CN109175382B - Preparation method of CuCrZr-W bimetallic material - Google Patents
Preparation method of CuCrZr-W bimetallic material Download PDFInfo
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- CN109175382B CN109175382B CN201810934613.0A CN201810934613A CN109175382B CN 109175382 B CN109175382 B CN 109175382B CN 201810934613 A CN201810934613 A CN 201810934613A CN 109175382 B CN109175382 B CN 109175382B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/062—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
- B22F7/064—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts using an intermediate powder layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
Abstract
The invention discloses a preparation method of a CuCrZr-W bimetallic material, which comprises the steps of firstly pretreating the surfaces of a tungsten block and a copper chromium zirconium block, then coating a framework layer on the surface of the pretreated tungsten block, then sintering the tungsten block coated with the framework layer, and then placing the tungsten block coated with the framework layer after sintering and the pretreated copper chromium zirconium block together for atmosphere protection sintering to realize melt-dip connection, thereby obtaining the CuCrZr-W bimetallic material. The bimetal composite material formed by the preparation method of the CuCrZr-W bimetal material has the respective superior performances of metal CuCrZr and metal W, and also has higher bonding strength.
Description
Technical Field
The invention belongs to the technical field of bimetallic composite material preparation methods, and particularly relates to a preparation method of a CuCrZr-W bimetallic material.
Background
Under severe service conditions in a fusion reaction device, the PFM must satisfy the following conditions: 1) high melting point, high heat conduction and strong thermal shock resistance; 2) the plasma has better compatibility with plasma; 3) low sputter etch rate; 4) the neutron irradiation damage resistance is strong. While none of the materials currently fully satisfies the above conditions, W is considered the most promising fully-functional PFM with high melting point, high thermal conductivity, low sputtering rate, low tritium retention, and good thermal shock resistance. In addition, the PFM in the fusion reactor device needs to transfer heat out in time through a heat sink material after suffering from high-heat energy particle impact, so that copper and alloy with ultrahigh heat conductivity are selected as heat sink materials. Because the working environment in a nuclear fusion experimental reactor is complex, and single copper and tungsten are difficult to meet the requirements of various use performances, the tungsten and the copper need to be connected to prepare a divertor component material which is high-temperature resistant and has high thermal conductivity, namely tungsten/copper heterogeneous tungsten/copper bimetallic.
As tungsten/copper heterogeneous metal is used as a special composite material, because the melting points of tungsten and copper are different greatly, the tungsten and the copper are not mutually soluble, and an intermetallic compound is not formed, the general connection method is difficult to realize the high-strength connection of the two materials. In addition, because the thermal expansion coefficients of tungsten and copper are different greatly, a large thermal stress is generated on an interface during working, and the joint is cracked seriously. Meanwhile, in the copper alloy, CuCrZr has the advantages of high strength, hardness, softening temperature, good heat conductivity, low cost and the like, so that a reliable connection technology is found to connect CuCrZr and W, and the preparation of the CuCrZr-W bimetal with good performance is very important.
Disclosure of Invention
The invention aims to provide a preparation method of a CuCrZr-W bimetal material, and the formed bimetal composite material has the respective superior performances of metal CuCrZr and W and also has higher bonding strength.
The technical scheme adopted by the invention is that the preparation method of the CuCrZr-W bimetallic material comprises the steps of firstly pretreating the surfaces of a tungsten block and a copper chromium zirconium block, then coating a framework layer on the surface of the pretreated tungsten block, then sintering the tungsten block coated with the framework layer, and then placing the tungsten block coated with the framework layer after sintering and the pretreated copper chromium zirconium block together for atmosphere protection sintering to realize the melt-dip connection, thereby obtaining the CuCrZr-W bimetallic material.
The present invention is also characterized in that,
the process of pretreating the surface of the tungsten block comprises the following steps: firstly, polishing oxide skin and dirt on the surface of the tungsten block by using sand paper, and then washing the surface of the tungsten block by using acetone.
The process of coating the skeleton layer on the surface of the pretreated tungsten block comprises the following steps: mixing tungsten powder and chromium powder according to a certain proportion, then mixing the tungsten-chromium mixed powder and paraffin according to a certain proportion, heating, melting and stirring uniformly, and coating the mixture on the surface of a pretreated tungsten block to form a framework layer with the thickness of 100-inch-doped 300 mu m.
