CN108262483B - SPS sintering connection method for tungsten and molybdenum dissimilar refractory metal - Google Patents
SPS sintering connection method for tungsten and molybdenum dissimilar refractory metal Download PDFInfo
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- CN108262483B CN108262483B CN201810171531.5A CN201810171531A CN108262483B CN 108262483 B CN108262483 B CN 108262483B CN 201810171531 A CN201810171531 A CN 201810171531A CN 108262483 B CN108262483 B CN 108262483B
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 84
- 239000010937 tungsten Substances 0.000 title claims abstract description 84
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000005245 sintering Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000003870 refractory metal Substances 0.000 title claims abstract description 32
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 30
- 239000011733 molybdenum Substances 0.000 title claims abstract description 30
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 34
- 229910002804 graphite Inorganic materials 0.000 claims description 34
- 239000010439 graphite Substances 0.000 claims description 34
- 238000002490 spark plasma sintering Methods 0.000 claims description 34
- 238000004321 preservation Methods 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 17
- HHIQWSQEUZDONT-UHFFFAOYSA-N tungsten Chemical compound [W].[W].[W] HHIQWSQEUZDONT-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 239000000758 substrate Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- 238000009792 diffusion process Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 238000003466 welding Methods 0.000 description 7
- 239000007790 solid phase Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 230000004927 fusion Effects 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000005219 brazing Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004870 electrical engineering Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000001208 nuclear magnetic resonance pulse sequence Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001052 transient effect Effects 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
- 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
-
- 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
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
Abstract
The invention discloses an SPS sintering connection method of tungsten and molybdenum dissimilar refractory metals, which takes blocky tungsten as a matrix and carries out sintering connection on the matrix and molybdenum powder through an SPS technology so as to obtain a connecting piece of the tungsten and molybdenum dissimilar refractory metals. By the connection method, molybdenum powder can be sintered and compacted on a tungsten substrate, and meanwhile, the tungsten and molybdenum metal can be sintered and connected to obtain a high-strength and well-formed connecting piece, and the room-temperature shear strength of the joint can reach 152.9 MPa.
Description
Technical Field
The invention relates to a sintering connection method of dissimilar refractory metals, in particular to a sintering connection method of dissimilar refractory metals of tungsten and molybdenum.
Background
Tungsten has high melting point, high density, high hardness, low thermal expansion coefficient, excellent electric conduction, heat conduction, electron emission and other performances, and has become a key material in high-technology fields such as medical field, weaponry, aerospace, atomic energy, microelectronic information, electrical engineering, machining and the like, for example: in the field of weapons, the device can be used for ultra-high-speed kinetic-energy armor piercing bullets; in the field of nuclear fusion, the plasma-oriented material can be used in a fusion reactor tokomak device; in the medical field, can be used for the rotary target material of a CT machine.
Molybdenum has high mechanical property, good corrosion resistance and processability, and is widely applied to the fields of medical treatment, aviation, aerospace, nuclear energy and the like, such as: the composite material can be used for radiating panels of spacecrafts, nozzles of rocket engines, gas distribution valve bodies bearing high temperature in torpedo engines, perforating heads of seamless stainless steel, furnace walls of high-temperature furnaces, heat shields of hot isostatic pressing machines, electronic tube parts, target materials and the like.
The effective connection of tungsten and molybdenum dissimilar refractory metals is a key for expanding the application of refractory metals in the fields of medical instruments, aerospace, nuclear energy and the like. However, the two materials have great differences in melting point and mechanical properties, so that the connection between the two materials is very difficult. At present, the connection of refractory metals and their alloys is mainly realized by fusion welding, brazing, solid phase diffusion connection and transient liquid phase connection. However, these methods have many disadvantages: it is difficult to make a joint with high bonding strength; the requirements on the surface smoothness of the metal piece and the vacuum degree of equipment are high; the temperature required by solid phase diffusion connection and instant liquid phase connection is high, and the heat preservation time is long, so that the connection between the solid phase diffusion connection and the instant liquid phase connection consumes time and energy, and the recrystallization brittleness is easily generated; cracks are easily generated by fusion welding; brazing, although at lower joining temperatures, is difficult to make joints that can be used at high temperatures because the melting point of the braze is generally low.
