CN110181050A - A kind of SPS sintering connection method of WRe/TZM/ graphite - Google Patents
A kind of SPS sintering connection method of WRe/TZM/ graphite Download PDFInfo
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- CN110181050A CN110181050A CN201910479310.9A CN201910479310A CN110181050A CN 110181050 A CN110181050 A CN 110181050A CN 201910479310 A CN201910479310 A CN 201910479310A CN 110181050 A CN110181050 A CN 110181050A
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- graphite
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- tzm
- wre
- alloy powder
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 90
- 239000010439 graphite Substances 0.000 title claims abstract description 90
- 238000005245 sintering Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 44
- 239000000956 alloy Substances 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 44
- 239000000463 material Substances 0.000 claims abstract description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005516 engineering process Methods 0.000 claims abstract description 13
- 238000005304 joining Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 13
- 229910000691 Re alloy Inorganic materials 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 238000004826 seaming Methods 0.000 claims description 9
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 7
- 238000003466 welding Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 229910052702 rhenium Inorganic materials 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 230000002742 anti-folding effect Effects 0.000 claims 1
- 238000009792 diffusion process Methods 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000280 densification Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 229910052751 metal Chemical group 0.000 description 2
- 239000002184 metal Chemical group 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 229910000753 refractory alloy Inorganic materials 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001778 solid-state sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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
- B22F3/02—Compacting only
- B22F3/03—Press-moulding apparatus therefor
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
- B22F7/02—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 layers
- B22F7/04—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 layers with one or more layers not made from powder, e.g. made from solid metal
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
Abstract
The invention discloses a kind of SPS of WRe/TZM/ graphite to be sintered connection method, using graphite gradient mold, while realizing WRe alloy powder and TZM alloy powder gradient sintering by SPS technology, the dissimilar material joining between TZM alloy powder and graphite block body is realized using titanium foil as intermediate layer, to obtain WRe/TZM/ graphite dissimilar material joining part.Densified sintering product can be obtained in connection method through the invention, the good WRe/TZM/ graphite dissimilar material joining part of uniform, bond strength height, perfect heat-dissipating, thermal-shock resistance is spread at company interface, WRe alloy-layer consistency reaches 98.07%, TZM alloy-layer consistency and reaches 97.98%, uniformly, the connector room temperature side shear strength WRe/TZM is up to 303.9MPa, TZM/ graphite side up to 31.2MPa for joint face diffusion.
Description
Technical field
The present invention relates to a kind of sintering connection methods of dissimilar material, and in particular to a kind of SPS burning of WRe/TZM/ graphite
Tie connection method.
Background technique
WRe alloy is the alloy as composed by W and Re, and W fusing point is high, elevated temperature strength is big, perfect heat-dissipating, atomic number
Height can excite strong x-ray under electron bombardment, but W has notch sensitive effect, be easy to cause the extension of crackle, deepen,
To make target matrix stripping, 500 DEG C of W high of the recrystallization temperature ratio of Re, and Re, there is no mould crisp transition temperature.Therefore, Re
The brittleness at room temperature that can significantly improve W is added, reduces and moulds crisp transition temperature, and can be in the mechanical property of certain high-temperature area enhancing W
Energy.TZM alloy is a kind of molybdenum-base alloy being widely used, and is mainly used in aerospace, power generation, nuclear reactor, army at present
The fields such as thing, medical instrument have high-melting-point, high elastic modulus, strong corrosion resistant, low thermal coefficient of expansion, high heat conductance and excellent
The features such as different mechanical behavior under high temperature.Graphite is a kind of widely used carbon materials, and special structure makes it have high temperature resistant
The performances such as property, good electrical and thermal conductivity, good chemical stability, anti-thermal shock, but graphite material intensity is not high, in modern work
Usually graphite and metal bonding can be got up use in industry, such as heat transfer component of high-power CT machine target, fusion reactor
Deng this composite construction while the excellent properties with graphite and metal.In addition, the density of graphite will be far below general alloy,
Lightweight is one of modern industry probing direction, under the premise of guaranteeing equipment quality, output power can be improved, reduce energy
Consumption, raising service life of equipment etc..
The prior art obtain WRe/TZM/ graphite connector to be realized by multistep, usually first sintering preparation WRe alloy,
TZM alloy, then WRe alloy is connect with TZM alloy diffusion, then by WRe-TZM alloy connector and joining of graphite, technique is multiple
Miscellaneous, higher cost, carrying out every step step by step can all cause alloy surface to be carbonized, and be needed in the next steps through machining removal carbonization
Layer, material loss are serious.
