CN110181050B - WRe/TZM/graphite SPS sintering connection method - Google Patents

WRe/TZM/graphite SPS sintering connection method Download PDF

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CN110181050B
CN110181050B CN201910479310.9A CN201910479310A CN110181050B CN 110181050 B CN110181050 B CN 110181050B CN 201910479310 A CN201910479310 A CN 201910479310A CN 110181050 B CN110181050 B CN 110181050B
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graphite
tzm
temperature
wre
sintering
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CN110181050A (en
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张久兴
沈学峰
施加利
韩翠柳
潘亚飞
杨新宇
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Hefei University of Technology
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Hefei University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • B22F3/03Press-moulding apparatus therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infra-red radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture 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
    • B22F7/02Manufacture 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 layers
    • B22F7/04Manufacture 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 layers with one or more layers not made from powder, e.g. made from solid metal
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04Alloys based on tungsten or molybdenum

Abstract

The invention discloses an SPS sintering connection method of WRe/TZM/graphite, which adopts a graphite gradient mold, realizes gradient sintering of WRe alloy powder and TZM alloy powder by an SPS technology, and simultaneously realizes dissimilar material connection between the TZM alloy powder and a graphite block by taking a titanium foil as an intermediate transition layer, thereby obtaining a WRe/TZM/graphite dissimilar material connection piece. The WRe/TZM/graphite dissimilar material connecting piece which is compact in sintering, uniform in continuous interface diffusion, high in bonding strength, good in heat dissipation performance and good in thermal shock resistance can be obtained through the connecting method, the density of the WRe alloy layer reaches 98.07%, the density of the TZM alloy layer reaches 97.98%, the diffusion of the connecting surface is uniform, the WRe/TZM side of the room-temperature shearing strength of the connecting piece can reach 303.9MPa, and the TZM/graphite side of the connecting piece can reach 31.2 MPa.

Description

WRe/TZM/graphite SPS sintering connection method
Technical Field
The invention relates to a sintering connection method of dissimilar materials, in particular to an SPS sintering connection method of WRe/TZM/graphite.
Background
The WRe alloy is an alloy consisting of W and Re, the W has high melting point, high-temperature strength, good heat dissipation performance and high atomic number, strong X-ray can be excited under electron bombardment, but the W has a notch sensitive effect and is easy to cause the expansion and deepening of cracks, so that a target material matrix is peeled off, the recrystallization temperature of the Re is 500 ℃ higher than that of the W, and the Re does not have a plastic-brittle transition temperature. Therefore, the addition of Re can obviously improve the room temperature brittleness of W, reduce the plastic-brittle transition temperature and enhance the mechanical property of W in a certain high-temperature area. The TZM alloy is a widely used molybdenum-based alloy, is mainly applied to the fields of aerospace, power generation, nuclear reactors, military, medical instruments and the like at present, and has the characteristics of high melting point, high elastic modulus, strong corrosion resistance, low thermal expansion coefficient, high thermal conductivity, excellent high-temperature mechanical property and the like. Graphite is a widely used carbon material, and the special structure makes it have high temperature resistance, good electric and thermal conductivity, good chemical stability, thermal shock resistance and other properties, but the strength of the graphite material is not high, graphite and metal are often used in combination in modern industry, such as a target material for a high-power CT machine, a heat transfer part of a nuclear fusion reactor and the like, and the composite structure has the excellent properties of graphite and metal. In addition, the density of graphite is far lower than that of common alloy, the light weight is one of the exploration directions of modern industry, and on the premise of ensuring the quality of equipment, the output power can be improved, the energy consumption can be reduced, the service life of the equipment can be prolonged, and the like.
The WRe/TZM/graphite connecting piece is obtained in the prior art through multiple steps, generally, the WRe alloy and the TZM alloy are prepared through sintering, then the WRe alloy and the TZM alloy are connected in a diffusion mode, and then the WRe-TZM alloy connecting piece is connected with graphite.
Disclosure of Invention
The invention aims to provide an SPS sintering connection method of WRe/TZM/graphite based on the current exploration of a WRe alloy powder and TZM alloy powder sintering technology, a WRe alloy and TZM alloy connection technology and a TZM alloy and graphite connection technology. The invention can realize WRe/TZM/graphite sintering connection in one step on the premise of compact sintering and good connection, effectively simplifies the process flow, has high material utilization rate and greatly reduces the energy consumption.
