CN104404282B - Tungsten copper alloy with low tungsten content and preparation method of tungsten copper alloy - Google Patents
Tungsten copper alloy with low tungsten content and preparation method of tungsten copper alloy Download PDFInfo
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- CN104404282B CN104404282B CN201410717402.3A CN201410717402A CN104404282B CN 104404282 B CN104404282 B CN 104404282B CN 201410717402 A CN201410717402 A CN 201410717402A CN 104404282 B CN104404282 B CN 104404282B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 87
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 74
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052721 tungsten Inorganic materials 0.000 title abstract description 11
- 239000010937 tungsten Substances 0.000 title abstract description 11
- 238000007731 hot pressing Methods 0.000 claims abstract description 72
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000011812 mixed powder Substances 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims description 27
- 229910052739 hydrogen Inorganic materials 0.000 claims description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 25
- 238000005245 sintering Methods 0.000 claims description 23
- 238000000137 annealing Methods 0.000 claims description 19
- 238000005098 hot rolling Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 13
- 238000005096 rolling process Methods 0.000 claims description 13
- 238000002203 pretreatment Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000005097 cold rolling Methods 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000001307 helium Substances 0.000 claims description 7
- 229910052734 helium Inorganic materials 0.000 claims description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000005056 compaction Methods 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000000462 isostatic pressing Methods 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 208000031481 Pathologic Constriction Diseases 0.000 claims description 2
- 210000001215 vagina Anatomy 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 2
- 239000010949 copper Substances 0.000 abstract description 17
- 229910052802 copper Inorganic materials 0.000 abstract description 17
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 230000007547 defect Effects 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 238000000280 densification Methods 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910000846 In alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000002360 explosive Substances 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
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention provides a method for preparing a tungsten copper alloy. The preparation method comprises the steps of preparing tungsten and copper mixed powder into a briquet for presintering, and hot-pressing the briquet at a temperature lower than a melting point of copper. The tungsten copper alloy prepared by the preparation method is uniform in texture, high in density, excellent in performance and high in rate of finished products.
Description
Technical field
The invention belongs to alloy field is and in particular to relatively low tungsten-copper alloy of a kind of W content and preparation method thereof.
Background technology
Tungsten-copper alloy is " pseudo-alloy " being made up of the copper of high-melting-point, the tungsten of high rigidity and high connductivity, thermal conductivity.Its tool
There are good resistance to arc erosion, resistance fusion welding, high intensity, high rigidity.Additionally, its heat conduction, electric conductivity and heat are swollen
Swollen coefficient can be designed by adjustment tungsten, copper constituent content.Therefore, tungsten-copper alloy is widely used as electrical contact material, electricity
Welding resistance, spark machined and plasma electrode material, electrothermal alloy and heavy alloy, the military project material of specific use are (as fire
Arrow nozzle, aircraft larynx lining) etc..In addition, tungsten-copper alloy is also used for computer central processing system, the drawing of large scale integrated circuit
The heat sink substrate of the electronic device such as wire frame and solid state microwave pipe.
With the continuous development of new and high technology, tungsten-copper alloy is applied in more fields.Especially in terms of military project, example
As aerospace craft, the medicine cover of tank high explosive anti-tank cartridge, the nozzle increasing journey big gun, material of magnetic artillery track etc..These fields
For tungsten-copper alloy performance requirement considerably beyond the requirement as general contact material.Therefore, improve tungsten-copper composite material
Physical property and processability, produce high performance product, the always focus of Chinese scholars research.
The method preparing tungsten-copper alloy at present is mainly infiltration method, first prepares the porous W skeleton of certain density, intensity,
Oozing in W skeleton again with molten copper liquid, so that copper liquid is packed in W skeleton using capillarity thus forming the compound of densification
Material.Preparation structure is uniform, W skeleton that is good to copper wettability, having a certain amount of interconnected pore is that infiltration method prepares tungsten copper material
The key of material.
For the relatively low tungsten-copper alloy of W content (W content is below 50 weight %), according to conventional infiltration method, difficult
To obtain up-to-standard tungsten-copper alloy.Main reason is that, it is difficult to obtain high-quality W skeleton when tungsten powder content is relatively low
Base.If tungsten powder is mixed with copper powder compacting after ooze copper, still have in the sintered blank obtaining unmanageable constriction zone and
The copper segregation area of large scale.
Prior art also prepares tungsten-copper alloy using high-temperature liquid-phase sintering process, because sintering temperature is very high, sintering time very
Long, therefore sintering character is poor, sintered density relatively low (being only the 90%～95% of solid density), the physics of material, electrically and
Mechanical property still not ideal enough it is impossible to meet use requirement.
Content of the invention
It is an object of the present invention to provide a kind of preparation method of tungsten-copper alloy.