Summary of the invention
The present invention is based on connect at present to WRe alloy powder with TZM sintering alloy powder technology, WRe alloy with TZM alloy
A kind of exploration of technology, TZM alloy and joining of graphite technology, it is desirable to provide SPS sintering connection method of WRe/TZM/ graphite.This
Invention can guarantee that under the premise of densified sintering product, connection are good, a step realizes the sintering connection of WRe/TZM/ graphite, effectively simplifies
Process flow, stock utilization is high, greatly reduces energy consumption.
The present invention connects the solid state sintering that SPS technology is applied to refractory alloy with solid-state diffusion, is made by the way that titanium foil is added
For intermediate layer, to reduce welding temperature, and complete solid solution is formed by atom counterdiffusion in weld seam, and then improve weldering
The mechanical property of connector.
The SPS of WRe/TZM/ graphite of the present invention is sintered connection method, includes the following steps:
Step 1: amount weighs W-5%Re alloy powder and TZM alloy powder raw material according to the ratio；Select with a thickness of 200 μm, it is pure
The titanium foil of degree >=99.0% carries out pickling, ultrasonic cleaning and dries, as intermediate layer；Graphite to be connected is taken, to graphite
Surface to be welded carries out pre-grinding, polishing and ultrasonic cleaning and is dried in vacuo；
Step 2: taking the cavity plate of graphite gradient mold to load onto bushing and push-down head, load weighted TZM powder is first put into stone
It in black mold, is compacted using hand-operated hydraulic press precompressed, then load weighted W-5%Re alloy powder is placed in the TZM powder of compacting
Upside is compacted using hand-operated hydraulic press precompressed, and precompressed parameter is pressure maintaining 2min under 10MPa pressure, push-down head is then removed, by titanium
Foil is placed in the TZM powder side after precompressed, adds graphite block body, finally adds upper push-down head, 10MPa pressure entirety precompressed
2min；In precompressed, the dress sample sequence of sample sequentially consists of graphite block body, titanium foil, TZM alloy-layer, W-5%Re alloy
Layer.
Step 3: the graphite jig equipped with connector to be sintered that step 2 is obtained is placed in discharge plasma sintering system
It in burner hearth, is evacuated to lower than 10Pa, then passes to DC pulse current, carry out gradient sintering connection.
In step 1, graphite to be connected directly is polished, is then cleaned by ultrasonic in alcohol, the graphite handled well is made
Surface to be welded flatness no more than 0.1mm, roughness be not more than 0.1 μm.Density >=1.86g/cm of the graphite3, resist
Roll over intensity >=59.0MPa.
In step 1, the Fisher particle size of the W-5%Re alloy powder is 3~4 μm, the Fei Shi grain of the TZM alloy powder
Degree is 2~3 μm.
In step 1, the pickling is that the dilute hydrochloric acid for the use of volumetric concentration being 5% impregnates titanium foil 10 minutes；The ultrasound
Cleaning is carried out in alcohol.
In step 2, the graphite gradient mold includes cavity plate, bushing, seaming chuck and push-down head.
The cavity plate is the hollow cavity structure of perforation, and the cavity plate is divided into upper and lower two according to the difference of cavity plate wall thickness
Part, top are that high-temperature region lower part is low-temperature space, and during being sintered connection, cavity plate high-temperature region and low-temperature space are in the horizontal direction
Interface be overlapped with the upper surface of TZM alloy-layer, high-temperature region with meet WRe alloy sintering densification temperature, low-temperature space with
Meet the densification of TZM alloy sintering and TZM alloy and the close-connected temperature of graphite block body.The wall thickness of high-temperature region is less than low-temperature space
Wall thickness, the temperature difference of high-temperature region and low-temperature space regulated and controled by wall thickness, passes through the thermometer hole point being arranged in high-temperature region and low-temperature space
Not Ce Liang high-temperature region and low-temperature space temperature.
The bushing is set to the inner surface of the cavity plate hollow cavity, is hollow graphite pipe, for placing WRe alloyed powder
End, TZM alloy powder and graphite block body.Since cavity plate is provided with thermometer hole, high pressure unbalance stress cavity plate easy to damage, bushing can be effective
Avoid this phenomenon.