The SPS technology is applied to solid sintering and solid diffusion connection of refractory alloy, the titanium foil is added to serve as an intermediate transition layer, so that the welding temperature is reduced, a complete solid solution is formed in a welding line through atomic interdiffusion, and the mechanical property of a welding joint is improved.
The WRe/TZM/graphite SPS sintering connection method comprises the following steps:
step 1: weighing W-5% of Re alloy powder and TZM alloy powder raw materials according to the proportion; selecting a titanium foil with the thickness of 200 mu m and the purity of more than or equal to 99.0 percent, and carrying out acid washing, ultrasonic cleaning and drying to be used as an intermediate transition layer; taking graphite to be connected, pre-grinding, polishing and ultrasonically cleaning the surface to be welded of the graphite, and drying in vacuum;
step 2: taking a female die of a graphite gradient die, installing a lining and a lower pressure head, putting weighed TZM powder into the graphite die, prepressing and compacting by adopting a manual hydraulic press, then putting the weighed W-5% Re alloy powder on the upper side of the compacted TZM powder, prepressing and compacting by adopting the manual hydraulic press, keeping the pressure for 2min under the prepressing parameter of 10MPa, then taking down the pressure head, putting a titanium foil on the prepressed TZM powder side, adding a graphite block, finally adding an upper pressure head and a lower pressure head, and prepressing for 2min integrally under the pressure of 10 MPa; during prepressing, the sample loading sequence of the sample is a graphite block, a titanium foil, a TZM alloy layer and a W-5% Re alloy layer from bottom to top.
And step 3: and (3) placing the graphite mold provided with the connecting piece to be sintered obtained in the step (2) in a hearth of a spark plasma sintering system, vacuumizing to be lower than 10Pa, and then introducing direct current pulse current to perform gradient sintering connection.
In the step 1, the graphite to be connected is directly polished and then ultrasonically cleaned in alcohol, so that the flatness of the surface to be welded of the treated graphite is not more than 0.1mm, and the roughness is not more than 0.1 mu m. The density of the graphite is more than or equal to 1.86g/cm3The breaking strength is more than or equal to 59.0 MPa.
In the step 1, the Fisher size of the W-5% Re alloy powder is 3-4 μm, and the Fisher size of the TZM alloy powder is 2-3 μm.
In the step 1, the acid washing is to soak the titanium foil for 10 minutes by using dilute hydrochloric acid with the volume concentration of 5%; the ultrasonic cleaning is carried out in alcohol.
In step 2, the graphite gradient mold comprises a female mold, a bushing, an upper pressure head and a lower pressure head.
The female die is of a through hollow cavity structure and is divided into an upper part and a lower part according to the difference of the wall thickness of the female die, the upper part is a high-temperature region, the lower part is a low-temperature region, in the sintering connection process, the interface of the high-temperature region and the low-temperature region of the female die in the horizontal direction is superposed with the upper surface of the TZM alloy layer, the high-temperature region meets the sintering densification temperature of WRe alloy, and the low-temperature region meets the sintering densification temperature of the TZM alloy and the tight connection temperature of the TZM alloy and the graphite block. The wall thickness of the high-temperature area is smaller than that of the low-temperature area, the temperature difference between the high-temperature area and the low-temperature area is regulated and controlled through the wall thickness, and the temperatures of the high-temperature area and the low-temperature area are respectively measured through temperature measuring holes arranged in the high-temperature area and the low-temperature area.
The bush is arranged on the inner surface of the cavity of the female die, is a hollow graphite tube and is used for placing WRe alloy powder, TZM alloy powder and graphite blocks. Because the female die is provided with the temperature measuring hole, the female die is easy to damage due to uneven high-pressure stress, and the bush can effectively avoid the phenomenon.
During assembly, the lower pressure head is inserted into the hollow cavity of the female die from the bottom of the female die to play a supporting role; and the upper pressure head is inserted into the hollow cavity of the female die from the upper part of the female die and is used for applying pressure to the sample.
Furthermore, the longitudinal section of the lower pressure head is of an inverted T-shaped structure, when the lower pressure head is assembled, the vertical protruding part of the inverted T-shaped structure is inserted into the hollow cavity of the female die from the bottom of the female die, and the transverse part of the inverted T-shaped structure is located below the female die and is tightly combined with the female die to play a role in limiting.
In the process of sintering connection, when the low-temperature region reaches the sintering temperature, the temperature difference between the high-temperature region and the low-temperature region is 200-220 ℃.
All the temperatures are subject to the temperature of the temperature measuring hole.
