CN110541152B - Tantalum/steel bimetal composite material and preparation method thereof - Google Patents

Tantalum/steel bimetal composite material and preparation method thereof Download PDF

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CN110541152B
CN110541152B CN201910912105.7A CN201910912105A CN110541152B CN 110541152 B CN110541152 B CN 110541152B CN 201910912105 A CN201910912105 A CN 201910912105A CN 110541152 B CN110541152 B CN 110541152B
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tantalum
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magnetron sputtering
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钟黎声
白海强
魏俊哲
许云华
彭建洪
朱建雷
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Xian 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
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

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Abstract

The invention discloses a tantalum/steel bimetal composite material which comprises a steel matrix and a tantalum coating on the surface of the steel matrix, wherein tantalum carbide particles are distributed between the steel matrix and the tantalum coating, the carbon content in the steel matrix is 0.5-1.0 wt%, and the thickness of the tantalum coating is 20-60 mu m. The invention also discloses a preparation method of the tantalum/steel bimetal composite material, which is characterized in that the tantalum/steel bimetal composite material is prepared by adopting a steel matrix with higher carbon content, tantalum and the steel matrix are compounded together through vacuum magnetron sputtering, and then the tantalum/steel composite material is subjected to composite annealing treatment of 'electric field + temperature field' at 780-820 ℃, so that residual stress generated in the deposition process of a Ta coating can be effectively eliminated, diffusion of C atoms in the steel matrix is accelerated, in-situ formation of a TaC pinning phase is promoted, the interface performance is improved, and the interface bonding strength is effectively improved.

Description

Tantalum/steel bimetal composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of bimetal composite materials, and relates to a tantalum/steel bimetal composite material and a preparation method thereof.
Background
Tantalum is a silvery-white rare high-melting-point metal, and has good ductility, stable chemical properties and strong corrosion resistance. Tantalum exists in two crystal forms, namely a body-centered cubic alpha phase and a tetragonal beta phase (metastable phase, beta-Ta → alpha-Ta phase transition occurs above 750 ℃). The alpha-Ta has better plastic toughness, good matching property with steel, good coating binding property and difficult peeling; and the beta-Ta is hard and brittle, has poor thermal stability and almost no practical application value, and can be converted into the alpha-Ta within the range of 750-1000 ℃. Although metallic tantalum has a number of excellent properties, it is relatively expensive to obtain a single component tantalum metal, due to its low natural resources and often its co-existence with metallic niobium in niobium tantalite, which limits its wide application.
In order to expand the application range of tantalum, some people compound tantalum and steel to form a tantalum steel composite material. For example, in chinese patent CN109048216A, a tantalum plate and a stainless steel plate are combined together by an explosive welding composite method to form a tantalum steel composite plate. In the technical report "characteristics of tantalum liners applied to 25-mm and 120-mm cannon bore sections via applied bonding" published by Vigilance et al of army research and development and engineering center 2001, army Bernit laboratory, USA, pure tantalum burning-resistant layers are prepared in bore of bore gun barrel by using explosive spraying technology, and analysis shows that the bonding between tantalum layer and steel matrix metal is good, but adiabatic shear bands appear in steel matrix and form Ta-Fe brittle intermetallic compound phase, thereby reducing the strength of bore gun barrel. Guo-Ji-an et al in 2018 published in the paper frictional wear performance of magnetron sputtering Ta coating on CrNi3MoVA steel surface in the research article B of Material guide, successfully deposited Ta coating on CrNi3MoVA steel surface by using magnetron sputtering technology, wherein the deposited Ta coating consists of alpha-Ta and metastable tetragonal phase beta-Ta, and is completely converted into alpha-Ta phase after vacuum annealing for 3h at 850 ℃, but simultaneously a large amount of TaFe and Ta are formed at the interface of the Ta coating and a substrate2A Fe metal compound.
The above contents indicate that the tantalum/steel bimetal composite material prepared by the prior art has the following problems:
(1) the problems of pollution, danger and the like exist in the preparation of the tantalum/steel bimetal composite material by explosion cladding, and particularly TaFe and Ta can be formed at a high-temperature interface during explosion2Intermetallic compounds such as Fe have low bonding strength;
(2) for the magnetron sputtering composite preparation of the tantalum/steel bimetal composite material, TaFe and Ta are used at the tantalum/steel interface2Fe and other intermetallic compounds are used as main components, and the carbon content of the steel matrix is limited to 0.35-0.5 percent, which is not beneficial to improving the overall strength of the material.