In assembly, the push-down head plays support out of the cavity plate is inserted into the bottom of the cavity plate hollow cavity
Effect；The seaming chuck is out of, the cavity plate is inserted on the top of the cavity plate hollow cavity, to apply pressure to sample.
Further, the vertical section of the push-down head is in inverted T-type structure, in assembly, the vertical projections portion of inverted T-type structure
Divide out of, the cavity plate is inserted into the bottom of the cavity plate hollow cavity, the lateral part of inverted T-type structure is located at the cavity plate
Lower section is combined closely with cavity plate, plays position-limiting action.
During being sintered connection, when low-temperature space reaches sintering temperature, the temperature difference of high-temperature region and low-temperature space is 200-
220℃。
Above-mentioned all temperature are subject to thermometer hole temperature.
In step 3, gradient sintering Joining Technology parameter setting is as follows:
Axial compressive force: fixed push-down head applies pressure 20-40MPa by seaming chuck；
Heating rate: it is heated up with the heating rate of 20-70 DEG C/min, when low-temperature space reaches 1450~1650 DEG C of sintering temperature
When, stop heating, keeps the temperature 10-60min；
Sintering connection temperature: 1450-1650 DEG C (low-temperature space)；
Rate of temperature fall: the rate of temperature fall that 1000 DEG C of section is down to from connection temperature is 10 DEG C/min, is down to from 1000 DEG C
The rate of temperature fall in 600 DEG C of section is 20 DEG C/min, from 600 DEG C to the furnace cooling of room temperature section；WRe/ is obtained after cooling
TZM/ graphite dissimilar material joining part.
Said welding method condition is groped and is obtained based on univariate Scientific experimental design and many experiments,
With this condition, the comprehensive performance of product is optimal.
Compared with prior art, the beneficial effects of the present invention are embodied in:
1, densified sintering product can be obtained in connection method through the invention, uniform, bond strength height, thermal diffusivity are spread in company interface
The WRe/TZM/ graphite dissimilar material joining part that energy is good, thermal-shock resistance is good.
2, the present invention uses SPS Diffusion Welding technology, have process flow is simple, technological parameter is easy to control, quality is stable,
Strong operability connects the characteristics of temperature is low, low energy consumption, to reduce production cycle and cost.
3, the present invention, can step realization WRe/TZM/ graphite sintering connection by gradient mold.The invention can ensure that burning
Under the premise of knot is fine and close, connection is good, effective simplification of flowsheet greatly reduces energy consumption, reduce the production cycle and at
This.
The WRe/TZM/ graphite composite material obtained through the invention, WRe alloy-layer consistency reach 98.07%, TZM conjunction
Layer gold consistency reaches 97.98%, joint face diffusion uniformly, the connector room temperature side shear strength WRe/TZM up to 303.9MPa,
TZM/ graphite side is up to 31.2MPa., needs of production can be met.
Detailed description of the invention
Fig. 1 and Fig. 2 is gradient mould structure and dress sample schematic diagram.
Figure label: 1 seaming chuck, 2 bushings, 3 cavity plates, 4 thermometer holes, 5 push-down heads, 6WRe alloy-layer, 7TZM alloy-layer,
8Ti foil, 9 graphite block bodies.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention is further explained, but embodiments of the present invention are not
It is only limitted to this.
Discharge plasma sintering furnace used in following embodiments is the LABOX- of Sinter Land inc company, Japan production
6020hv discharge plasma sintering system, current type are DC pulse current, pulse train 40:7；Gradient graphite used
Die bushing internal diameter is Φ 30mm, and gradient mold is divided into upper and lower two parts, and top is divided into high-temperature region, lower part is divided into low-temperature space, ladder
The Wall-Thickness Difference for spending mold high-temperature region and low-temperature space is 10mm, so that high-temperature region and the low-temperature space temperature difference meet WRe alloy and TZM alloy
Sintering densification required temperature and graphite and TZM alloy solid diffusivity temperature.
WRe alloy powder used in following embodiments (W-5%Re alloy powder) is from the limited public affairs of Weihai polycrystalline tungsten science and technology
Department, 3~4 μm of Fisher particle size.
TZM alloy powder used in following embodiments come from Jinduicheng Molybdenum Co., Ltd, 2~3 μm of Fisher particle size.