In step 3, the parameters of the gradient sintering connection process are set as follows:
axial pressure: fixing a lower pressure head, and applying pressure of 20-40MPa through an upper pressure head;
the heating rate is as follows: heating at a heating rate of 20-70 ℃/min, stopping heating when the low-temperature region reaches the sintering temperature of 1450-1650 ℃, and preserving heat for 10-60 min;
sintering connection temperature: 1450 ℃ and 1650 ℃ (low temperature region);
cooling rate: the temperature reduction rate of the interval from the connection temperature to 1000 ℃ is 10 ℃/min, the temperature reduction rate of the interval from 1000 ℃ to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace; and obtaining the WRe/TZM/graphite dissimilar material connecting piece after cooling.
The welding process conditions are obtained based on univariate scientific experimental design and a large number of experimental groceries, and under the conditions, the comprehensive performance of the product is optimal.
Compared with the prior art, the invention has the beneficial effects that:
1. the WRe/TZM/graphite dissimilar material connecting piece which is compact in sintering, uniform in diffusion of a connecting interface, high in bonding strength, good in heat dissipation performance and good in thermal shock resistance can be obtained through the connecting method.
2. The invention adopts SPS diffusion welding technology, and has the characteristics of simple process flow, easy control of process parameters, stable quality, strong operability, low connection temperature and low energy consumption, thereby reducing the production period and the cost.
3. The method can realize WRe/TZM/graphite sintering connection in one step through the gradient die. The invention can effectively simplify the process flow, greatly reduce the energy consumption and reduce the production period and the cost on the premise of ensuring compact sintering and good connection.
According to the WRe/TZM/graphite composite material obtained by the invention, the density of a WRe alloy layer reaches 98.07%, the density of a TZM alloy layer reaches 97.98%, the diffusion of a connecting surface is uniform, the room-temperature shear strength WRe/TZM side of a joint can reach 303.9MPa, and the room-temperature shear strength TZM/graphite side of the joint can reach 31.2 MPa. And the actual production requirement can be met.
Drawings
Fig. 1 and 2 are schematic diagrams of a gradient mold structure and sample loading.
Reference numbers in the figures: 1 upper pressure head, 2 lining, 3 concave die, 4 temperature measuring holes, 5 lower pressure head, 6WRe alloy layer, 7TZM alloy layer, 8Ti foil and 9 graphite block.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples, but the embodiments of the present invention are not limited thereto.
The spark plasma sintering furnace used in the following examples is a LABOX-6020hv spark plasma sintering system manufactured by Sinter Land inc, Japan, the current type of which is DC pulse current, the pulse sequence is 40: 7; the inner diameter of a liner of the gradient graphite mold is phi 30mm, the gradient mold is divided into an upper part and a lower part, the upper part is a high-temperature area, the lower part is a low-temperature area, and the wall thickness difference between the high-temperature area and the low-temperature area of the gradient mold is 10mm, so that the temperature difference between the high-temperature area and the low-temperature area meets the temperature required by sintering densification of WRe alloy and TZM alloy and the solid-phase connection temperature of graphite and TZM alloy.
The WRe alloy powder (W-5% Re alloy powder) used in the following examples was from Wighai polycrystalline tungsten molybdenum technology, Inc., and had a Fisher size of 3 to 4 μm.
The TZM alloy powder used in the following examples is from Mo, Mach-Zehnder, Inc., with a Fisher size of 2-3 μm.
The bulk graphite used in the following examples was high strength graphite from carbon corporation of east China sea, Japan, under the designation G535.
The temperature measured by the following embodiments is measured by taking the temperature of the temperature measuring hole in the low temperature region as a reference, and the temperature measuring hole in the high temperature region is used for auxiliary measurement.
Example 1:
in the embodiment, the SPS diffusion welding of the TZM and the graphite dissimilar material is carried out according to the following steps:
1. taking graphite to be connected, pre-grinding, polishing, ultrasonically cleaning and vacuum drying the to-be-welded surface of the graphite, and ensuring that the flatness of the to-be-welded surface of the graphite is not more than 0.1mm and the roughness is not more than 0.1 mu m.
2. And (3) putting the titanium foil into dilute hydrochloric acid with the volume concentration of 5% for acid washing for 10min, then putting the titanium foil into alcohol for ultrasonic cleaning, and finally drying for later use.