Inventor finds, carries out hot pressing by the temperature below copper fusing point to the pressed compact of tungsten powder and copper powder mixed-powder,
Be obtained in that the tungsten-copper alloy of high-compactness, especially high-compactness, tungsten-copper alloy that W content is relatively low.Overcome tradition molten
Ooze method and the defect of lqiuid phase sintering method.
The present invention provides a kind of preparation method of tungsten-copper alloy, and it comprises the following steps：
(1) pressed compact：By pressed compact after the mix homogeneously of tungsten powder and copper powder；
(2) presintering：The pressed compact that step (1) is obtained carries out presintering, and pre-sintering temperature is preferably 1000～1050 DEG C
(such as 1010 DEG C, 1020 DEG C, 1030 DEG C or 1040 DEG C), sintering time is preferably 30～120 minutes (such as 50 minutes, 60 points
Clock, 90 minutes, 100 minutes)；
(3) hot pressing：The sintered blank that step (2) is obtained carries out hot pressing, and the temperature of hot pressing is preferably 850～1070 DEG C of (examples
As 1000～1070 DEG C), pressure is preferably 2500～4000KN (more preferably 2800～3800KN or 3000～3500KN
Or 3000～3200KN, such as 3100KN, 3150KN or 3180KN), the dwell time is preferably 1-3 minute (such as 2 minutes)；
(4) optionally, the heat-press step of repeat step (3) 2～3 times.
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, the wherein heat of step (3)
Pressure is that the sintered blank first obtaining step (2) is heated to 850～1070 DEG C (such as 1000～1070 DEG C), is incubated 15～60 minutes
After (preferably be incubated 15～40 minutes, such as 20 minutes, 30 minutes, 40 minutes or 50 minutes), be placed on press (for example press or
Hydraulic press) upper pressurization, dwell time preferably 1-3 minute.
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, wherein said tungsten copper
In alloy, W content is 5～50wt% (such as 50wt%, 40wt%, 30wt%, 20wt% or 10wt%).
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, the wherein pressure of step (1)
Base pass through isostatic pressing (such as cold isostatic compaction or hip moulding), preferred isostatic pressed pressure be 100～
300MPa (such as 150MPa, 200MPa, 250MPa or 280MPa).
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, wherein said tungsten powder
Purity >=99.95%, preferably average Fisher particle size is 3～8 microns of tungsten powder；
Preferably, described copper powder is electrolytic copper powder, purity >=99.95% of further preferred copper powder, more preferably copper powder
Granularity be -300 mesh.
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, wherein tungsten powder and copper powder
Mixing before, also to carry out pre-treatment to tungsten powder, to break up the agglomerate of tungsten powder, it is preferred to use air current classifying equipment (such as model
Air current classifying equipment for MQW10) pre-treatment is carried out to tungsten powder.Tungsten powder is carried out with airflow crash staged care be conducive to improving conjunction
The uniformity of gold and compactness.
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, wherein step (3) hot pressing
When, pressurizeed in mould pressed compact being put into monolateral 1～3mm (such as 2mm) gap.
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, wherein step (2) is pre-
The hot pressing of sintering or step (3) is in nonoxidizing atmosphere, such as vacuum, blanket of nitrogen, reducing atmosphere (such as hydrogen or decomposition ammonia)
Or carry out in inert atmosphere (such as argon, helium), carry out presintering preferably in atmosphere of hydrogen, preferably enter in atmosphere of hydrogen
Heating stepses in row hot pressing.
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, the method also includes multiple
The step of sintering, the blank after the hot pressing that step (3) or step (4) are obtained carries out resintering knot, and resintering is tied preferably non-oxide
In atmosphere, such as vacuum, blanket of nitrogen, reducing atmosphere (such as hydrogen or decomposition ammonia) or inert atmosphere (such as argon, helium)
Carry out, resintering junction temperature is preferably 1150～1180 DEG C, temperature retention time is preferably 15～30 minutes (such as 20 minutes, 22 minutes
Or 25 minutes), preferably press blank surface with graphite cake lid during resintering knot.Resintering knot is carried out to the blank after hot pressing, can eliminate
The defect occurring in hot pressing.During resintering knot, blank surface is covered with graphite cake, can prevent hydrogen in stove from washing away and make
Become blank surface defect.
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, the method also include with
In lower step one or more：
I () is surface-treated, preferably surface treatment is selected from one or more of following process：Remove the fine fisssure on surface
Stricture of vagina, removal aoxidize speckle, the rough place of polishing, cut the side bulge producing during hot pressing；
(ii) hot rolling, the temperature of hot rolling be preferably 400～600 DEG C (more preferably 450 DEG C, 480 DEG C, 500 DEG C or
550 DEG C), preferably rolling lower amount every time is 0.5～1.5mm (such as 0.8mm, 1mm, 1.2mm), selects suitable rolling as needed
Number of times (preferably rolls 3～4 times)；
(iii) anneal, annealing temperature is preferably 800～1000 DEG C (preferably 900 DEG C or 950 DEG C), during the insulation of annealing
Between be preferably 30～90 minutes (such as 40～60 minutes)；
(iv) cold rolling, preferably rolling lower amount every time is 0.01～0.5mm, selects suitable rolling number of times as needed.