Block graphite used in following embodiments comes from Japanese East Sea Tan Su Co., Ltd., is the high-strength graphite of trade mark G535.
Following embodiment measured temperatures are on the basis of measuring low-temperature space thermometer hole temperature, high-temperature region thermometer hole subsidiary.
Embodiment 1:
The SPS Diffusion Welding of TZM and graphite dissimilar material carry out as follows in the present embodiment:
1, graphite to be connected is taken, pre-grinding, polishing and ultrasonic cleaning are carried out to the surface to be welded of graphite and is dried in vacuo, is guaranteed
The flatness of the surface to be welded of graphite is not more than 0.1 μm no more than 0.1mm, roughness.
2, pickling 10min in the dilute hydrochloric acid for being 5% as volumetric concentration by titanium foil, is subsequently placed in alcohol and is cleaned by ultrasonic,
Finally it is dried for standby.
3, W-5%Re alloy powder and TZM alloy powder raw material are weighed on demand.
4, graphite cavity plate is taken to load onto bushing and push-down head, successively by load weighted TZM alloy powder, WRe alloy powder
It is put into graphite jig, hand-operated hydraulic press is respectively adopted and carries out precompressed, pressure 10MPa, pressure maintaining 2min then remove pushing
Ti foil is placed in TZM powder side after precompressed, adds graphite block body, finally adds upper push-down head by head, and 10MPa pressure is integrally pre-
Press 2min.
5, the graphite jig equipped with to-be-welded pieces is placed in the burner hearth of discharge plasma sintering system, is evacuated to and is lower than
10Pa then passes to DC pulse current, is sintered Joining Technology are as follows:
Axial compressive force: fixed push-down head applies pressure 30MPa by seaming chuck；
Heating rate: being heated up with the heating rate of 20-70 DEG C/min, when low-temperature space reaches sintering temperature 1450, is stopped
Heating keeps the temperature 30min；
Sintering connection temperature: 1500 DEG C (low-temperature space), 1690 DEG C (high-temperature region)；
Rate of temperature fall: the rate of temperature fall for being down to 1000 DEG C of section from connection temperature is 10 DEG C/min, from connection temperature drop
Rate of temperature fall to 600 DEG C of sections is 20 DEG C/min, from 600 DEG C to the furnace cooling of room temperature section；It obtains after cooling
WRe/TZM/ graphite dissimilar material joining part.
After tested, WRe/TZM/ graphite composite material obtained by this example, WRe alloy-layer consistency reach 94.53%, TZM
Alloy-layer consistency reaches 97.55%, joint face diffusion uniformly, the connector room temperature side shear strength WRe/TZM up to 283.8MPa,
TZM/ graphite side is up to 23.6MPa.
Embodiment 2:
The SPS Diffusion Welding of TZM and graphite dissimilar material carry out as follows in the present embodiment:
1, graphite to be connected is taken, pre-grinding, polishing and ultrasonic cleaning are carried out to the surface to be welded of graphite and is dried in vacuo, is guaranteed
The flatness of the surface to be welded of graphite is not more than 0.1 μm no more than 0.1mm, roughness.
2, pickling 10min in the dilute hydrochloric acid for being 5% as volumetric concentration by titanium foil, is subsequently placed in alcohol and is cleaned by ultrasonic,
Finally it is dried for standby.
3, W-5%Re alloy powder and TZM alloy powder raw material are weighed on demand.
4, graphite cavity plate is taken to load onto bushing and push-down head, successively by load weighted TZM alloy powder, WRe alloy powder
It is put into graphite jig, hand-operated hydraulic press is respectively adopted and carries out precompressed, pressure 10MPa, pressure maintaining 2min then remove pushing
Ti foil is placed in TZM powder side after precompressed, adds graphite block body, finally adds upper push-down head by head, and 10MPa pressure is integrally pre-
Press 2min.
5, the graphite jig equipped with to-be-welded pieces is placed in the burner hearth of discharge plasma sintering system, is evacuated to and is lower than
10Pa then passes to DC pulse current, is sintered Joining Technology are as follows:
Axial compressive force: fixed push-down head applies pressure 30MPa by seaming chuck；
Heating rate: it is heated up with the heating rate of 20-70 DEG C/min, when low-temperature space reaches 1550 DEG C of sintering temperature, is stopped
It only heats up, keeps the temperature 30min；
Sintering connection temperature: 1550 DEG C (low-temperature space), 1780 DEG C (high-temperature region)；
Rate of temperature fall: the rate of temperature fall for being down to 1000 DEG C of section from connection temperature is 10 DEG C/min, from connection temperature drop
Rate of temperature fall to 600 DEG C of sections is 20 DEG C/min, from 600 DEG C to the furnace cooling of room temperature section；It obtains after cooling
WRe/TZM/ graphite dissimilar material joining part.