The chromium powder accounts for the tungsten-chromium mixed powder by mass percent: 5 to 20 percent.
Mixing the tungsten powder and the chromium powder in a mixer for 3-6 h.
Mixing the tungsten-chromium mixed powder with paraffin according to the weight ratio of 5: mixing at a mass ratio of 0.6-1.2.
The process of sintering the tungsten block coated with the skeleton layer comprises the following steps: placing the tungsten block coated with the skeleton layer in a crucible, then placing the crucible in an atmosphere protection sintering furnace, introducing hydrogen, heating to 930-990 ℃, preserving heat for 30-90min, then heating to 1300-1400 ℃, preserving heat for 60-150min, and introducing nitrogen to cool along with the furnace.
The surface of the copper chromium zirconium block is pretreated by the following steps: firstly, polishing oxide skin and dirt on the surface of a copper-chromium-zirconium block by using sand paper, cleaning residual oxide skin which is not polished off by using dilute nitric acid with the concentration of 4-10%, washing residual acid liquor on the surface by using water, and drying.
The specific process of putting the sintered tungsten block and the pretreated copper-chromium-zirconium block together for atmosphere protection sintering to realize the melt-leaching connection comprises the following steps: and (2) placing the tungsten block coated with the framework layer after sintering treatment and the copper-chromium-zirconium block after pretreatment into a crucible, then placing the crucible into an atmosphere protection sintering furnace, introducing hydrogen for sintering, heating to the temperature of 930 plus 990 ℃, preserving heat for 30-60min, exchanging nitrogen for sintering, heating to the temperature of 1300 plus 1400 ℃, preserving heat for 60-150min, slowly cooling to the temperature of 800 plus 950 ℃ for 2-5h, and cooling along with the furnace to obtain the CuCrZr-W bimetal material.
And when the tungsten block coated with the framework layer after sintering treatment and the copper chromium zirconium block after pretreatment are placed in a crucible, the tungsten block is arranged below, and the copper chromium zirconium block is arranged above the tungsten block.
The invention has the beneficial effects that: the invention relates to a preparation method of a CuCrZr-W bimetal material, which is characterized in that a thin tungsten-chromium framework layer prepared in advance is sintered on the surface of W by utilizing the difference of the melting points of CuCrZr and W, and the high-strength metallurgical bonding of the CuCrZr and the W is realized through atmosphere protection sintering and slow cooling treatment, so that the formed bimetal composite material has the respective excellent performances of the CuCrZr and the W, also has higher bonding strength, the shear strength of the bimetal composite material can reach 132MPa at most, and the structural function integration is realized.
Drawings
FIG. 1 is a diagram of the appearance of a CuCrZr-W bimetal interface of a framework layer when chromium powder accounts for 20% of the tungsten-chromium mixed powder by mass;
FIG. 2 hardness profile at the CuCrZr-W bimetallic interface for examples 1-4.
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 preparation method of a CuCrZr-W bimetallic material, which comprises the following steps of firstly pretreating the surfaces of a tungsten block and a copper-chromium-zirconium block, wherein the pretreatment process of the surface of the tungsten block comprises the following steps: firstly, polishing oxide skin and dirt on the surface of a tungsten block by using sand paper, and then washing the surface of the tungsten block by using acetone; the surface of the copper chromium zirconium block is pretreated by the following steps: firstly, polishing oxide skin and dirt on the surface of a copper-chromium-zirconium block by using sand paper, cleaning residual oxide skin which is not polished off by using dilute nitric acid with the concentration of 4-10%, washing residual acid liquor on the surface by using water, and drying; then coating a skeleton layer on the surface of the pretreated tungsten block, wherein the specific process comprises the following steps: mixing tungsten powder and chromium powder according to a certain proportion, then mixing the tungsten-chromium mixed powder and paraffin according to a certain proportion, then mixing the tungsten-chromium mixed powder and the paraffin according to a certain proportion, heating, melting and stirring uniformly, and coating the mixture on the surface of a pretreated tungsten block to form a framework layer with the thickness of 100-doped 300 mu m, wherein the mass percentage of the chromium powder in the tungsten-chromium mixed powder is as follows: 5% -20%; mixing tungsten powder and chromium powder in a mixer for 