Disclosure of Invention
The invention aims to provide a tantalum/steel bimetal composite material, which solves the problems of low bonding strength and low overall strength of the existing tantalum/steel bimetal composite material.
Another object of the present invention is to provide a method for preparing a tantalum/steel bimetal composite material.
The first technical scheme adopted by the invention is that the tantalum/steel bimetal composite material comprises a steel substrate and a tantalum coating on the surface of the steel substrate, tantalum carbide particles are distributed between the steel substrate and the tantalum coating, the carbon content in the steel substrate is 0.5-1.0 wt%, and the thickness of the tantalum coating is 20-60 mu m.
The second technical scheme adopted by the invention is that the preparation method of the tantalum/steel bimetal composite material comprises the following steps:
step 1: preparing a steel matrix and a tantalum target material, wherein the carbon content of the steel matrix is 0.5-1.0 wt%, and the tantalum content Ta of the tantalum target material is more than or equal to 99.99 wt%;
step 2: carrying out grinding and polishing treatment on the surface of a steel matrix, and then cleaning and blow-drying;
and step 3: sputtering a tantalum target material on the surface of a steel substrate by adopting vacuum magnetron sputtering equipment to prepare a tantalum steel composite material;
and 4, step 4: and (3) placing the tantalum steel composite material in an electric field and a temperature field for composite annealing treatment to obtain the tantalum/steel bimetal composite material.
The invention is also characterized in that:
the steel substrate is alloy steel, carbon steel or tool steel.
And 2, polishing the surface of the steel matrix to ensure that the roughness of the surface of the steel matrix is 0.01-0.04 mu m, and then putting the steel matrix into ethanol for ultrasonic cleaning.
The specific process of the step 3 is as follows:
step 3.1: fixing a steel substrate on a sputtering platform of vacuum magnetron sputtering equipment, then placing a tantalum target material into a magnetron sputtering chamber, ensuring that the distance between the surface of the steel substrate and the tantalum target material is 50-70 mm, and closing the magnetron sputtering chamber;
step 3.2: vacuumizing the magnetron sputtering chamber to make the vacuum degree in the magnetron sputtering chamber be 6 x 10-5Pa～2×10-4Pa, introducing argon into the magnetron sputtering chamber, starting a bias power supply when the air pressure in the magnetron sputtering chamber is 0.7-1.2 Pa, and sputtering and cleaning the steel substrate for 10-20 min to complete the preparation work before coating;
step 3.3: and adjusting the air pressure in the magnetron sputtering chamber to 0.25-0.6 Pa, starting magnetron sputtering for 2-6 h, and preparing the tantalum steel composite material after magnetron sputtering.
The sputtering power of magnetron sputtering is 30-60W, the direct current bias power supply is negative bias of-80-200V, and the sputtering power density is 2.5W/cm2～8W/cm2And the temperature of the steel matrix layer is 200-400 ℃.
The specific process of the step 4 is as follows:
step 4.1: fixing the tantalum steel composite material between an upper red copper electrode and a lower red copper electrode in a composite annealing treatment furnace, applying an external power supply to the two red copper electrodes, and enabling a steel matrix to be close to the negative electrode of the external power supply so that the current flowing through the tantalum steel composite material is 50-400A;
step 4.2: and heating and annealing the tantalum steel composite material at 780-820 ℃ for 2-6 h to obtain the tantalum/steel bimetal composite material.
The external power supply is RDY 2000A/12V direct current power supply.
The composite annealing treatment is carried out in an argon atmosphere.
The method has the beneficial effects that the tantalum/steel bimetal composite material is prepared by adopting the steel matrix with higher carbon content (0.5-1.0 wt%), so that the in-situ formation of a TaC pinning phase is promoted, and the strength of the tantalum/steel bimetal composite material is improved; tantalum and a steel matrix are compounded together through vacuum magnetron sputtering to prepare a tantalum steel composite material, the tantalum steel composite material is subjected to composite annealing treatment of 'electric field + temperature field' at 780-820 ℃, so that residual stress generated in the deposition process of a Ta coating can be effectively eliminated, diffusion of C atoms in the steel matrix is accelerated, in-situ formation of a TaC pinning phase is promoted, and TaFe and Ta at an interface are reduced2The content of intermetallic compounds such as Fe and the like,the interface performance is improved, and the interface bonding strength is effectively improved.