After tested, WRe/TZM/ graphite composite material obtained by this example, WRe alloy-layer consistency reach 98.07%, TZM
Alloy-layer consistency reaches 97.98%, joint face diffusion uniformly, the connector room temperature side shear strength WRe/TZM up to 303.9MPa,
TZM/ graphite side is up to 31.2MPa.
Embodiment 3:
The SPS Diffusion Welding of TZM and graphite dissimilar material carry out as follows in the present embodiment:
1, graphite to be connected is taken, pre-grinding, polishing and ultrasonic cleaning are carried out to the surface to be welded of graphite and is dried in vacuo, is guaranteed
The flatness of the surface to be welded of graphite is not more than 0.1 μm no more than 0.1mm, roughness.
2, pickling 10min in the dilute hydrochloric acid for being 5% as volumetric concentration by titanium foil, is subsequently placed in alcohol and is cleaned by ultrasonic,
Finally it is dried for standby.
3, W-5%Re alloy powder and TZM alloy powder raw material are weighed on demand.
4, graphite cavity plate is taken to load onto bushing and push-down head, successively by load weighted TZM alloy powder, WRe alloy powder
It is put into graphite jig, hand-operated hydraulic press is respectively adopted and carries out precompressed, pressure 10MPa, pressure maintaining 2min then remove pushing
Ti foil is placed in TZM powder side after precompressed, adds graphite block body, finally adds upper push-down head by head, and 10MPa pressure is integrally pre-
Press 2min.
5, the graphite jig equipped with to-be-welded pieces is placed in the burner hearth of discharge plasma sintering system, is evacuated to and is lower than
10Pa then passes to DC pulse current, is sintered Joining Technology are as follows:
Axial compressive force: fixed push-down head applies pressure 30MPa by seaming chuck；
Heating rate: it is heated up with the heating rate of 20-70 DEG C/min, when low-temperature space reaches 1550 DEG C of sintering temperature, is stopped
It only heats up, keeps the temperature 15min；
Sintering connection temperature: 1550 DEG C (low-temperature space), 1770 DEG C (high-temperature region)；
Rate of temperature fall: the rate of temperature fall for being down to 1000 DEG C of section from connection temperature is 10 DEG C/min, from connection temperature drop
Rate of temperature fall to 600 DEG C of sections is 20 DEG C/min, from 600 DEG C to the furnace cooling of room temperature section；It obtains after cooling
WRe/TZM/ graphite dissimilar material joining part.
After tested, WRe/TZM/ graphite composite material obtained by this example, WRe alloy-layer consistency reach 98.04%, TZM
Alloy-layer consistency reaches 97.82%, joint face diffusion uniformly, the connector room temperature side shear strength WRe/TZM up to 296.0MPa,
TZM/ graphite side is up to 29.9MPa.
Claims (10)
1. a kind of SPS of WRe/TZM/ graphite is sintered connection method, it is characterised in that:
Using graphite gradient mold, while realizing WRe alloy powder and TZM alloy powder gradient sintering by SPS technology, with
Titanium foil realizes the dissimilar material joining between TZM alloy powder and graphite block body as intermediate layer, to obtain WRe/TZM/
Graphite dissimilar material joining part.
2. according to the method described in claim 1, it is characterized by:
The graphite gradient mold includes cavity plate, bushing, seaming chuck and push-down head；
The cavity plate is the hollow cavity structure of perforation, and the cavity plate is divided into upper and lower two parts according to the difference of cavity plate wall thickness,
Top is high-temperature region, and lower part is low-temperature space；During being sintered connection, cavity plate high-temperature region and in the horizontal direction point of low-temperature space
Interface is overlapped with the upper surface of TZM alloy-layer；The wall thickness of high-temperature region is less than the wall thickness of low-temperature space, the temperature of high-temperature region and low-temperature space
Difference is regulated and controled by wall thickness.
3. according to the method described in claim 2, it is characterized by:
Thermometer hole is respectively arranged in high-temperature region and low-temperature space to measure the temperature of high-temperature region and low-temperature space.