The Spark Plasma Sintering (SPS) technique is a new method for rapidly consolidating and forming powder by using a strong pulse direct current to flow through the powder or a die to generate joule heat. In recent years, this method has come to be used in the field of welding, and enables connection of the same material (alloy to alloy, ceramic to ceramic) and a different material (alloy to ceramic). Compared with the traditional solid phase diffusion welding, the SPS solid phase diffusion welding has the advantages of high heating rate and low energy consumption, and particularly, an electric field is introduced into the SPS on the basis of a temperature field and a stress field required by the traditional solid phase diffusion welding. Under the action of an electric field, electromigration effects can accelerate substance diffusion. Therefore, by reasonably setting conditions, the adoption of the SPS technology is expected to realize effective connection of tungsten and molybdenum dissimilar refractory metals at a lower temperature in a shorter time.
Disclosure of Invention
Aiming at the defects of the existing tungsten and molybdenum metal connection technology, the invention aims to apply the SPS technology to the solid diffusion connection of refractory metals and provides a quick and efficient connection method of tungsten and molybdenum dissimilar refractory metals.
The invention adopts the following technical scheme for realizing the purpose:
the invention relates to an SPS sintering connection method of tungsten and molybdenum dissimilar refractory metals, which is characterized in that: the method is characterized in that blocky tungsten is used as a matrix, and the matrix and molybdenum powder are sintered and connected through an SPS technology, so that the connecting piece of tungsten and molybdenum dissimilar refractory metals is obtained. The method specifically comprises the following steps:
step 1,
After ball milling, putting tungsten powder into a die and prepressing, and then putting the die into a hearth of a discharge plasma sintering system for sintering to obtain sintered-state disk-shaped blocky tungsten;
pre-grinding, polishing and ultrasonically cleaning two surfaces of the blocky tungsten, and then putting the blocky tungsten into a vacuum drying oven for drying;
step 2,
Taking a graphite mold, wherein the graphite mold comprises an upper pressure head, a lower pressure head and a graphite female mold;
sequentially placing the blocky tungsten and molybdenum powder treated in the step 1 into a graphite female die from bottom to top, and then tightly pressing the blocky tungsten and molybdenum powder by using an upper pressing head and a lower pressing head, wherein the lengths of the upper pressing head and the lower pressing head exposed out of the graphite female die are the same;
step 3,
Placing a graphite mold filled with a sample to be sintered in a hearth of a spark plasma sintering system, vacuumizing to no more than 10Pa, and then introducing direct current pulse current to sinter and connect tungsten and molybdenum dissimilar refractory metals, wherein the sintering and connecting process comprises the following steps:
the axial pressure is 10-40 MPa,
the temperature rise rate is 70-100 ℃/min,
the connection temperature is 1500-1700 ℃,
the heat preservation time is 15-30 min,
the cooling rate is: the temperature reduction rate of the interval from the connection temperature to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace;
and cooling to obtain the connecting piece of the tungsten and molybdenum dissimilar refractory metals.
Further, in step 1, the sintering conditions are as follows:
the axial pressure is 40MPa,
the temperature rise rate is 70-100 ℃/min,
the sintering temperature is 1900 ℃,
the heat preservation time is 3min,
and cooling to room temperature along with the furnace after the heat preservation is finished.
Further, in step 1, the pre-grinding is performed by using #400, #800, #1000, #1500, and #2000 metallographic sandpaper in this order.
Further, the relative density of the bulk tungsten obtained in step 1 is not less than 97.0% of its theoretical density.
Further, in step 3, the axial pressure is 10MPa when rising from room temperature to 800 ℃ and 40MPa when rising from 800 ℃ to the joining temperature.
Further, in step 3, the temperature rise rate is 100 ℃/min when the temperature rises from room temperature to 600 ℃, and is 70 ℃/min when the temperature rises from 600 ℃ to the connection temperature.
Compared with the prior art, the invention has the beneficial effects that:
1. the method can realize the quick and efficient connection of tungsten and molybdenum dissimilar refractory metals by adopting the SPS technology, and compared with the traditional connection process, the method has the advantages of low connection temperature, short heat preservation time, low energy consumption and low requirement on the vacuum degree of equipment; meanwhile, atom diffusion is promoted through the electromigration effect, and the high-efficiency connection of tungsten and molybdenum dissimilar refractory metals is realized on the premise of not reducing the strength of the material.