Drawings
FIG. 1 is a schematic structural view of a tantalum/steel bi-metal composite of the present invention;
FIG. 2 is a schematic view of the annealing process in the method for preparing the tantalum/steel bimetal composite material according to the present invention.
In the figure, 1, a steel substrate, 2, a tantalum coating, 3, tantalum carbide particles, 4, a red copper electrode and 5, an external power supply are arranged.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a tantalum/steel bimetal composite material, which comprises a steel substrate 1 and a tantalum coating 2 on the surface of the steel substrate 1, wherein tantalum carbide particles 3 are distributed between the steel substrate 1 and the tantalum coating 2, the carbon content in the steel substrate is 0.5-1.0 wt%, and the thickness of the tantalum coating is 20-60 mu m.
The invention relates to a preparation method of a tantalum/steel bimetal composite material, which comprises the following steps:
step 1: preparing a steel matrix and a tantalum target material, wherein the carbon content of the steel matrix is 0.5-1.0 wt%, and the tantalum content Ta of the tantalum target material is more than or equal to 99.99 wt%; the steel substrate is alloy steel, carbon steel or tool steel.
Step 2: polishing the surface of the steel matrix to ensure that the roughness of the surface of the steel matrix is 0.01-0.04 mu m, putting the steel matrix into ethanol for ultrasonic cleaning, and then cleaning and blow-drying;
and step 3: sputtering a tantalum target material on the surface of a steel substrate by adopting vacuum magnetron sputtering equipment to prepare a tantalum steel composite material;
the specific process of the step 3 is as follows:
step 3.1: fixing a steel substrate on a sputtering platform of vacuum magnetron sputtering equipment, then placing a tantalum target material into a magnetron sputtering chamber, ensuring that the distance between the surface of the steel substrate and the tantalum target material is 50-70 mm, and closing the magnetron sputtering chamber;
step 3.2: vacuumizing the magnetron sputtering chamber to make the vacuum degree in the magnetron sputtering chamber be 6 x 10-5Pa～2×10-4Pa, introducing argon into the magnetron sputtering chamber, starting a bias power supply when the air pressure in the magnetron sputtering chamber is 0.7-1.2 Pa, and sputtering and cleaning the steel substrate for 10-20 min to complete the preparation work before coating;
step 3.3: adjusting the air pressure in the magnetron sputtering chamber to 0.25-0.6 Pa, starting magnetron sputtering for 2-6 h, wherein the sputtering power of magnetron sputtering is 30-60W, the direct-current bias power supply is negative bias voltage of-80-200V, and the sputtering power density is 2.5W/cm2～8W/cm2And controlling the temperature of the steel substrate layer to be 200-400 ℃, and preparing the tantalum steel composite material after magnetron sputtering.
And 4, step 4: placing the tantalum steel composite material in an electric field and a temperature field for composite annealing treatment to obtain a tantalum/steel bimetal composite material;
the specific process of the step 4 is as follows:
step 4.1: referring to fig. 2, the tantalum steel composite material is fixed between an upper red copper electrode 4 and a lower red copper electrode 4 in a composite annealing treatment furnace, an external power supply 5 is applied to the two red copper electrodes 4, the external power supply 5 is an RDY 2000A/12V direct current power supply, and a steel substrate 1 is close to the negative electrode of the external power supply, so that the current flowing through the tantalum steel composite material is 50A-400A;
step 4.2: and (2) heating and annealing the tantalum steel composite material at 780-820 ℃ for 2-6 h, and carrying out composite annealing treatment in an argon atmosphere to obtain the tantalum/steel bimetal composite material, wherein tantalum carbide particles are distributed between a steel matrix and a tantalum coating of the composite material.
