a pure element target multi-target co-sputtering method, so that the process conditions are conveniently optimized, the coating can be prepared on the surfaces of various material substrates, precursor powder materials or reaction gases are not needed, the deposition efficiency in the preparation process is high, and the component structure of the coating is controllable.
4. The tantalum-hafnium-carbon ternary ceramic carbide coating and the preparation method thereof can change the components and the structure of the coating by optimizing the design and adjusting the preparation process, and control the mechanical properties such as hardness, elastic modulus and the like, and the physical properties such as melting point, thermal expansion coefficient and the like, thereby realizing good combination and matching with substrates made of different materials and achieving the effect of protecting the ultrahigh-temperature surface.
Drawings
FIG. 1 is (Ta) prepared by an example of the present invention0.66Hf0.34) XRD diffraction pattern of C ternary ceramic carbide coating phase composition. In the figure, the abscissa 2 θ represents the diffraction angle (degrees), and the ordinate Intensity represents the relative Intensity (arb. units).
FIG. 2 is a graph of the change in the values of hardness (a) and elastic modulus (b) measured by nanoindentation of coating samples prepared in accordance with an example of the present invention over a range of compositions.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples. The purity of the target material used in the following examples is more than or equal to 99.9 wt%, the volume purity of high-purity argon gas is more than or equal to 99.999%, and the component representation modes are all atomic percent.
Example 1:
in this example, the nominal composition of the tantalum-hafnium-carbon ternary ceramic carbide coating is (Ta)0.66Hf0.34)C：
The method adopts targets of three pure elements (purity 99.9%) of tantalum, hafnium and carbon for multi-target co-sputtering: firstly, cleaning and drying an alumina substrate in ethanol, placing the alumina substrate on a sample table which is provided with a resistance heating device and a baffle in a vacuum cavity, and pumping the vacuum degree of the back substrate to 3 multiplied by 10-5Handkerchief; then introducing high-purity argon with the purity of 99.999 percent into the vacuum chamber to ensure that the air pressure reaches 0.4 Pa, heating the sample to 400 ℃ and keeping the temperature for 30 minutes to ensure that the surface temperature of the sample is uniform; and then applying 300 volt, 240 volt and 400 volt direct current negative bias on the tantalum, hafnium and carbon magnetron sputtering targets respectively to start the targets to be arc, removing a baffle of a sample table to start deposition after sputtering and cleaning for 10 minutes, grounding the potential of the sample table in the deposition process, and rotating the sample table at the speed of 20 revolutions per minute. After 3 hours of deposition (Ta) with a thickness of 2 μm was obtained0.66Hf0.34) C coating, the X-ray diffraction result proves that the coating is a single-phase solid solution, the nano-indentation measured hardness is 30GPa, and the elastic modulus is 460 GPa.
In this example, the atomic percentages of Ta, Hf, and C are: tantalum 33%, hafnium 17%, carbon 50%; the concentration of carbon vacancies in the ternary carbide is less than 3 atomic percent, calculated as the stoichiometric ratio.
Example 2:
in this example, the nominal composition of the tantalum-hafnium-carbon ternary ceramic carbide coating is (Ta)0.5Hf0.5)C：
The method adopts targets of three pure elements (purity 99.9%) of tantalum, hafnium and carbon for multi-target co-sputtering: firstly, cleaning and drying an alumina substrate in acetone, placing the alumina substrate on a sample table which is provided with a resistance heating device and a baffle in a vacuum cavity, and pumping the vacuum degree of the back substrate to 4 multiplied by 10-5Handkerchief; then introducing high-purity argon with the purity of 99.999 percent into the vacuum chamber to ensure that the air pressure reaches 0.4 Pa, heating the sample to 550 ℃ and keeping the temperature for 30 minutes to ensure that the surface temperature of the sample is uniform; and then applying 200V, 240V and 400V direct current negative bias voltage on the tantalum, hafnium and carbon magnetron sputtering targets respectively to start the targets to be arc, removing a baffle of a sample table to start deposition after sputtering and cleaning for 10 minutes, grounding the potential of the sample table in the deposition process, and rotating the sample table at the speed of 20 revolutions per minute. After 3 hours of deposition (Ta) with a thickness of 2 μm was obtained0.5Hf0.5) C coating, the X-ray diffraction result proves that the coating is a single-phase solid solution, the nano-indentation measured hardness is 32GPa, and the elastic modulus is 515 GPa.
In this example, the atomic percentages of Ta, Hf, and C are: 25% of tantalum, 25% of hafnium and 50% of carbon; the concentration of carbon vacancies in the ternary carbide is less than 3 atomic percent, calculated as the stoichiometric ratio.