2. By the connecting method, tungsten and molybdenum do not need to be sintered into blocks and then welded, and the direct connection of the block tungsten and molybdenum powder can reduce production procedures and reduce cost. Meanwhile, the influence caused by the inconsistent thermal expansion coefficient in the welding of the block body and the block body can be weakened in the connection of the powder and the block body, so that the tungsten and molybdenum dissimilar refractory metal connecting piece with high strength and good molding can be obtained, and the shear strength of the joint at room temperature can reach 152.9 MPa.
3. The invention optimizes the SPS sintering connection process of tungsten and molybdenum dissimilar refractory metals, and can fully exert the advantages of the connection process when the connection temperature and the heat preservation time are respectively preferred to be 1600 ℃ and 15 min.
Detailed Description
The present invention is further illustrated by the following 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-350 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 graphite mold has an inner diameter of phi 20mm and comprises an upper pressure head, a lower pressure head and a graphite female mold.
Example 1
The SPS sintering connection of the tungsten metal and the molybdenum metal is carried out according to the following steps:
step 1,
Carrying out ball milling on tungsten powder with the particle size of 3 mu m (the rotating speed of a ball mill is 400r/min, and the ball milling time is 12 h);
24.2g of tungsten powder after ball milling is weighed, filled into a die and pre-pressed (the pre-pressing pressure is 10MPa), and then the tungsten powder is placed into an SPS furnace chamber for sintering to prepare sintered compact disk-shaped blocky tungsten with the diameter of 20mm and the thickness of 4mm, wherein the relative density of the blocky tungsten is about 98.0 percent of the theoretical density. The sintering conditions are as follows:
the axial pressure is 40MPa,
the heating rate is 70 ℃/min,
the sintering temperature is 1900 ℃,
the heat preservation time is 3min,
and cooling to room temperature along with the furnace after the heat preservation is finished.
Pre-grinding two surfaces of the blocky tungsten (sequentially using #400, #800, #1000, #1500 and #2000 metallographic abrasive paper), polishing and ultrasonically cleaning, and then putting into a vacuum drying oven for drying;
step 2,
Taking a graphite die, sequentially putting the blocky tungsten and molybdenum powder processed in the step (1) into a graphite female die from bottom to top, and then tightly pressing the blocky tungsten and molybdenum powder by using an upper pressing head and a lower pressing head, wherein the lengths of the upper pressing head and the lower pressing head exposed out of the graphite female die are consistent;
step 3,
Placing a graphite mold filled with a sample to be sintered in a hearth of a spark plasma sintering system, vacuumizing to no more than 10Pa, and then introducing direct current pulse current to sinter and connect tungsten and molybdenum dissimilar refractory metals, wherein the sintering and connecting process comprises the following steps:
axial pressure: 10MPa when the temperature is increased from room temperature to 800 ℃, and 40MPa when the temperature is increased from 800 ℃ to the connection temperature;
the heating rate is as follows: 100 ℃/min when the temperature is raised from room temperature to 600 ℃, and 70 ℃/min when the temperature is raised from 600 ℃ to the connection temperature;
connection temperature: 1500 ℃;
and (3) heat preservation time: 15 min;
the cooling rate is: the temperature reduction rate of the interval from the connection temperature to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace;
and cooling to obtain the tungsten metal and molybdenum metal connecting piece. The room temperature shear strength of the joint was tested to be 132.8 MPa.
Example 2
The SPS sintering connection of the tungsten metal and the molybdenum metal is carried out according to the following steps:
step 1,
Carrying out ball milling on tungsten powder with the particle size of 3 mu m (the rotating speed of a ball mill is 400r/min, and the ball milling time is 12 h);
24.2g of tungsten powder after ball milling is weighed, filled into a die and pre-pressed (the pre-pressing pressure is 10MPa), and then the tungsten powder is placed into an SPS furnace chamber for sintering to prepare sintered compact disk-shaped blocky tungsten with the diameter of 20mm and the thickness of 4mm, wherein the relative density of the blocky tungsten is about 98.0 percent of the theoretical density. The sintering conditions are as follows:
the axial pressure is 40MPa,
the heating rate is 70 ℃/min,
the sintering temperature is 1900 ℃,
the heat preservation time is 3min,
and cooling to room temperature along with the furnace after the heat preservation is finished.