Example 1
The method for preparing the tantalum/steel bimetal composite material by adopting 55CrNi2MoV alloy steel comprises the following steps:
step 1: preparing a steel matrix and a tantalum target material, wherein the steel matrix is 55CrNi2MoV alloy steel, and the carbon content is 0.5 wt%; the tantalum content Ta of the tantalum target material is more than or equal to 99.99 wt%, the diameter is 40mm, and the thickness is 5.5 mm;
step 2: polishing the surface of the steel matrix to ensure that the roughness of the surface of the steel matrix is 0.02 mu m, putting the steel matrix into ethanol for ultrasonic cleaning, and then cleaning and blow-drying;
and step 3: fixing a steel substrate on a sputtering platform of vacuum magnetron sputtering equipment, then placing a tantalum target material into a magnetron sputtering chamber, ensuring that the distance between the surface of the steel substrate and the tantalum target material is 60mm, and closing the magnetron sputtering chamber;
vacuumizing the magnetron sputtering chamber to make the vacuum degree in the magnetron sputtering chamber be 1 × 10-4Pa, introducing argon into the magnetron sputtering chamber, starting a bias power supply when the air pressure in the magnetron sputtering chamber is 1.0Pa, and sputtering and cleaning the steel substrate for 15min to finish the preparation work before coating;
adjusting the air pressure in the magnetron sputtering chamber to 0.4Pa, starting magnetron sputtering for 4h, wherein the sputtering power of the magnetron sputtering is 45W, the direct-current bias power supply is negative bias-150V, and the sputtering power density is 5W/cm2And the temperature of the steel substrate layer is 300 ℃, and the tantalum steel composite material is prepared after magnetron sputtering.
And 4, step 4: fixing the tantalum steel composite material between an upper red copper electrode and a lower red copper electrode in a composite annealing treatment furnace, applying an external power supply to the two red copper electrodes, wherein the external power supply is a RDY 2000A/12V direct-current power supply, and a steel substrate is close to the negative electrode of the external power supply, so that the current flowing through the tantalum steel composite material is 200A;
the tantalum steel composite material is subjected to heating annealing at the annealing temperature of 800 ℃ for 4h, the annealing treatment is performed in an argon atmosphere, and the composite annealing treatment of the electric field and the temperature field can effectively eliminate residual stress generated in the deposition process of a tantalum coating, accelerate the diffusion of C atoms in a steel matrix, promote the in-situ formation of a TaC pinning phase and improve the interface bonding strength;
and finally, taking out the heat-treated sample, ultrasonically cleaning the sample with ethanol for 2.5min, and drying the sample with an electric blower to obtain the tantalum/steel bimetal composite material.
The tantalum coating thickness in the prepared tantalum/steel bimetal composite material was measured to be about 40 μm, and the physical properties thereof are as described in table 1.
Example 2
The method for preparing the tantalum/steel bimetal composite material by adopting 60 carbon steel comprises the following steps:
step 1: preparing a steel substrate and a tantalum target material, wherein the steel substrate is 60 carbon steel, and the carbon content is 0.65 wt%; the tantalum content Ta of the tantalum target material is more than or equal to 99.99 wt%, the diameter is 30mm, and the thickness is 5 mm;
step 2: polishing the surface of the steel matrix to ensure that the roughness of the surface of the steel matrix is 0.01 mu m, putting the steel matrix into ethanol for ultrasonic cleaning, and then cleaning and blow-drying;
and step 3: fixing a steel substrate on a sputtering platform of vacuum magnetron sputtering equipment, then placing a tantalum target material into a magnetron sputtering chamber, ensuring that the distance between the surface of the steel substrate and the tantalum target material is 50mm, and closing the magnetron sputtering chamber;
vacuumizing the magnetron sputtering chamber to ensure that the vacuum degree in the magnetron sputtering chamber is 2 multiplied by 10-4Pa, introducing argon into the magnetron sputtering chamber, starting a bias power supply when the air pressure in the magnetron sputtering chamber is 0.7Pa, and sputtering and cleaning the steel substrate for 10min to finish the preparation work before coating;
adjusting the air pressure in the magnetron sputtering chamber to 0.25Pa, starting magnetron sputtering for 2h, wherein the sputtering power of the magnetron sputtering is 30W, the direct-current bias power supply is negative bias-80V, and the sputtering power density is 2.5W/cm2And the temperature of the steel substrate layer is 200 ℃, and the tantalum steel composite material is prepared after magnetron sputtering.