3. Weighing W-5% of Re alloy powder and TZM alloy powder as required.
4. And (2) taking a graphite female die, installing a bushing and a lower pressing head, sequentially putting weighed TZM alloy powder and WRe alloy powder into a graphite die, respectively prepressing by adopting a manual hydraulic press at the pressure of 10MPa for 2min, then taking down the pressing head, placing Ti foil on the side of the prepressed TZM alloy powder, adding a graphite block, finally adding an upper pressing head and a lower pressing head, and integrally prepressing at the pressure of 10MPa for 2 min.
5. Placing a graphite mold with a to-be-welded part in a hearth of a discharge plasma sintering system, vacuumizing to be lower than 10Pa, and then introducing direct current pulse current, wherein the sintering connection process comprises the following steps:
axial pressure: fixing a lower pressure head, and applying pressure of 30MPa through an upper pressure head;
the heating rate is as follows: heating at a heating rate of 20-70 deg.C/min, stopping heating when the low-temperature region reaches the sintering temperature 1450, and keeping the temperature for 30 min;
sintering connection temperature: 1500 ℃ (low temperature zone) and 1690 ℃ (high temperature zone);
cooling rate: the temperature reduction rate of the interval from the connection temperature to 1000 ℃ is 10 ℃/min, the temperature reduction rate of the interval from 1000 ℃ to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace; and obtaining the WRe/TZM/graphite dissimilar material connecting piece after cooling.
Tests prove that the WRe/TZM/graphite composite material obtained in the embodiment has the advantages that the density of the WRe alloy layer reaches 94.53%, the density of the TZM alloy layer reaches 97.55%, the diffusion of the connection surface is uniform, the room-temperature shear strength WRe/TZM side of the joint can reach 283.8MPa, and the room-temperature shear strength TZM/graphite side of the joint can reach 23.6 MPa.
Example 2:
in the embodiment, the SPS diffusion welding of the TZM and the graphite dissimilar material is carried out according to the following steps:
1. taking graphite to be connected, pre-grinding, polishing, ultrasonically cleaning and vacuum drying the to-be-welded surface of the graphite, and ensuring that the flatness of the to-be-welded surface of the graphite is not more than 0.1mm and the roughness is not more than 0.1 mu m.
2. And (3) putting the titanium foil into dilute hydrochloric acid with the volume concentration of 5% for acid washing for 10min, then putting the titanium foil into alcohol for ultrasonic cleaning, and finally drying for later use.
3. Weighing W-5% of Re alloy powder and TZM alloy powder as required.
4. And (2) taking a graphite female die, installing a bushing and a lower pressing head, sequentially putting weighed TZM alloy powder and WRe alloy powder into a graphite die, respectively prepressing by adopting a manual hydraulic press at the pressure of 10MPa for 2min, then taking down the pressing head, placing Ti foil on the side of the prepressed TZM alloy powder, adding a graphite block, finally adding an upper pressing head and a lower pressing head, and integrally prepressing at the pressure of 10MPa for 2 min.
5. Placing a graphite mold with a to-be-welded part in a hearth of a discharge plasma sintering system, vacuumizing to be lower than 10Pa, and then introducing direct current pulse current, wherein the sintering connection process comprises the following steps:
axial pressure: fixing a lower pressure head, and applying pressure of 30MPa through an upper pressure head;
the heating rate is as follows: heating at a heating rate of 20-70 deg.C/min, stopping heating when the low-temperature region reaches the sintering temperature of 1550 deg.C, and keeping the temperature for 30 min;
sintering connection temperature: 1550 ℃ (low temperature zone) and 1780 ℃ (high temperature zone);
cooling rate: the temperature reduction rate of the interval from the connection temperature to 1000 ℃ is 10 ℃/min, the temperature reduction rate of the interval from 1000 ℃ to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace; and obtaining the WRe/TZM/graphite dissimilar material connecting piece after cooling.
Tests prove that the WRe/TZM/graphite composite material obtained in the embodiment has the WRe alloy layer density of 98.07%, the TZM alloy layer density of 97.98%, the connection surface is uniformly diffused, the room-temperature shear strength WRe/TZM side of the joint can reach 303.9MPa, and the TZM/graphite side can reach 31.2 MPa.
Example 3:
in the embodiment, the SPS diffusion welding of the TZM and the graphite dissimilar material is carried out according to the following steps:
1. taking graphite to be connected, pre-grinding, polishing, ultrasonically cleaning and vacuum drying the to-be-welded surface of the graphite, and ensuring that the flatness of the to-be-welded surface of the graphite is not more than 0.1mm and the roughness is not more than 0.1 mu m.