Pre-grinding two surfaces of the blocky tungsten (sequentially using #400, #800, #1000, #1500 and #2000 metallographic abrasive paper), polishing and ultrasonically cleaning, and then putting into a vacuum drying oven for drying;
step 2,
Taking a graphite die, sequentially putting the blocky tungsten and molybdenum powder processed in the step (1) into a graphite female die from bottom to top, and then tightly pressing the blocky tungsten and molybdenum powder by using an upper pressing head and a lower pressing head, wherein the lengths of the upper pressing head and the lower pressing head exposed out of the graphite female die are consistent;
step 3,
Placing a graphite mold filled with a sample to be sintered in a hearth of a spark plasma sintering system, vacuumizing to no more than 10Pa, and then introducing direct current pulse current to sinter and connect tungsten and molybdenum dissimilar refractory metals, wherein the sintering and connecting process comprises the following steps:
axial pressure: 10MPa when the temperature is increased from room temperature to 800 ℃, and 40MPa when the temperature is increased from 800 ℃ to the connection temperature;
the heating rate is as follows: 100 ℃/min when the temperature is raised from room temperature to 600 ℃, and 70 ℃/min when the temperature is raised from 600 ℃ to the connection temperature;
connection temperature: 1500 ℃;
and (3) heat preservation time: 30 min;
the cooling rate is: the temperature reduction rate of the interval from the connection temperature to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace;
and cooling to obtain the tungsten metal and molybdenum metal connecting piece. The room temperature shear strength of the joint was tested to be 146.0 MPa.
Example 3
The SPS sintering connection of the tungsten metal and the molybdenum metal is carried out according to the following steps:
step 1,
Carrying out ball milling on tungsten powder with the particle size of 3 mu m (the rotating speed of a ball mill is 400r/min, and the ball milling time is 12 h);
24.2g of tungsten powder after ball milling is weighed, filled into a die and pre-pressed (the pre-pressing pressure is 10MPa), and then the tungsten powder is placed into an SPS furnace chamber for sintering to prepare sintered compact disk-shaped blocky tungsten with the diameter of 20mm and the thickness of 4mm, wherein the relative density of the blocky tungsten is about 98.0 percent of the theoretical density. The sintering conditions are as follows:
the axial pressure is 40MPa,
the heating rate is 70 ℃/min,
the sintering temperature is 1900 ℃,
the heat preservation time is 3min,
and cooling to room temperature along with the furnace after the heat preservation is finished.
Pre-grinding two surfaces of the blocky tungsten (sequentially using #400, #800, #1000, #1500 and #2000 metallographic abrasive paper), polishing and ultrasonically cleaning, and then putting into a vacuum drying oven for drying;
step 2,
Taking a graphite die, sequentially putting the blocky tungsten and molybdenum powder processed in the step (1) into a graphite female die from bottom to top, and then tightly pressing the blocky tungsten and molybdenum powder by using an upper pressing head and a lower pressing head, wherein the lengths of the upper pressing head and the lower pressing head exposed out of the graphite female die are consistent;
step 3,
Placing a graphite mold filled with a sample to be sintered in a hearth of a spark plasma sintering system, vacuumizing to no more than 10Pa, and then introducing direct current pulse current to sinter and connect tungsten and molybdenum dissimilar refractory metals, wherein the sintering and connecting process comprises the following steps:
axial pressure: 10MPa when the temperature is increased from room temperature to 800 ℃, and 40MPa when the temperature is increased from 800 ℃ to the connection temperature;
the heating rate is as follows: 100 ℃/min when the temperature is raised from room temperature to 600 ℃, and 70 ℃/min when the temperature is raised from 600 ℃ to the connection temperature;
connection temperature: 1600 ℃;
and (3) heat preservation time: 15 min;
the cooling rate is: the temperature reduction rate of the interval from the connection temperature to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace;
and cooling to obtain the tungsten metal and molybdenum metal connecting piece. The room temperature shear strength of the joint was tested to be 152.9 MPa.