In the present invention, the purpose of described surface treatment is the defect removing blank surface, makes any surface finish, color one
Cause, for example：The micro-crack polishing off blank surface, the oxidation speckle removing blank surface, polishing blank surface are roughly
Just, cut the side bulge producing during hot pressing.Cutting the side bulge producing during hot pressing can prevent from deforming not in the operation of rolling
All cause edge cracks.
In a preferred embodiment, the preparation method of tungsten-copper alloy of the present invention, specifically includes following step
Suddenly：
A () takes purity >=99.95%, average Fisher particle size is 3 microns of tungsten powder, takes purity >=99.95%, particle mean size
Stand-by for the electrolytic copper powder of -300 mesh；
B () carries out powder pre-treatment with airflow crash classifying equipoment to described tungsten powder, to break up the agglomerate of tungsten powder；
C the tungsten powder broken up that step (b) obtains is mixed homogeneously in powder mixer by () with electrolytic copper powder, mixed
Powder；
D mixed-powder isostatic pressing (such as cold isostatic compaction or hip moulding) that step (c) is obtained by (),
Isostatic pressed pressure 100～300MPa, obtains pressed compact；
E pressed compact that step (d) is obtained by () is in nonoxidizing atmosphere, such as vacuum, blanket of nitrogen, reducing atmosphere (such as hydrogen
Gas or decompose ammonia) or inert atmosphere (such as argon, helium) in carry out presintering, pre-sintering temperature be 1000～1050 DEG C, burn
The knot time is preferably 30～120 minutes, cools to room temperature with the furnace, obtains sintered blank；
F sintered blank that step (e) is obtained by () is in nonoxidizing atmosphere, such as vacuum, blanket of nitrogen, reducing atmosphere (for example
Hydrogen or decompose ammonia) or inert atmosphere (such as argon, helium) in be heated to 850～1070 DEG C, insulation 20～60 minutes after, take
Go out to be placed directly in hot pressing on hydraulic press, pressure 2500～4000KN, pressurize 1～3 minute, the pressed compact of heating can be put into during hot pressing
In the mould in monolateral 2mm gap, split with reducing the side producing in hot pressing；
(g) repeat step (f) 1～3 time (preferably 2～3 times)；
Blank after h hot pressing that step (g) is obtained by () is in nonoxidizing atmosphere, such as vacuum, blanket of nitrogen, reducing atmosphere
Carry out resintering knot, resintering junction temperature 1150～1180 in (such as hydrogen or decomposition ammonia) or inert atmosphere (such as argon, helium)
DEG C, sintering time 15～30min, blank upper surface graphite cake is pushed down；
Blank after i resintering knot that step (h) is obtained by () is surface-treated, and preferably surface treatment is selected from following place
One or more of reason：Remove the micro-crack on surface, remove oxidation speckle, the rough place of polishing, cut and produce during hot pressing
Raw side bulge；
Blank after j surface treated that step (i) is obtained by () is rolled, 500 DEG C of hot rollings, rolls lower amount every time and is
0.5～1.5mm, Repeat-heating rolls 3～4 times；
Blank after k hot rolling that step (j) is obtained by () is made annealing treatment, 800 DEG C of annealing temperature；
(l) the annealing blank that step (k) obtains is carried out cold rolling, roll every time lower amount be 0.01-0.5mm, repeatedly roll
System, is rolled to desired thickness.
The present invention also provides a kind of tungsten-copper alloy, is prepared by the preparation method of tungsten-copper alloy of the present invention.By
The relative density of the tungsten-copper alloy that the preparation method of tungsten-copper alloy of the present invention prepares is more than 98%.
Herein, the "-" number before mesh number represents the screen cloth of " passing through " described mesh number.For example, " -300 mesh " represents logical
Cross the screen cloth of 300 mesh, particle mean size is that the electrolytic copper powder of -300 mesh represents that this electrolytic copper powder all can pass through the sieve of 300 mesh
Net.
Beneficial effects of the present invention：
The invention provides a kind of method preparing tungsten-copper alloy, particularly a kind of W content is 5wt%～50wt%'s
The preparation method of low W content tungsten-copper alloy, the briquet that this preparation method is first made to tungsten powder and copper powder mixed-powder carries out pre-burning
Knot, then carries out hot pressing using the temperature less than copper fusing point to briquet, to ensure all even densification of its tissue.Using the present invention
The relatively low tungsten-copper alloy even tissue of W content of preparation method preparation, consistency height, function admirable, high yield rate.