2. And (3) putting the titanium foil into dilute hydrochloric acid with the volume concentration of 5% for acid washing for 10min, then putting the titanium foil into alcohol for ultrasonic cleaning, and finally drying for later use.
3. Weighing W-5% of Re alloy powder and TZM alloy powder as required.
4. And (2) taking a graphite female die, installing a bushing and a lower pressing head, sequentially putting weighed TZM alloy powder and WRe alloy powder into a graphite die, respectively prepressing by adopting a manual hydraulic press at the pressure of 10MPa for 2min, then taking down the pressing head, placing Ti foil on the side of the prepressed TZM alloy powder, adding a graphite block, finally adding an upper pressing head and a lower pressing head, and integrally prepressing at the pressure of 10MPa for 2 min.
5. Placing a graphite mold with a to-be-welded part in a hearth of a discharge plasma sintering system, vacuumizing to be lower than 10Pa, and then introducing direct current pulse current, wherein the sintering connection process comprises the following steps:
axial pressure: fixing a lower pressure head, and applying pressure of 30MPa through an upper pressure head;
the heating rate is as follows: heating at a heating rate of 20-70 deg.C/min, stopping heating when the low-temperature region reaches the sintering temperature of 1550 deg.C, and keeping the temperature for 15 min;
sintering connection temperature: 1550 ℃ (low temperature zone) and 1770 ℃ (high temperature zone);
cooling rate: the temperature reduction rate of the interval from the connection temperature to 1000 ℃ is 10 ℃/min, the temperature reduction rate of the interval from 1000 ℃ to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace; and obtaining the WRe/TZM/graphite dissimilar material connecting piece after cooling.
Tests prove that the WRe/TZM/graphite composite material obtained in the embodiment has the WRe alloy layer density of 98.04%, the TZM alloy layer density of 97.82%, the connection surface is uniformly diffused, the room-temperature shear strength WRe/TZM side of the joint can reach 296.0MPa, and the TZM/graphite side can reach 29.9 MPa.

Claims (3)

1. An SPS sintering connection method of WRe/TZM/graphite is characterized in that:
adopting a graphite gradient die, realizing gradient sintering of WRe alloy powder and TZM alloy powder by using an SPS technology, and simultaneously realizing the connection of dissimilar materials between the TZM alloy powder and a graphite block by using a titanium foil as an intermediate transition layer, thereby obtaining a WRe/TZM/graphite dissimilar material connecting piece; the method specifically comprises the following steps:
step 1: weighing W-5% of Re alloy powder and TZM alloy powder raw materials according to the proportion; selecting a titanium foil with the thickness of 200 mu m and the purity of more than or equal to 99.0 percent, and carrying out acid washing, ultrasonic cleaning and drying to be used as an intermediate transition layer; taking graphite to be connected, pre-grinding, polishing and ultrasonically cleaning the surface to be welded of the graphite, and drying in vacuum;
step 2: taking a female die of a graphite gradient die, installing a lining and a lower pressure head, putting weighed TZM powder into the graphite die, prepressing and compacting by adopting a manual hydraulic press, then putting the weighed W-5% Re alloy powder on the upper side of the compacted TZM powder, prepressing and compacting by adopting the manual hydraulic press, keeping the pressure for 2min under the prepressing parameter of 10MPa, then taking down the pressure head, putting a titanium foil on the prepressed TZM powder side, adding a graphite block, finally adding an upper pressure head and a lower pressure head, and prepressing for 2min integrally under the pressure of 10 MPa; during prepressing, the sample loading sequence of the sample sequentially comprises a graphite block, a titanium foil, a TZM alloy layer and a W-5% Re alloy layer from bottom to top;
and step 3: placing the graphite mold provided with the connecting piece to be sintered obtained in the step 2 in a hearth of a spark plasma sintering system, vacuumizing to be lower than 10Pa, and then introducing direct current pulse current to perform gradient sintering connection;
in step 3, the parameters of the gradient sintering connection process are set as follows:
axial pressure: fixing a lower pressure head, and applying pressure of 30MPa through an upper pressure head;
the heating rate is as follows: heating at a heating rate of 20-70 deg.C/min, stopping heating when the low-temperature region reaches the sintering temperature of 1550 deg.C, and keeping the temperature for 30 min;
sintering connection temperature: the low temperature region is 1550 ℃ and the high temperature region is 1780 ℃;