Example 4
The SPS sintering connection of the tungsten metal and the molybdenum metal is carried out according to the following steps:
step 1,
Carrying out ball milling on tungsten powder with the particle size of 3 mu m (the rotating speed of a ball mill is 400r/min, and the ball milling time is 12 h);
24.2g of tungsten powder after ball milling is weighed, filled into a die and pre-pressed (the pre-pressing pressure is 10MPa), and then the tungsten powder is placed into an SPS furnace chamber for sintering to prepare sintered compact disk-shaped blocky tungsten with the diameter of 20mm and the thickness of 4mm, wherein the relative density of the blocky tungsten is about 98.0 percent of the theoretical density. The sintering conditions are as follows:
the axial pressure is 40MPa,
the heating rate is 70 ℃/min,
the sintering temperature is 1900 ℃,
the heat preservation time is 3min,
and cooling to room temperature along with the furnace after the heat preservation is finished.
Pre-grinding two surfaces of the blocky tungsten (sequentially using #400, #800, #1000, #1500 and #2000 metallographic abrasive paper), polishing and ultrasonically cleaning, and then putting into a vacuum drying oven for drying;
step 2,
Taking a graphite die, sequentially putting the blocky tungsten and molybdenum powder processed in the step (1) into a graphite female die from bottom to top, and then tightly pressing the blocky tungsten and molybdenum powder by using an upper pressing head and a lower pressing head, wherein the lengths of the upper pressing head and the lower pressing head exposed out of the graphite female die are consistent;
step 3,
Placing a graphite mold filled with a sample to be sintered in a hearth of a spark plasma sintering system, vacuumizing to no more than 10Pa, and then introducing direct current pulse current to sinter and connect tungsten and molybdenum dissimilar refractory metals, wherein the sintering and connecting process comprises the following steps:
axial pressure: 10MPa when the temperature is increased from room temperature to 800 ℃, and 40MPa when the temperature is increased from 800 ℃ to the connection temperature;
the heating rate is as follows: 100 ℃/min when the temperature is raised from room temperature to 600 ℃, and 70 ℃/min when the temperature is raised from 600 ℃ to the connection temperature;
connection temperature: 1600 ℃;
and (3) heat preservation time: 30 min;
the cooling rate is: the temperature reduction rate of the interval from the connection temperature to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace;
and cooling to obtain the tungsten metal and molybdenum metal connecting piece. The room temperature shear strength of the joint was tested to be 127.6 MPa.
Example 5
The SPS sintering connection of the tungsten metal and the molybdenum metal is carried out according to the following steps:
step 1,
Carrying out ball milling on tungsten powder with the particle size of 3 mu m (the rotating speed of a ball mill is 400r/min, and the ball milling time is 12 h);
24.2g of tungsten powder after ball milling is weighed, filled into a die and pre-pressed (the pre-pressing pressure is 10MPa), and then the tungsten powder is placed into an SPS furnace chamber for sintering to prepare sintered compact disk-shaped blocky tungsten with the diameter of 20mm and the thickness of 4mm, wherein the relative density of the blocky tungsten is about 98.0 percent of the theoretical density. The sintering conditions are as follows:
the axial pressure is 40MPa,
the heating rate is 70 ℃/min,
the sintering temperature is 1900 ℃,
the heat preservation time is 3min,
and cooling to room temperature along with the furnace after the heat preservation is finished.
Pre-grinding two surfaces of the blocky tungsten (sequentially using #400, #800, #1000, #1500 and #2000 metallographic abrasive paper), polishing and ultrasonically cleaning, and then putting into a vacuum drying oven for drying;
step 2,
Taking a graphite die, sequentially putting the blocky tungsten and molybdenum powder processed in the step (1) into a graphite female die from bottom to top, and then tightly pressing the blocky tungsten and molybdenum powder by using an upper pressing head and a lower pressing head, wherein the lengths of the upper pressing head and the lower pressing head exposed out of the graphite female die are consistent;
step 3,
Placing a graphite mold filled with a sample to be sintered in a hearth of a spark plasma sintering system, vacuumizing to no more than 10Pa, and then introducing direct current pulse current to sinter and connect tungsten and molybdenum dissimilar refractory metals, wherein the sintering and connecting process comprises the following steps:
axial pressure: 10MPa when the temperature is increased from room temperature to 800 ℃, and 40MPa when the temperature is increased from 800 ℃ to the connection temperature;
the heating rate is as follows: 100 ℃/min when the temperature is raised from room temperature to 600 ℃, and 70 ℃/min when the temperature is raised from 600 ℃ to the connection temperature;
connection temperature: 1700 ℃;
and (3) heat preservation time: 15 min;
the cooling rate is: the temperature reduction rate of the interval from the connection temperature to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace;
and cooling to obtain the tungsten metal and molybdenum metal connecting piece. The room temperature shear strength of the joint was tested to be 111.0 MPa.