The method of the present invention directly by pressed compact after the mix homogeneously of tungsten powder and copper powder, directly prepares tungsten copper according to product requirement
Component content, need not ooze copper in down-stream.
Additionally, the present invention is before the mixing of tungsten powder and copper powder, pre-treatment is carried out to tungsten powder, (excellent with the agglomerate of breaing up tungsten powder
Choosing carries out pre-treatment using air current classifying equipment to tungsten powder), thus obtaining even-grained tungsten powder.Using this even-grained tungsten
After powder is mixed with copper powder, the tungsten-copper alloy even tissue that sintered, hot pressing obtains, compactness are high, are substantially free of chi inside alloy
The very little continuous accumulation regions of wolfram element being more than 100 μm.
Brief description
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the application, this
Bright schematic description and description is used for explaining the present invention, does not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 and Fig. 2 be respectively embodiment 1 preparation tungsten-copper alloy surface is polished and metallograph after corroding, in figure
Graininess region is tungsten, and back end region is copper.
Specific embodiment
Below by drawings and Examples, technical scheme is described in further detail.
Embodiment 1：W content is 50wt%, the preparation of the tungsten-copper alloy (W50Cu50) for 50wt% for the copper content
Preparation method comprises the steps：
(1) take purity >=99.95%, average Fisher particle size is 5 microns of tungsten powder, takes purity >=99.95%, particle mean size
Stand-by for the electrolytic copper powder of -300 mesh；
(2) powder pre-treatment is carried out to described tungsten powder with airflow crash classifying equipoment (unit type MQW10), to break up tungsten
The agglomerate of powder；
(3) tungsten powder broken up obtaining step (2) is mixed homogeneously in powder mixer with electrolytic copper powder, is mixed
Powder；
(4) the mixed-powder cold isostatic compaction that step (3) is obtained, isostatic pressed pressure 300MPa, obtain pressed compact, pressed compact
Thick 20mm；
(5) pressed compact that step (4) obtains is carried out presintering in logical hydrogen resistance furnace, pre-sintering temperature is 1050 DEG C, burn
The knot time is 120 minutes, is down to room temperature with stove, obtains sintered blank；
(6) sintered blank that step (5) obtains is heated in logical hydrogen resistance furnace, be heated to 1070 DEG C, after being incubated 30 minutes,
Taking-up is placed directly in the upper hot pressing of hydraulic press (FS32-315), pressure 3150KN, pressurize 3 minutes.Can be by the pressed compact of heating during hot pressing
Put in the mould in monolateral 2mm gap, split with reducing the side producing in hot pressing；
(7) pressed compact after the hot pressing obtaining step (6), puts back in logical hydrogen resistance furnace, is heated to 1070 DEG C and is incubated 20 points
Zhong Hou, takes out and is placed directly in hydraulic press hot pressing, pressure 3150KN, pressurize 3 minutes again.The pressed compact of heating can be put into during hot pressing
In the mould in monolateral 2mm gap, it is allowed to densification, obtaining pressed compact thickness is 12mm；
(8) pressed compact after the hot pressing obtaining step (7) carries out resintering knot, to reduce hot pressing in logical hydrogen resistance furnace
The internal flaw of middle appearance, 1180 DEG C of resintering junction temperature, sintering time 20min, pressed compact upper surface graphite cake is pushed down, and prevents stove
Middle hydrogen washes away and causes pressed compact surface defect；
(9) pressed compact after the resintering knot obtaining step (8) is surface-treated, and the defect on pressed compact surface is ground off, example
As polished off micro-crack, oxidation speckle, rough place etc., make any surface finish, solid colour, and the side that will produce during hot pressing
Face bulge cuts, and is not respectively formed edge cracks to prevent from deforming in the operation of rolling；
(10) pressed compact after the surface treated obtaining step (9) is rolled, 500 DEG C of hot rollings, rolls lower amount every time
For 1mm, little roll lower amount, multi-pass, Repeat-heating rolls, and is rolled to 5mm；
(11) pressed compact after the hot rolling obtaining step (10) is made annealing treatment, 900 DEG C of annealing temperature, and temperature retention time is
60 minutes；
(12) the annealing pressed compact that step (11) is obtained carry out cold rolling, every time roll lower amount be 0.2-0.5mm, light reduction
Multi- pass rolling, is rolled to 1.5mm, obtains the tungsten-copper alloy of the present embodiment.