4. according to the method described in claim 2, it is characterized by:
The vertical section of the push-down head is in inverted T-type structure, and in assembly, the vertical projections part of inverted T-type structure is from the cavity plate
Bottom be inserted into the hollow cavity of the cavity plate, the lateral part of inverted T-type structure is located at the lower section of the cavity plate, tight with cavity plate
Close combination, plays position-limiting action.
5. according to the method described in claim 2, it is characterized by comprising following steps:
Step 1: amount weighs W-5%Re alloy powder and TZM alloy powder raw material according to the ratio；Select with a thickness of 200 μm, purity >=
99.0% titanium foil carries out pickling, ultrasonic cleaning and dries, as intermediate layer；Graphite to be connected is taken, to the to be welded of graphite
Junction carries out pre-grinding, polishing and ultrasonic cleaning and is dried in vacuo；
Step 2: taking the cavity plate of graphite gradient mold to load onto bushing and push-down head, load weighted TZM powder is first put into graphite mo(u)ld
It in tool, is compacted using hand-operated hydraulic press precompressed, then load weighted W-5%Re alloy powder is placed on the upside of the TZM powder of compacting,
It is compacted using hand-operated hydraulic press precompressed, precompressed parameter is pressure maintaining 2min under 10MPa pressure, then removes push-down head, titanium foil is set
TZM powder side after precompressed, adds graphite block body, finally adds upper push-down head, 10MPa pressure entirety precompressed 2min；?
When precompressed, the dress sample sequence of sample sequentially consists of graphite block body, titanium foil, TZM alloy-layer, W-5%Re alloy-layer；
Step 3: the graphite jig equipped with connector to be sintered that step 2 is obtained is placed in the burner hearth of discharge plasma sintering system
In, it is evacuated to lower than 10Pa, then passes to DC pulse current, carry out gradient sintering connection.
6. according to the method described in claim 5, it is characterized in that
In step 1, graphite to be connected directly is polished, is then cleaned by ultrasonic in alcohol, make the graphite handled well to
The flatness of welding surface is not more than 0.1 μm no more than 0.1mm, roughness；Density >=1.86g/cm of the graphite3, anti-folding is by force
Degree >=59.0MPa.
7. according to the method described in claim 5, it is characterized in that
In 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.
8. according to the method described in claim 5, it is characterized in that
In step 1, the pickling is that the dilute hydrochloric acid for the use of volumetric concentration being 5% impregnates titanium foil 10 minutes；The ultrasonic cleaning
It is to be carried out in alcohol.
9. according to the method described in claim 5, it is characterized in that
In step 3, gradient sintering Joining Technology parameter setting is as follows:
Axial compressive force: fixed push-down head applies pressure 20-40MPa by seaming chuck；
Heating rate: being heated up with the heating rate of 20-70 DEG C/min, when low-temperature space reaches 1450~1650 DEG C of sintering temperature,
Stop heating, keeps the temperature 10-60min；
Sintering connection temperature: 1450-1650 DEG C of low-temperature space；
Rate of temperature fall: the rate of temperature fall that 1000 DEG C of section is down to from connection temperature is 10 DEG C/min, is down to 600 DEG C from 1000 DEG C
The rate of temperature fall in section be 20 DEG C/min, from 600 DEG C to the furnace cooling of room temperature section；WRe/TZM/ stone is obtained after cooling
Black dissimilar material joining part.
10. according to the method described in claim 9, it is characterized by:
During being sintered connection, when low-temperature space reaches sintering temperature, the temperature difference of high-temperature region and low-temperature space is 200-220
℃。
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| CN112091211A (en) * | 2020-08-20 | 2020-12-18 | 上海交通大学 | Preparation method of diffusion multi-element joint |
| CN112958770A (en) * | 2021-02-02 | 2021-06-15 | 合肥工业大学 | Preparation method of WRe/TZM composite material |
| 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 |
| CN115971599A (en) * | 2023-02-16 | 2023-04-18 | 安庆瑞迈特科技有限公司 | Brazing method for improving connection strength of high-capacity rotating target disc for CT bulb tube |
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| CN115971599A (en) * | 2023-02-16 | 2023-04-18 | 安庆瑞迈特科技有限公司 | Brazing method for improving connection strength of high-capacity rotating target disc for CT bulb tube |
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