The present invention is not limited to the above exemplary embodiments, and any modifications, equivalent replacements, and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. An SPS sintering connection method of tungsten and molybdenum dissimilar refractory metals is characterized in that: the method is characterized in that blocky tungsten is used as a matrix, and the matrix and molybdenum powder are sintered and connected through an SPS technology, so that the connecting piece of tungsten and molybdenum dissimilar refractory metals is obtained, and the method comprises the following steps:
step 1,
After ball milling, putting tungsten powder into a die and prepressing, and then putting the die into a hearth of a discharge plasma sintering system for sintering to obtain sintered-state disk-shaped blocky tungsten;
pre-grinding, polishing and ultrasonically cleaning two surfaces of the blocky tungsten, and then putting the blocky tungsten into a vacuum drying oven for drying;
step 2,
Taking a graphite mold, wherein the graphite mold comprises an upper pressure head, a lower pressure head and a graphite female mold;
sequentially placing the blocky tungsten and molybdenum powder treated in the step 1 into a graphite female die from bottom to top, and then tightly pressing the blocky tungsten and molybdenum powder by using an upper pressing head and a lower pressing head, wherein the lengths of the upper pressing head and the lower pressing head exposed out of the graphite female die are the same;
step 3,
Placing a graphite mold filled with a sample to be sintered in a hearth of a spark plasma sintering system, vacuumizing to no more than 10Pa, and then introducing direct current pulse current to sinter and connect tungsten and molybdenum dissimilar refractory metals, wherein the sintering and connecting process comprises the following steps:
the axial pressure is 10MPa when the temperature is increased from room temperature to 800 ℃, and is 40MPa when the temperature is increased from 800 ℃ to the connection temperature;
the heating rate is 100 ℃/min when the temperature is raised from room temperature to 600 ℃, and is 70 ℃/min when the temperature is raised from 600 ℃ to the connection temperature;
the connection temperature is 1500-1700 ℃,
the heat preservation time is 15-30 min,
the cooling rate is: the temperature reduction rate of the interval from the connection temperature to 600 ℃ is 20 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace;
and cooling to obtain the connecting piece of the tungsten and molybdenum dissimilar refractory metals.
2. The method for SPS bonding of tungsten and molybdenum dissimilar refractory metals as claimed in claim 1, wherein: in the step 1, the sintering conditions are as follows:
the axial pressure is 40MPa,
the temperature rise rate is 70-100 ℃/min,
the sintering temperature is 1900 ℃,
the heat preservation time is 3min,
and cooling to room temperature along with the furnace after the heat preservation is finished.
3. The method for SPS bonding of tungsten and molybdenum dissimilar refractory metals as claimed in claim 1, wherein: in step 1, the pre-grinding is performed by using #400, #800, #1000, #1500 and #2000 metallographic sandpaper in sequence.
4. The method for SPS bonding of tungsten and molybdenum dissimilar refractory metals as claimed in claim 1, wherein: the relative density of the bulk tungsten obtained in step 1 is not less than 97.0% of its theoretical density.
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| CN109680173B (en) * | 2019-01-11 | 2020-02-07 | 重庆文理学院 | Preparation method of tungsten-tantalum-rhenium refractory alloy |
| CN111872401B (en) * | 2020-07-30 | 2022-11-08 | 合肥工业大学 | Discharge plasma diffusion bonding method of ODSW/TZM alloy |
| CN113523273B (en) * | 2021-06-17 | 2022-10-21 | 北京科技大学 | Powder metallurgy method for rapidly preparing ultrafine crystal pure tungsten material under multi-field coupling |
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