Tungsten-copper alloy prepared by embodiment 1 carries out surface and polishes and corrode, and in diverse location sampling, metallograph is respectively
As depicted in figs. 1 and 2, wherein graininess region is tungsten, and back end region is copper.From Fig. 1 and Fig. 2, the tungsten of present invention preparation
Uniformly, consistency is high for copper alloy metallographic structure, and condition is good, is substantially free of the continuous accumulation regions of wolfram element that size is more than 100 μm.
Embodiment 2：W content is 30wt%, the preparation of the tungsten-copper alloy (W30Cu70) for 70wt% for the copper content
Preparation method comprises the steps：
(1) take purity >=99.95%, average Fisher particle size is 8 microns of tungsten powder, takes purity >=99.95%, particle mean size
Stand-by for the electrolytic copper powder of -300 mesh；
(2) powder pre-treatment is carried out to described tungsten powder with airflow crash classifying equipoment (unit type MQW10), to break up tungsten
The agglomerate of powder；
(3) tungsten powder broken up obtaining step (2) is mixed homogeneously in powder mixer with electrolytic copper powder, is mixed
Powder；
(4) the mixed-powder cold isostatic compaction that step (3) is obtained, isostatic pressed pressure 200MPa, obtain pressed compact, pressed compact
Thick 20mm；
(5) pressed compact that step (4) obtains is carried out presintering in logical hydrogen resistance furnace, pre-sintering temperature is 1030 DEG C, burn
The knot time is 60 minutes, cools to room temperature with the furnace, obtains sintered blank；
(6) sintered blank that step (5) obtains is heated in logical hydrogen resistance furnace, be heated to 1000 DEG C, after being incubated 30 minutes,
Taking-up is placed directly in the upper hot pressing of hydraulic press (FS32-315), pressure 3150KN, pressurize 2 minutes.Can be by the pressed compact of heating during hot pressing
Put in the mould in monolateral 2mm gap, split with reducing the side producing in hot pressing；
(7) pressed compact after the hot pressing obtaining step (6) is put back in logical hydrogen resistance furnace, after 1000 DEG C of insulations 20 minutes,
Take out and be placed directly in hot pressing on hydraulic press, pressure 3150KN, pressurize 2 minutes again.The pressed compact of heating can be put into list during hot pressing
In the mould in side 2mm gap, it is allowed to densification, obtaining pressed compact thickness is 12mm；
(8) pressed compact after the hot pressing obtaining step (7) carries out resintering knot, to reduce hot pressing in logical hydrogen resistance furnace
The internal flaw of middle appearance, 1160 DEG C of resintering junction temperature, sintering time 20min, pressed compact upper surface graphite cake is pushed down, and prevents stove
Middle hydrogen washes away and causes pressed compact surface defect；
(9) pressed compact after the resintering knot obtaining step (8) is surface-treated, and the defect on pressed compact surface is ground off, example
As polished off micro-crack, oxidation speckle, rough place etc., make any surface finish, solid colour, and the side that will produce during hot pressing
Face bulge cuts, and is not respectively formed edge cracks to prevent from deforming in the operation of rolling；
(10) pressed compact after the surface treated obtaining step (9) is rolled, 500 DEG C of hot rollings, rolls lower amount every time
For 1mm, little roll lower amount, multi-pass, Repeat-heating rolls, and is rolled to 5mm；
(11) pressed compact after the hot rolling obtaining step (10) is made annealing treatment, 900 DEG C of annealing temperature, temperature retention time 40
Minute；
(12) the annealing pressed compact that step (11) is obtained carry out cold rolling, every time roll lower amount be 0.05-0.5mm, little pressure
Amount multi- pass rolling, is rolled to 0.5mm, obtains the tungsten-copper alloy of the present embodiment.