cooling rate: the temperature reduction rate of the interval from the connection temperature to 1000 ℃ is 10 ℃/min, the temperature reduction rate of the interval from 1000 ℃ to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace; obtaining a WRe/TZM/graphite dissimilar material connecting piece after cooling; tests prove that the density of the WRe alloy layer of the obtained WRe/TZM/graphite composite material reaches 98.07 percent, the density of the TZM alloy layer reaches 97.98 percent, the diffusion of the connecting surface is uniform, the room-temperature shear strength WRe/TZM side of the joint can reach 303.9MPa, and the room-temperature shear strength TZM/graphite side of the joint can reach 31.2 MPa;
the graphite gradient mold comprises a female mold, a bushing, an upper pressure head and a lower pressure head;
the female die is a through hollow cavity structure and is divided into an upper part and a lower part according to the difference of the wall thickness of the female die, wherein the upper part is a high-temperature area, and the lower part is a low-temperature area; in the process of sintering connection, the interface of the high-temperature area and the low-temperature area of the female die in the horizontal direction is superposed with the upper surface of the TZM alloy layer; the wall thickness of the high-temperature area is smaller than that of the low-temperature area, and the temperature difference between the high-temperature area and the low-temperature area is regulated and controlled through the wall thickness;
in the step 1, directly polishing graphite to be connected, and then ultrasonically cleaning the graphite in alcohol to ensure that the planeness of a to-be-welded surface of the treated graphite is not more than 0.1mm and the roughness is not more than 0.1 mu m; the density of the graphite is more than or equal to 1.86g/cm3The breaking strength is more than or equal to 59.0 MPa;
in the step 1, the Fisher particle size of the W-5% Re alloy powder is 3-4 μm, and the Fisher particle size of the TZM alloy powder is 2-3 μm;
in the step 1, the acid washing is to soak the titanium foil for 10 minutes by using dilute hydrochloric acid with the volume concentration of 5%; the ultrasonic cleaning is carried out in alcohol.
2. The method of claim 1, wherein:
temperature measuring holes are respectively arranged in the high-temperature area and the low-temperature area to measure the temperature of the high-temperature area and the low-temperature area.
3. The method of claim 1, wherein:
the longitudinal section of the lower pressure head is of an inverted T-shaped structure, when the lower pressure head is assembled, the vertical protruding part of the inverted T-shaped structure is inserted into the hollow cavity of the female die from the bottom of the female die, and the transverse part of the inverted T-shaped structure is located below the female die and is tightly combined with the female die to play a role in limiting.
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CN112091211B (en) * 2020-08-20 2021-09-10 上海交通大学 Preparation method of diffusion multi-element joint
CN112958772A (en) * 2021-02-02 2021-06-15 合肥工业大学 Method for repairing waste WRe/TZM composite rotary anode target disc
CN112958770A (en) * 2021-02-02 2021-06-15 合肥工业大学 Preparation method of WRe/TZM composite material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3223403B2 (en) * 1993-10-28 2001-10-29 日本電信電話株式会社 One-frequency time-division two-way spread spectrum communication system
CN107175398A (en) * 2017-06-28 2017-09-19 合肥工业大学 A kind of SPS diffusion welding methods of molybdenum alloy and tungsten alloy
CN107486619A (en) * 2017-08-30 2017-12-19 合肥工业大学 TZM and WRe xenogenesis refractory alloys a kind of SPS diffusion welding methods
CN109048030A (en) * 2018-08-20 2018-12-21 合肥工业大学 A kind of SPS diffusion welding method of TZM and graphite dissimilar material
CN109590476A (en) * 2018-12-21 2019-04-09 合肥工业大学 The method that one-step method prepares high-compactness WRe/TZM gradient composites

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2698854B2 (en) * 1990-01-26 1998-01-19 住友重機械工業株式会社 Method of manufacturing screw for plastic molding machine and method of forming alloy layer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3223403B2 (en) * 1993-10-28 2001-10-29 日本電信電話株式会社 One-frequency time-division two-way spread spectrum communication system
CN107175398A (en) * 2017-06-28 2017-09-19 合肥工业大学 A kind of SPS diffusion welding methods of molybdenum alloy and tungsten alloy
CN107486619A (en) * 2017-08-30 2017-12-19 合肥工业大学 TZM and WRe xenogenesis refractory alloys a kind of SPS diffusion welding methods
CN109048030A (en) * 2018-08-20 2018-12-21 合肥工业大学 A kind of SPS diffusion welding method of TZM and graphite dissimilar material
CN109590476A (en) * 2018-12-21 2019-04-09 合肥工业大学 The method that one-step method prepares high-compactness WRe/TZM gradient composites

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