Example 3:
in this example, the nominal composition of the tantalum-hafnium-carbon ternary ceramic carbide coating is (Ta)0.40Hf0.60)C：
The method adopts targets of three pure elements (purity 99.9%) of tantalum, hafnium and carbon for multi-target co-sputtering: firstly, the alumina substrate is cleaned and dried in ethanol, and is placed on a sample table with a resistance heating device and a baffle plate in a vacuum cavity, and the vacuum degree of the back substrate is pumped to 5 multiplied by 10-5Handkerchief; then introducing high-purity argon with the purity of 99.999 percent into the vacuum chamber to ensure that the air pressure reaches 0.4 Pa, heating the sample to 700 ℃ and keeping the temperature for 30 minutes to ensure that the surface temperature of the sample is uniform; then, 300V, 240V and 400V DC negative voltages are respectively applied on the tantalum, hafnium and carbon magnetron sputtering targetsAnd (3) biasing to enable the target to be in arc striking, removing the baffle of the sample table to start deposition after sputtering and cleaning for 10 minutes, grounding the potential of the sample table in the deposition process, and rotating the sample table at the speed of 20 revolutions per minute. After 3 hours of deposition (Ta) with a thickness of 2 μm was obtained0.40Hf0.60) C coating, the X-ray diffraction result proves that the coating is a single-phase solid solution, the nano-indentation measured hardness is 28GPa, and the elastic modulus is 490 GPa.
In this example, the atomic percentages of Ta, Hf, and C are: 20% of tantalum, 30% of hafnium and 50% of carbon; the concentration of carbon vacancies in the ternary carbide is less than 3 atomic percent calculated as the stoichiometric ratio.
(Ta) prepared in the examples of the present invention, as shown in FIG. 10.66Hf0.34) XRD diffraction pattern of C ternary ceramic carbide coating phase composition, only able from FIG. 1 (Ta)0.66Hf0.34) The (111) and (222) peaks of C, indicating that crystalline coatings can be obtained at this deposition temperature; only (Ta) is detected in FIG. 10.66Hf0.34) And C, a diffraction peak indicates that the obtained coating forms a single-phase solid solution structure.
As shown in fig. 2, the nano-indentation measured Hardness (Hardness) and Modulus of elasticity (Modulus) of the coating samples prepared according to the example of the present invention are plotted against the change in the composition, as shown in fig. 2, the atomic percent range of the composition of the samples in this experiment covers: 22-45% of tantalum, 15-31% of hafnium and 40-50% of carbon, wherein the component span of adjacent sample units is less than 1 mol.%, the hardness range is 28.5-32 GPa, and the elastic modulus range is 394.5-530 GPa.
The embodiment result shows that the component ranges with high hardness and high elastic modulus in the tantalum-hafnium-carbon ternary compound system are screened out by a high-throughput experimental method, and the tantalum-hafnium-carbon ternary compound crystalline coating is prepared by adopting a combined magnetron sputtering method. The coating prepared by the method is characterized in that: the preparation method has the characteristics of simple process, no need of ceramic powder precursors and reaction gases, controllable coating components and microstructure, compact coating and the like.
Claims (5)
1. The high-hardness high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating is characterized in that the carbide coating is a completely-miscible single-phase face-centered cubic solid solution, and the thickness of the carbide coating ranges from 0.1 to 10 micrometers; the atomic percentages of Ta, Hf and C are: 15-45% of tantalum, 15-45% of hafnium and 40-50% of carbon; the concentration range of carbon vacancies in the ternary carbide calculated according to the stoichiometric ratio is 0-10% in atomic percentage; based on nano indentation measurement, the hardness of the carbide coating is more than 25GPa, and the elastic modulus is more than 400 GPa.
2. The high hardness high modulus tantalum hafnium carbon ternary ceramic carbide coating of claim 1, wherein the single phase face centered cubic solid solution is a mixture of TaC and HfC.
3. The high hardness high modulus tantalum hafnium carbon ternary ceramic carbide coating of claim 1, wherein preferably the atomic percentages of Ta, Hf and C are: 22 to 45 percent of tantalum, 15 to 31 percent of hafnium and 40 to 50 percent of carbon; the concentration of carbon vacancies in the ternary carbide ranges in atomic percent < 5% calculated as a stoichiometric ratio.
4. The high hardness and high modulus tantalum hafnium carbon ternary ceramic carbide coating of claim 1, wherein the carbide coating is prepared on the surface of a substrate made of silicon wafer, alumina, carbon/carbon composite, stainless steel or high temperature alloy.
5. The preparation method of the high-hardness high-modulus tantalum-hafnium-carbon ternary ceramic carbide coating according to any one of claims 1 to 4, characterized by adopting multi-target co-sputtering of three pure-element targets of tantalum, hafnium and carbon: firstly, cleaning and drying the substrate in ethanol or acetone, placing the substrate on a sample table in a vacuum cavity, and pumping the vacuum degree of the back to 5 multiplied by 10-5Below Pa; then introducing high-purity argon with the purity of 99.999 percent into the vacuum chamber to ensure that the air pressure is between 0.2 and 1 Pa, and heating the sampleKeeping the temperature to 400-800 ℃ for 20-40 minutes to make the surface temperature of the sample uniform; and then respectively applying 200-1000V direct current negative bias on the magnetron sputtering target to enable the target to be in an arc state, starting deposition after sputtering and cleaning for 5-20 minutes, wherein in the deposition process, the potential of the sample table is grounded or 50-100V direct current negative bias is applied, the sample table rotates at the speed of 0-20 revolutions per minute, and the deposition time is 20-5 hours.
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| LUIS YATE.ET.AL.: "Robust tribo-mechanical and hot corrosion resistance of ultrarefractory Ta-Hf-C ternary alloy films", 《SCIENTIFIC REPORTS》 * |
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