Embodiment 3：W content is 10wt%, the preparation of the tungsten-copper alloy (W10Cu90) for 90wt% for the copper content
Preparation method comprises the steps：
(1) take purity >=99.95%, average Fisher particle size is 3 microns of tungsten powder, takes purity >=99.95%, particle mean size
Stand-by for the electrolytic copper powder of -300 mesh；
(2) powder pre-treatment is carried out to described tungsten powder with airflow crash classifying equipoment (unit type MQW10), to break up tungsten
The agglomerate of powder；
(3) tungsten powder broken up obtaining step (2) is mixed homogeneously in powder mixer with electrolytic copper powder, is mixed
Powder；
(4) the mixed-powder cold isostatic compaction that step (3) is obtained, isostatic pressed pressure 100MPa, obtain pressed compact, pressed compact
Thick 20mm；
(5) pressed compact that step (4) obtains is carried out presintering in logical hydrogen resistance furnace, pre-sintering temperature is 1000 DEG C, burn
The knot time is 30 minutes, cools to room temperature with the furnace, obtains sintered blank；
(6) sintered blank that step (5) obtains is heated in logical hydrogen resistance furnace, be heated to 850 DEG C, after being incubated 30 minutes,
Taking-up is placed directly in the upper hot pressing of hydraulic press (FS32-315), pressure 3150KN, pressurize 3 minutes.Can be by the pressed compact of heating during hot pressing
Put in the mould in monolateral 2mm gap, split with reducing the side producing in hot pressing；
(7) pressed compact after the hot pressing obtaining step (6), puts back in logical hydrogen resistance furnace, is incubated 20 minutes at 850 DEG C, so
After take out and be placed directly in hydraulic press hot pressing again, pressure 3150KN, pressurize 2 minutes.During hot pressing, the pressed compact of heating is put into monolateral
In the mould in 2mm gap, it is allowed to densification, obtaining pressed compact thickness is 12mm；
(8) pressed compact after the hot pressing obtaining step (7) carries out resintering knot, to reduce hot pressing in logical hydrogen resistance furnace
The internal flaw of middle appearance, 1150 DEG C of resintering junction temperature, sintering time 20min, pressed compact upper surface graphite cake is pushed down, and prevents stove
Middle hydrogen washes away and causes pressed compact surface defect；
(9) pressed compact after the resintering knot obtaining step (8) is surface-treated, and the defect on pressed compact surface is ground off, example
As polished off micro-crack, oxidation speckle, rough place etc., make any surface finish, solid colour, and the side that will produce during hot pressing
Face bulge cuts, and is not respectively formed edge cracks to prevent from deforming in the operation of rolling；
(10) pressed compact after the surface treated obtaining step (9) is rolled, 500 DEG C of hot rollings, rolls lower amount every time
For 1mm, little roll lower amount, multi-pass, Repeat-heating rolls, and is rolled to 5mm；
(11) pressed compact after the hot rolling obtaining step (10) is made annealing treatment, 800 DEG C of annealing temperature, temperature retention time 30
Minute；
(12) the annealing pressed compact that step (11) is obtained carry out cold rolling, every time roll lower amount be 0.01-0.5mm, little pressure
Amount multi- pass rolling, is rolled to 0.1mm, obtains the tungsten-copper alloy of the present embodiment.
By standard GB/T/T 1423-1996, the density of tungsten-copper alloy prepared by embodiment 1～3 is measured, then
Calculate relative density (ratio of actual density and solid density), concrete numerical value is as shown in the table.
Finally it should be noted that：Above example is only not intended to limit in order to technical scheme to be described；To the greatest extent
Pipe has been described in detail to the present invention with reference to preferred embodiment, and those of ordinary skill in the art should be understood：Still
The specific embodiment of the present invention can be modified or equivalent is carried out to some technical characteristics；Without deviating from this
The spirit of bright technical scheme, it all should be covered in the middle of the technical scheme scope that the present invention is claimed.
Claims (56)
1. a kind of preparation method of tungsten-copper alloy, it comprises the following steps：
(1) pressed compact：By pressed compact after tungsten powder and copper powder mix homogeneously；
(2) presintering：The pressed compact that step (1) is obtained carries out presintering, and pre-sintering temperature is 1000～1050 DEG C；
(3) hot pressing：The sintered blank that step (2) is obtained carries out hot pressing, and the temperature of hot pressing is 850～1070 DEG C；
(4) optionally, the heat-press step of repeat step (3) 2～3 times；
The step that the method also includes resintering knot, the blank after the hot pressing that step (3) or step (4) are obtained carries out resintering knot,
Resintering junction temperature is 1150～1180 DEG C, and temperature retention time is 15～30 minutes；
In described tungsten-copper alloy, W content is 5～50wt%.
2. the preparation method of the tungsten-copper alloy of claim 1, wherein, the sintering time of step (2) presintering is 30～120 points
Clock.
3. the preparation method of the tungsten-copper alloy of claim 1, wherein, the temperature of step (3) hot pressing is 1000～1070 DEG C.
4. the preparation method of the tungsten-copper alloy of claim 1, wherein, the pressure of step (3) hot pressing is 2500～4000KN.
5. the preparation method of the tungsten-copper alloy of claim 1, wherein, the pressure of step (3) hot pressing is 2800～3800KN.
6. the preparation method of the tungsten-copper alloy of claim 1, wherein, the pressure of step (3) hot pressing is 3000～3500KN.
7. the preparation method of the tungsten-copper alloy of claim 1, wherein, the pressure of step (3) hot pressing is 3000～3200KN.
8. the preparation method of the tungsten-copper alloy of claim 1, wherein, the dwell time of step (3) hot pressing is 1-3 minute.
9. the preparation method of the tungsten-copper alloy of claim 1, wherein, the dwell time of step (3) hot pressing is 2 minutes.