And 4, step 4: fixing the tantalum steel composite material between an upper red copper electrode and a lower red copper electrode in a composite annealing treatment furnace, applying an external power supply to the two red copper electrodes, wherein the external power supply is a RDY 2000A/12V direct-current power supply, and a steel matrix layer is close to the negative electrode of the external power supply, so that the current flowing through the tantalum steel composite material is 50A;
the tantalum steel composite material is subjected to heating annealing at 780 ℃, the annealing time is 2 hours, the annealing treatment is performed in an argon atmosphere, and the composite annealing treatment of the electric field and the temperature field can effectively eliminate residual stress generated in the deposition process of a tantalum coating, accelerate the diffusion of C atoms in a steel matrix, promote the in-situ formation of a TaC pinning phase and improve the interface bonding strength;
and finally, taking out the heat-treated sample, ultrasonically cleaning the sample with ethanol for 2.5min, and drying the sample with an electric blower to obtain the tantalum/steel bimetal composite material.
The tantalum coating thickness of the prepared tantalum/steel bimetal composite material was measured to be about 21 μm, and the physical properties thereof are as described in table 1.
Example 3
The method for preparing the tantalum/steel bimetal composite material by using the T7 tool steel comprises the following steps:
step 1: preparing a steel substrate and a tantalum target material, wherein the steel substrate is T7 tool steel, and the carbon content in the steel substrate is 0.7 wt%; the tantalum content Ta of the tantalum target material is more than or equal to 99.99 wt%, the diameter is 50mm, and the thickness is 6 mm;
step 2: polishing the surface of the steel matrix to ensure that the roughness of the surface of the steel matrix is 0.02 mu m, putting the steel matrix into ethanol for ultrasonic cleaning, and then cleaning and blow-drying;
and step 3: fixing a steel substrate on a sputtering platform of vacuum magnetron sputtering equipment, then placing a tantalum target material into a magnetron sputtering chamber, ensuring that the distance between the surface of the steel substrate and the tantalum target material is 70mm, and closing the magnetron sputtering chamber;
vacuumizing the magnetron sputtering chamber to make the vacuum degree in the magnetron sputtering chamber be 6 x 10-5Pa, introducing argon into the magnetron sputtering chamber, starting a bias power supply when the air pressure in the magnetron sputtering chamber is 1.2Pa, and sputtering and cleaning the steel substrate for 20min to finish the preparation work before coating;
adjusting the air pressure in the magnetron sputtering chamber to 0.6Pa, starting magnetron sputtering for 6h with the sputtering power of 60W, the DC bias power supply of minus bias voltage of-200V and the sputtering power density of 8W/cm2And the temperature of the steel substrate layer is 400 ℃, and the tantalum steel composite material is prepared after magnetron sputtering.
And 4, step 4: fixing the tantalum steel composite material between an upper red copper electrode and a lower red copper electrode in a composite annealing treatment furnace, applying an external power supply to the two red copper electrodes, wherein the external power supply is a RDY 2000A/12V direct-current power supply, and a steel matrix layer is close to the negative electrode of the external power supply, so that the current flowing through the tantalum steel composite material is 400A;
the tantalum steel composite material is subjected to heating annealing at 820 ℃ for 6h, the annealing treatment is carried out in an argon atmosphere, and the composite annealing treatment of the electric field and the temperature field can effectively eliminate residual stress generated in the deposition process of a tantalum coating, accelerate the diffusion of C atoms in a steel matrix, promote the in-situ formation of a TaC pinning phase and improve the interface bonding strength;
and finally, taking out the heat-treated sample, ultrasonically cleaning the sample with ethanol for 2.5min, and drying the sample with an electric blower to obtain the tantalum/steel bimetal composite material.
The tantalum coating thickness in the prepared tantalum/steel bimetallic composite was measured to be about 59 μm, and the physical properties are shown in table 1.
Example 4
The method for preparing the tantalum/steel bimetal composite material by adopting 55CrNi2MoV alloy steel comprises the following steps:
step 1: preparing a steel matrix and a tantalum target material, wherein the steel matrix is 55CrNi2MoV alloy steel, and the carbon content is 0.5 wt%; the tantalum content Ta of the tantalum target material is more than or equal to 99.99 wt%, the diameter is 35mm, and the thickness is 5.5 mm;
step 2: polishing the surface of the steel matrix to ensure that the roughness of the surface of the steel matrix is 0.02 mu m, putting the steel matrix into ethanol for ultrasonic cleaning, and then cleaning and blow-drying;
and step 3: fixing a steel substrate on a sputtering platform of vacuum magnetron sputtering equipment, then placing a tantalum target material into a magnetron sputtering chamber, ensuring that the distance between the surface of the steel substrate and the tantalum target material is 55mm, and closing the magnetron sputtering chamber;
vacuumizing the magnetron sputtering chamber to make the vacuum degree in the magnetron sputtering chamber be 1 × 10-4Pa, introducing argon into the magnetron sputtering chamber, starting a bias power supply when the air pressure in the magnetron sputtering chamber is 0.9Pa, and sputtering and cleaning the steel substrate for 12min to finish the preparation work before coating;
adjusting the air pressure in the magnetron sputtering chamber to 0.3Pa, starting magnetron sputtering for 4h, wherein the sputtering power of the magnetron sputtering is 37W, the direct-current bias power supply is negative bias-110V, and the sputtering power density is 3W/cm2And the temperature of the steel substrate layer is 250 ℃, and the tantalum steel composite material is prepared after magnetron sputtering.