3-6 h; mixing the tungsten-chromium mixed powder with paraffin according to the weight ratio of 5: mixing at a mass ratio of 0.6-1.2; and sintering the tungsten block coated with the framework layer, wherein the specific process comprises the following steps: placing the tungsten block coated with the framework layer in a crucible, then placing the crucible in an atmosphere protection sintering furnace, introducing hydrogen, heating to 930-990 ℃, preserving heat for 30-90min, then heating to 1300-1400 ℃, preserving heat for 60-150min, and introducing nitrogen to cool along with the furnace; then placing the sintered tungsten block coated with the framework layer and the pretreated copper chromium zirconium block together for atmosphere protection sintering to realize the melt-leaching connection, wherein the specific process of placing the sintered tungsten block and the pretreated copper chromium zirconium block together for atmosphere protection sintering to realize the melt-leaching connection is as follows: placing the tungsten block coated with the framework layer after sintering treatment and the copper chromium zirconium block after pretreatment into a crucible (the tungsten block is below, the copper chromium zirconium block is above the tungsten block), then placing the crucible into an atmosphere protection sintering furnace, introducing hydrogen for sintering, heating to the temperature of 930-990 ℃, preserving heat for 30-60min, exchanging nitrogen for sintering, heating to the temperature of 1300-1400 ℃, preserving heat for 60-150min, slowly cooling to the temperature of 800-950 ℃ for 2-5h, and then cooling with the furnace to obtain the CuCrZr-W bimetal material.
Example 1
Preparing a CuCrZr-W bimetal composite material, processing a tungsten block into a cylinder with the size of phi 20mm multiplied by 15mm, and simultaneously processing a CuCrZr block into a cylinder with the size of phi 20mm multiplied by 40 mm.
Firstly, polishing oxide skin and dirt on the surface of a tungsten block by using sand paper, and then washing the surface of the tungsten block by using acetone; mixing tungsten powder and chromium powder according to a certain proportion (the mass percent of chromium is 5%), mixing in a mixer for 3 hours, and mixing the tungsten-chromium mixed powder with paraffin according to a ratio of 5: mixing at a mass ratio of 0.6, heating to melt, stirring uniformly, and coating on the surface of a tungsten block to form a skeleton layer with a thickness of 200 μm.
And (3) polishing oxide skin and dirt on the surface of the CuCrZr block by using sand paper, cleaning the unabraded oxide skin by using dilute nitric acid with the concentration of 4%, and drying after washing the residual acid liquor on the surface by using water.
Placing the tungsten block coated with the framework layer in a crucible, introducing hydrogen into an atmosphere protection sintering furnace, heating to 930 ℃, preserving heat for 90min, heating to 1300 ℃, preserving heat for 150min, introducing nitrogen, and cooling along with the furnace.
Putting the W block and the CuCrZr block which are burned with the framework layer into a crucible (the tungsten block is under, and the copper chromium zirconium block is above), then putting the crucible into an atmosphere protection sintering furnace, introducing hydrogen for sintering, preserving heat for 60min when the temperature of the sintering furnace reaches 930 ℃, exchanging nitrogen for sintering, preserving heat for 150min when the temperature reaches 1300 ℃, slowly cooling to 950 ℃ after 2h and furnace cooling after the copper liquid is immersed into the framework on the surface of the tungsten block to complete diffusion molding, and obtaining the CuCrZr-W bimetal material. As shown in FIG. 2, the average thickness of the skeleton was found to be 167. mu.m, the hardness in the vicinity of the interface was found to be in a gradient distribution, the hardness at the W-side interface was found to be 212HV, and the interface shear strength was found to be 113 MPa.
Example 2
Preparing a CuCrZr-W bimetal composite material, processing a tungsten block into a cylinder with the size of phi 20mm multiplied by 15mm, and simultaneously processing a CuCrZr block into a cylinder with the size of phi 20mm multiplied by 40 mm.
Firstly, polishing oxide skin and dirt on the surface of a tungsten block by using sand paper, and then washing the surface of the tungsten block by using acetone; mixing tungsten powder and chromium powder according to a certain proportion (the mass percent of chromium is 10 percent), mixing for 4 hours in a mixer, and then mixing the tungsten-chromium mixed powder with paraffin according to a ratio of 5: mixing at a mass ratio of 0.8, heating to melt, stirring uniformly, and coating on the surface of a tungsten block to form a skeleton layer with a thickness of 200 μm.