10. the preparation method of any one of claim 1～9, the hot pressing of wherein step (3) is the sintering first obtaining step (2)
Base is heated to 850～1070 DEG C, after being incubated 15～60 minutes, is placed on pressurization on press.
The hot pressing of the preparation method of 11. claim 10, wherein step (3) is that the sintered blank first obtaining step (2) is heated to
1000～1070 DEG C, after being incubated 15～60 minutes, it is placed on pressurization on press.
The hot pressing of the preparation method of 12. claim 10, wherein step (3) is that the sintered blank first obtaining step (2) is heated to
850～1070 DEG C, after being incubated 15～40 minutes, it is placed on pressurization on press.
The hot pressing of the preparation method of 13. claim 10, wherein step (3) is that the sintered blank first obtaining step (2) is heated to
850～1070 DEG C, insulation 20 minutes, 30 minutes, 40 minutes or after 50 minutes, it is placed on pressurization on press.
The preparation method of 14. claim 10, described press is press or hydraulic press.
The preparation method of 15. claim 10, wherein, the dwell time being placed on pressurization on press is 1-3 minute.
The preparation method of 16. any one of claim 1～9, in wherein said tungsten-copper alloy, W content is 5～40wt%.
The preparation method of 17. any one of claim 1～9, in wherein said tungsten-copper alloy, W content is 5～30wt%.
The preparation method of 18. any one of claim 1～9, in wherein said tungsten-copper alloy, W content is 5～20wt%.
The preparation method of 19. any one of claim 1～9, in wherein said tungsten-copper alloy, W content is 5～10wt%.
The preparation method of 20. any one of claim 1-9, the wherein pressed compact of step (1) pass through isostatic pressing.
The preparation method of 21. claim 20, described isostatic pressing is cold isostatic compaction or hip moulding.
The preparation method of 22. claim 20, wherein isostatic pressed pressure are 100～300MPa.
The preparation method of 23. claim 20, wherein isostatic pressed pressure are 150MPa, 200MPa, 250MPa or 280MPa.
The preparation method of 24. any one of claim 1-9, purity >=99.95% of wherein said tungsten powder.
The preparation method of 25. claim 24, tungsten powder is the tungsten powder that average Fisher particle size is 3～8 microns.
The preparation method of 26. claim 24, copper powder is electrolytic copper powder.
The preparation method of 27. claim 24, purity >=99.95% of copper powder.
The preparation method of 28. claim 24, the granularity of copper powder is -300 mesh.
Before the preparation method of 29. any one of claim 1-9, the wherein mixing of tungsten powder and copper powder, also to carry out front place to tungsten powder
Reason, to break up the agglomerate of tungsten powder.
Before the mixing of the preparation method of 30. claim 29, wherein tungsten powder and copper powder, also to carry out pre-treatment to tungsten powder, to beat
The agglomerate of scattered tungsten powder, carries out pre-treatment using air current classifying equipment to tungsten powder.
During the preparation method of 31. any one of claim 1-9, wherein step (3) hot pressing, pressed compact is put into monolateral 1～3mm gap
Mould in pressurizeed.
During the preparation method of 32. claim 31, wherein step (3) hot pressing, enter in mould pressed compact being put into monolateral 2mm gap
Row pressurization.
The preparation method of 33. any one of claim 1-9, wherein the hot pressing of the presintering of step (2) or step (3) is non-oxide
Carry out in atmosphere.
The preparation method of the tungsten-copper alloy of 34. claim 33, described nonoxidizing atmosphere is vacuum, blanket of nitrogen, reducing atmosphere
Or inert atmosphere.
The preparation method of the tungsten-copper alloy of 35. claim 34, described reducing atmosphere is hydrogen or decomposes ammonia.
The preparation method of the tungsten-copper alloy of 36. claim 34, described inert atmosphere is argon or helium.
The preparation method of the tungsten-copper alloy of 37. claim 33, carries out presintering in hydrogen atmosphere.
The preparation method of the tungsten-copper alloy of 38. claim 33, carries out the heating stepses in hot pressing in atmosphere of hydrogen.
The preparation method of the tungsten-copper alloy of 39. any one of claim 1-9, is sintered in carrying out in nonoxidizing atmosphere again.
The preparation method of the tungsten-copper alloy of 40. claim 39, described nonoxidizing atmosphere is vacuum, blanket of nitrogen, reducing atmosphere
Or inert atmosphere.
The preparation method of the tungsten-copper alloy of 41. claim 40, described reducing atmosphere is hydrogen or decomposes ammonia.
The preparation method of the tungsten-copper alloy of 42. claim 40, described inert atmosphere is argon or helium.
The preparation method of the tungsten-copper alloy of 43. any one of claim 1-9, the temperature retention time of resintering knot is 20 minutes, 22 minutes
Or 25 minutes.