And 4, step 4: fixing the tantalum steel composite material between an upper red copper electrode and a lower red copper electrode in a composite annealing treatment furnace, applying an external power supply to the two red copper electrodes, wherein the external power supply is a RDY 2000A/12V direct-current power supply, and a steel matrix layer is close to the negative electrode of the external power supply, so that the current flowing through the tantalum steel composite material is 200A;
the tantalum steel composite material is subjected to heating annealing at the annealing temperature of 790 ℃ for 3h, the annealing treatment is performed in an argon atmosphere, and the composite annealing treatment of the electric field and the temperature field can effectively eliminate residual stress generated in the deposition process of a tantalum coating, accelerate the diffusion of C atoms in a steel matrix, promote the in-situ formation of a TaC pinning phase and improve the interface bonding strength; and (3) taking out the heat-treated sample at the argon flow rate of 8mL/min, ultrasonically cleaning the sample with ethanol for 2.5min, and drying the sample with an electric blower to obtain the tantalum/steel bimetal composite material.
The tantalum coating thickness in the prepared tantalum/steel bimetallic composite was measured to be about 29 μm, and the physical properties are shown in table 1.
Example 5
The method for preparing the tantalum/steel bimetal composite material by using the T7 tool steel comprises the following steps:
step 1: preparing a steel substrate and a tantalum target material, wherein the steel substrate is T7 tool steel, and the carbon content in the steel substrate is 0.7 wt%; the tantalum content Ta of the tantalum target material is more than or equal to 99.99 wt%, the diameter is 45mm, and the thickness is 5.5 mm;
step 2: polishing the surface of the steel matrix to ensure that the roughness of the surface of the steel matrix is 0.02 mu m, putting the steel matrix into ethanol for ultrasonic cleaning, and then cleaning and blow-drying;
and step 3: fixing a steel substrate on a sputtering platform of vacuum magnetron sputtering equipment, then placing a tantalum target material into a magnetron sputtering chamber, ensuring that the distance between the surface of the steel substrate and the tantalum target material is 65mm, and closing the magnetron sputtering chamber;
vacuumizing the magnetron sputtering chamber to make the vacuum degree in the magnetron sputtering chamber 9 × 10-5Pa, introducing argon into the magnetron sputtering chamber, starting a bias power supply when the air pressure in the magnetron sputtering chamber is 1.1Pa, and sputtering and cleaning the steel substrate for 17min to finish the preparation work before coating;
adjusting the air pressure in the magnetron sputtering chamber to 0.5Pa, and starting magnetron sputteringThe sputtering time is 5h, the sputtering power of magnetron sputtering is 53W, the direct-current bias power supply is negative bias-170V, and the sputtering power density is 7W/cm2And the temperature of the steel substrate layer is 350 ℃, and the tantalum steel composite material is prepared after magnetron sputtering.
And 4, step 4: fixing the tantalum steel composite material between an upper red copper electrode and a lower red copper electrode in a composite annealing treatment furnace, applying an external power supply to the two red copper electrodes, wherein the external power supply is a RDY 2000A/12V direct-current power supply, and a steel matrix layer is close to the negative electrode of the external power supply, so that the current flowing through the tantalum steel composite material is 200A;
the tantalum steel composite material is subjected to heating annealing at the annealing temperature of 810 ℃ for 4h, the annealing treatment is performed in an argon atmosphere, and the composite annealing treatment of the electric field and the temperature field can effectively eliminate residual stress generated in the deposition process of a tantalum coating, accelerate the diffusion of C atoms in a steel matrix, promote the in-situ formation of a TaC pinning phase and improve the interface bonding strength;
and finally, taking out the heat-treated sample, ultrasonically cleaning the sample with ethanol for 2.5min, and drying the sample with an electric blower to obtain the tantalum/steel bimetal composite material.