And (3) polishing oxide skin and dirt on the surface of the CuCrZr block by using sand paper, cleaning the unabraded oxide skin by using dilute nitric acid with the concentration of 6%, and drying after washing the residual acid liquor on the surface by using water.
Placing the tungsten block coated with the framework layer in a crucible, introducing hydrogen into an atmosphere protection sintering furnace, heating to 950 ℃, preserving heat for 70min, heating to 1350 ℃, preserving heat for 120min, introducing nitrogen, and cooling along with the furnace.
Putting the W block and the CuCrZr block which are burned with the framework layer into a crucible (the tungsten block is under, and the copper chromium zirconium block is above), then putting the crucible into an atmosphere protection sintering furnace, introducing hydrogen for sintering, preserving heat for 50min when the temperature of the sintering furnace reaches 950 ℃, exchanging nitrogen for sintering, preserving heat for 90min when the temperature reaches 1330, slowly cooling to 900 ℃ after 3h after copper liquid is immersed into the framework on the surface of the tungsten block to complete diffusion molding, and furnace-cooling to obtain the CuCrZr-W bimetal material. As shown in FIG. 2, the average thickness of the skeleton was found to be 252 μm, the hardness in the vicinity of the interface was found to be distributed in a gradient manner, the hardness at the W-side interface was found to be 253HV, and the interface shear strength was found to be 125 MPa.
Example 3
Preparing a CuCrZr-W bimetal composite material, processing a tungsten block into a cylinder with the size of phi 20mm multiplied by 15mm, and simultaneously processing the CuCrZr into a cylinder with the size of phi 20mm multiplied by 40 mm.
Firstly, polishing oxide skin and dirt on the surface of a tungsten block by using sand paper, and then washing the surface of the tungsten block by using acetone; mixing tungsten powder and chromium powder according to a certain proportion (the mass percent of chromium is 15 percent), mixing the tungsten powder and the chromium powder in a mixer for 5 hours, and then mixing the tungsten powder and the chromium powder with paraffin according to a ratio of 5: 1, heating, melting and stirring uniformly, and coating the mixture on the surface of a tungsten block to form a skeleton layer with the thickness of 200 mu m.
And (3) polishing oxide skins and dirt on the surfaces of the copper-chromium-zirconium blocks by using sand paper, cleaning the oxide skins which are not polished off by using dilute nitric acid with the concentration of 8%, and drying after washing residual acid liquor on the surfaces by using water.
And placing the tungsten block coated with the framework layer in a crucible, introducing hydrogen into an atmosphere protection sintering furnace, heating to 970 ℃, preserving heat for 40min, heating to 1400 ℃, preserving heat for 90min, introducing nitrogen, and cooling along with the furnace.
Putting the W block and the CuCrZr block which are burned with the framework layer into a crucible (the tungsten block is under, and the copper chromium zirconium block is above), then putting the crucible into an atmosphere protection sintering furnace, introducing hydrogen for sintering, preserving heat for 40min when the temperature of the sintering furnace reaches 970 ℃, exchanging nitrogen for sintering, preserving heat for 90min when the temperature reaches 1380 ℃, after copper liquid is immersed into the framework on the surface of the tungsten block to complete diffusion molding, slowly cooling to 850 ℃ after 4h, and furnace-cooling to obtain the CuCrZr-W bimetal material. As shown in FIG. 2, the average thickness of the skeleton was found to be 208 μm, the hardness in the vicinity of the interface was found to be in a gradient distribution, the hardness at the W-side interface was found to be 283HV, and the interface shear strength was found to be 130MPa.
Example 4
Preparing a CuCrZr-W bimetal composite material, processing a tungsten block into a cylinder with the size of phi 20mm multiplied by 15mm, and simultaneously processing a copper chromium zirconium block into a cylinder with the size of phi 20mm multiplied by 40 mm.
Firstly, polishing oxide skin and dirt on the surface of a tungsten block by using sand paper, and then washing the surface of the tungsten block by using acetone; mixing tungsten powder and chromium powder according to a certain proportion (the mass percent of chromium is 20 percent), mixing in a mixer for 6 hours, and then mixing the tungsten-chromium mixed powder with paraffin according to a ratio of 5: 1.2, heating, melting and stirring uniformly, and then coating the mixture on the surface of a tungsten block to form a skeleton layer with the thickness of 200 mu m.