The preparation method of the tungsten-copper alloy of 44. any one of claim 1-9, presses blank surface with graphite cake lid during resintering knot.
The preparation method of 45. any one of claim 1-9, one or more during the method is further comprising the steps of：
I () is surface-treated；
(ii) hot rolling；
(iii) anneal；
(iv) cold rolling.
The preparation method of 46. claim 45, surface treatment is selected from one or more of following process：Remove the fine fisssure on surface
Stricture of vagina, removal aoxidize speckle, polishing is rough local or cuts the side bulge producing during hot pressing.
The preparation method of 47. claim 45, the temperature of hot rolling is 400～600 DEG C.
The preparation method of 48. claim 45, the temperature of hot rolling is 450 DEG C, 480 DEG C, 500 DEG C or 550 DEG C.
The preparation method of 49. claim 45, the lower amount of rolling every time of hot rolling is 0.5～1.5mm.
The preparation method of 50. claim 45, the lower amount of rolling every time of hot rolling is 0.8mm, 1mm, 1.2mm.
The preparation method of 51. claim 45, annealing temperature is 800～1000 DEG C.
The preparation method of 52. claim 45, annealing temperature is 900 DEG C or 950 DEG C.
The preparation method of 53. claim 45, cold rolling roll every time lower amount be 0.5～1.5mm.
The preparation method of 54. any one of claim 1-9, the method comprises the following steps：
A () takes purity >=99.95%, average Fisher particle size is 3 microns of tungsten powder, takes purity >=99.95%, particle mean size be-
The electrolytic copper powder of 300 mesh is stand-by；
B () carries out powder pre-treatment with airflow crash classifying equipoment to described tungsten powder, to break up the agglomerate of tungsten powder；
C the tungsten powder broken up that step (b) obtains is mixed homogeneously in powder mixer by () with electrolytic copper powder, obtain mixed powder
End；
D mixed-powder isostatic pressing that step (c) is obtained by (), isostatic pressed pressure 100～300MPa, obtain pressed compact；
E the pressed compact that step (d) obtains is carried out presintering in nonoxidizing atmosphere by (), pre-sintering temperature is 1000～1050 DEG C,
Sintering time is 30～120 minutes, cools to room temperature with the furnace, obtains sintered blank；
F the sintered blank that step (e) obtains is heated to 850～1070 DEG C in atmosphere of hydrogen by (), after being incubated 15～60 minutes, take
Go out to be placed directly in hot pressing on hydraulic press, pressure 2500～4000KN, pressurize 1～3 minute, during hot pressing, the pressed compact of heating is put into list
In the mould in side 2mm gap；
(g) repeat step (f) 1～3 time；
Blank after h hot pressing that step (g) is obtained by () carries out resintering knot in nonoxidizing atmosphere, and resintering junction temperature 1150～
1180 DEG C, sintering time 15～30min, blank upper surface graphite cake is pushed down；
Blank after i resintering knot that step (h) is obtained by () is surface-treated, and described surface treatment is selected from following process
One or more：Remove the micro-crack on surface, to remove oxidation speckle, polishing rough local or cut and produce during hot pressing
Side bulge；
Blank after j surface treated that step (i) is obtained by () is rolled, 500 DEG C of hot rollings, roll every time lower amount be 0.5～
1.5mm, Repeat-heating rolls 3～4 times；
Blank after k hot rolling that step (j) is obtained by () is made annealing treatment, 800 DEG C of annealing temperature；
(l) the annealing blank that step (k) obtains is carried out cold rolling, roll every time lower amount be 0.01-0.5mm, repeatedly roll, roll
To desired thickness.
The tungsten-copper alloy that the preparation method of 55. any one of claim 1-54 prepares.
The tungsten-copper alloy of 56. claim 55, its relative density is more than 98%.
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| CN109234597A (en) * | 2018-11-22 | 2019-01-18 | 江苏经纬阀业有限公司 | A kind of tungsten-copper alloy and preparation method thereof |
| CN109609792A (en) * | 2018-12-17 | 2019-04-12 | 河源市凯源硬质合金有限公司 | A method of preparing tungsten-copper alloy |
| CN110885957A (en) * | 2019-12-20 | 2020-03-17 | 西安华山钨制品有限公司 | Process for improving density of tungsten-nickel-copper alloy |
| CN113084166B (en) * | 2021-03-30 | 2023-06-02 | 西安理工大学 | Method for preparing tungsten-copper gradient composite material |
| CN113881864A (en) * | 2021-06-11 | 2022-01-04 | 广东金鑫得新材料有限公司 | Rapid preparation method of high-thermal-conductivity tungsten copper |
| CN113718250A (en) * | 2021-09-02 | 2021-11-30 | 国网江苏省电力有限公司丹阳市供电分公司 | Method for manufacturing tungsten-copper electrical contact material |
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