The tantalum coating thickness in the prepared tantalum/steel bimetallic composite was measured to be about 51 μm, and the physical properties are shown in table 1.
TABLE 1 Performance test results for tantalum/steel bimetallic composites prepared in examples 1-5
Examples Hardness of steel base (HV)0.5) Interfacial bond strength (MPa) NbC content (%)
1 1372 215 0.015
2 1344 210 0.010
3 1381 226 0.021
4 1357 212 0.013
5 1365 221 0.017

Claims (7)

1. The preparation method of the tantalum/steel bimetal composite material is characterized by comprising the following steps:
step 1: preparing a steel substrate (1) and a tantalum target material, wherein the carbon content of the steel substrate (1) is 0.5-1.0 wt%, and the tantalum content Ta of the tantalum target material is more than or equal to 99.99 wt%;
step 2: carrying out grinding and polishing treatment on the surface of a steel matrix, and then cleaning and blow-drying;
and step 3: sputtering a tantalum target material on the surface of a steel substrate (1) by adopting vacuum magnetron sputtering equipment to prepare a tantalum steel composite material;
and 4, step 4: placing the tantalum steel composite material in an electric field and a temperature field for composite annealing treatment to obtain a tantalum/steel bimetal composite material;
the specific process of the step 4 is as follows:
step 4.1: fixing the tantalum steel composite material between an upper red copper electrode (4) and a lower red copper electrode (4) in a composite annealing treatment furnace, applying an external power supply (5) to the two red copper electrodes, and enabling a steel matrix (1) to be close to the negative electrode of the external power supply (5) so that the current flowing through the tantalum steel composite material is 50-400A;
step 4.2: the tantalum/steel bimetal composite material is prepared by heating and annealing the tantalum/steel composite material at 780-820 ℃ for 2-6 h, wherein the tantalum/steel bimetal composite material comprises a steel matrix (1) and a tantalum coating (2) on the surface of the steel matrix (1), tantalum carbide particles (3) are distributed between the steel matrix (1) and the tantalum coating (2), the carbon content in the steel matrix (1) is 0.5-1.0 wt%, and the thickness of the tantalum coating (2) is 20-60 mu m.
2. The method for preparing a tantalum/steel bimetal composite material according to claim 1, wherein the steel substrate (1) is alloy steel, carbon steel or tool steel.
3. The preparation method of the tantalum/steel bimetal composite material according to claim 1, wherein in the step 2, the surface of the steel substrate (1) is polished to make the roughness of the surface of the steel substrate (1) be 0.01-0.04 μm, and then the steel substrate (1) is placed in ethanol for ultrasonic cleaning.
4. The method for preparing the tantalum/steel bimetal composite material according to claim 1, wherein the specific process of the step 3 is as follows:
step 3.1: fixing a steel substrate (1) on a sputtering platform of vacuum magnetron sputtering equipment, then placing a tantalum target material into a magnetron sputtering chamber, ensuring that the distance between the surface of the steel substrate (1) and the tantalum target material is 50-70 mm, and closing the magnetron sputtering chamber;
step 3.2: vacuumizing the magnetron sputtering chamber to make the vacuum degree in the magnetron sputtering chamber 610-5Pa～2×10-4Pa, introducing argon into the magnetron sputtering chamber, starting a bias power supply when the air pressure in the magnetron sputtering chamber is 0.7-1.2 Pa, and sputtering and cleaning the steel substrate (1) for 10-20 min to finish the preparation work before coating;
step 3.3: and adjusting the air pressure in the magnetron sputtering chamber to 0.25-0.6 Pa, starting magnetron sputtering for 2-6 h, and preparing the tantalum steel composite material after magnetron sputtering.
5. The method for preparing the tantalum/steel bimetal composite material as claimed in claim 4, wherein the sputtering power of the magnetron sputtering is 30-60W, the direct current bias power supply is negative bias voltage of-80-200V, and the sputtering power density is 2.5W/cm2～8W/cm2And the temperature of the steel matrix layer is 200-400 ℃.
6. The method for preparing the tantalum/steel bimetal composite material as recited in claim 1, wherein the external power supply (5) is a RDY 2000A/12V direct current power supply.
7. The method of claim 1, wherein the composite annealing is performed under an argon atmosphere.
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