And (3) polishing oxide skins and dirt on the surfaces of the copper-chromium-zirconium blocks by using sand paper, cleaning the unabraded oxide skins by using 10% dilute nitric acid, washing the residual acid liquor on the surfaces by using water, and drying.
And placing the tungsten block coated with the skeleton layer in a crucible, introducing hydrogen into an atmosphere protection sintering furnace, heating to 990 ℃, preserving heat for 30min, heating to 1400 ℃, preserving heat for 60min, introducing nitrogen, and cooling along with the furnace.
Putting the W block and the CuCrZr block which are burned with the framework layer into a crucible (the tungsten block is under, and the copper chromium zirconium block is above), then putting the crucible into an atmosphere protection sintering furnace, introducing hydrogen for sintering, preserving heat for 30min when the temperature of the sintering furnace reaches 990 ℃, exchanging nitrogen for sintering, preserving heat for 60min when the temperature reaches 1400 ℃, after copper liquid is immersed into the framework on the surface of the tungsten block to complete diffusion molding, slowly cooling to 800 ℃ after 5h, and furnace-cooling to obtain the CuCrZr-W bimetal material. As shown in FIGS. 1 and 2, the average thickness of the skeleton was found to be 265. mu.m, the hardness in the vicinity of the interface was graded, the hardness at the W-side interface reached 286HV, and the interface shear strength reached 132 MPa.
Claims (6)
1. The preparation method of the CuCrZr-W bimetallic material is characterized by firstly pretreating the surfaces of a tungsten block and a copper-chromium-zirconium block, then mixing tungsten powder and chromium powder according to a certain proportion to obtain tungsten-chromium mixed powder, wherein the chromium powder accounts for the tungsten-chromium mixed powder by mass percent: 5% -20%, then mixing the tungsten-chromium mixed powder with paraffin according to a certain proportion, heating to melt and stirring uniformly, coating the mixture on the surface of a pretreated tungsten block to form a framework layer with the thickness of 100-plus-material 300 mu m, then placing the tungsten block coated with the framework layer in a crucible, then placing the crucible in an atmosphere protection sintering furnace, introducing hydrogen to heat to 930-plus-material 990 ℃, preserving heat for 30-90min, heating to 1300-plus-material 1400 ℃, preserving heat for 60-150min, and introducing nitrogen to cool along with the furnace;
and (3) placing the tungsten block coated with the framework layer after sintering treatment and the copper-chromium-zirconium block after pretreatment into a crucible, placing the crucible into an atmosphere protection sintering furnace, introducing hydrogen for sintering, heating to the temperature of 930 plus 990 ℃, preserving heat for 30-60min, exchanging nitrogen for sintering, heating to the temperature of 1300 plus 1400 ℃, preserving heat for 60-150min, slowly cooling to 800 plus 950 ℃ for 2-5h, and cooling with the furnace to obtain the CuCrZr-W bimetal material.
2. The method for preparing the CuCrZr-W bimetal material according to claim 1, wherein the pretreatment process for the surface of the tungsten block comprises the following steps: firstly, polishing oxide skin and dirt on the surface of the tungsten block by using sand paper, and then washing the surface of the tungsten block by using acetone.
3. The method for preparing the CuCrZr-W bimetallic material as in claim 1, wherein the tungsten powder and the chromium powder are mixed in a mixer for 3-6 h.
4. The method for preparing the CuCrZr-W bimetal material according to claim 1, wherein the tungsten-chromium mixed powder and paraffin wax are mixed according to the weight ratio of 5: mixing at a mass ratio of 0.6-1.2.
5. The preparation method of the CuCrZr-W bimetal material as claimed in claim 1, wherein the pretreatment process for the surface of the copper chromium zirconium block comprises the following steps: firstly, polishing oxide skin and dirt on the surface of a copper-chromium-zirconium block by using sand paper, cleaning residual oxide skin which is not polished off by using dilute nitric acid with the concentration of 4-10%, washing residual acid liquor on the surface by using water, and drying.
6. The method for preparing the CuCrZr-W bimetal material according to claim 1, wherein when the tungsten block coated with the framework layer after the sintering treatment and the copper chromium zirconium block after the pretreatment are placed in a crucible, the tungsten block is arranged at the bottom, and the copper chromium zirconium block is arranged on the tungsten block.
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