CN108359872A - A kind of tungsten alloy and preparation method thereof - Google Patents
A kind of tungsten alloy and preparation method thereof Download PDFInfo
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- CN108359872A CN108359872A CN201810255015.0A CN201810255015A CN108359872A CN 108359872 A CN108359872 A CN 108359872A CN 201810255015 A CN201810255015 A CN 201810255015A CN 108359872 A CN108359872 A CN 108359872A
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- 229910001080 W alloy Inorganic materials 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 92
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 48
- 239000010937 tungsten Substances 0.000 claims abstract description 47
- 238000005245 sintering Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 230000008569 process Effects 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000012216 screening Methods 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 22
- 229910052593 corundum Inorganic materials 0.000 claims description 22
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 22
- 239000012188 paraffin wax Substances 0.000 claims description 21
- 238000003825 pressing Methods 0.000 claims description 21
- 239000000654 additive Substances 0.000 claims description 19
- 230000000996 additive effect Effects 0.000 claims description 19
- 229910000831 Steel Inorganic materials 0.000 claims description 17
- 239000010959 steel Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 16
- 239000001993 wax Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 14
- 238000000748 compression moulding Methods 0.000 claims description 13
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000009768 microwave sintering Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 59
- 239000012071 phase Substances 0.000 abstract description 27
- 239000000956 alloy Substances 0.000 abstract description 24
- 239000011230 binding agent Substances 0.000 abstract description 20
- 229910045601 alloy Inorganic materials 0.000 abstract description 14
- 239000007791 liquid phase Substances 0.000 abstract description 9
- 239000007788 liquid Substances 0.000 abstract description 6
- 238000013467 fragmentation Methods 0.000 abstract description 5
- 238000006062 fragmentation reaction Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 5
- 229910000863 Ferronickel Inorganic materials 0.000 abstract description 4
- 238000005728 strengthening Methods 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 239000010439 graphite Substances 0.000 description 10
- 229910002804 graphite Inorganic materials 0.000 description 10
- 229910003271 Ni-Fe Inorganic materials 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 239000011162 core material Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 238000005422 blasting Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910001037 White iron Inorganic materials 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- WIGAYVXYNSVZAV-UHFFFAOYSA-N ac1lavbc Chemical compound [W].[W] WIGAYVXYNSVZAV-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003657 tungsten Chemical class 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- B22F3/24—After-treatment of workpieces or articles
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
-
- 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
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- 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
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
-
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of tungsten alloys and preparation method thereof, are formed by tungsten basal body, Ni powder, Fe powder and Re powder mixed sinterings, and tungsten basal body is W powder, coated composite powder and nickel powder.Include the following steps, wet mixing, drying and screening, mix wax, drying and screening shapes, dewaxing/pre-burning, and sintering is heat-treated after sintering.It is more effective solution strengthening element to add Re, can improve the density of alloy, and keep preferable plasticity.Ferronickel Binder Phase exists with liquid phase in entire sintering process, and hole is completely filled between tungsten particle, and the liquid phase between tungsten particle in hole is formed by capillary force and the liquid matrix mutually VISCOUS FLOW of itself, makes tungsten particle adjustment position, is uniformly distributed again.By the Al for adding different-grain diameter2O3Powder, ensure that reduces tensile strength under the precondition of the certain dynamic compressive strength of tungsten alloy and plasticity, improves the fragility of material, it is ensured that tungsten alloy material forms fragmentation to achieve the purpose that secondary injure after armour-piercing.
Description
Technical field
The present invention relates to technical field of alloy, and in particular to a kind of tungsten alloy and preparation method thereof.
Background technology
Tungsten-bast alloy is especially accounted in national defense industry in the industry in modern times because have many advantages, such as high density, high intensity
According to consequence, with the development of industry, more stringent requirements are proposed to its performance by people.
Armor-piercing bullet requires bullet core material during wearing target by the interaction and the performance characteristics of itself for playing target, automatically
Be broken into mass efficient fragmentation, after armour-piercing formed tapered expansion fragmentation barrage, to improve armor-piercing bullet to armed helicopter, lead
The penetration and secondary damage effectiveness of body and Light armoured vehicle.To ensure the emissive porwer of bullet core material and running through enough
Ability, bullet core material should have sufficiently high dynamic compression strength, while in order to ensure the brokenness of bullet core material, it should have again
There is lower dynamic tensile strength.
Major influence factors for improving tungsten-alloyed white iron self-sharpening energy are the thermal coefficient and Binder Phase of material
Performance, since the Adiabatic Shear of material occurs from material in the narrow zone of shearing strain high concentration, and in alloy
The property of tungsten particle does not allow malleable, so to make material " from sharp " phenomenon occur, it can setting from change Binder Phase
Meter achievees the purpose that improve tungsten alloy self-sharpening.
The patent No. 200810030663.2, a kind of grain-refining W-Ni-Fe alloy preparation method containing rare earth, using solubility
Ultra-fine/nanometer W-Ni-Fe composite powders of tungsten salt, soluble nickel salt, soluble iron salt crystal, trace soluble Rare Earth Y, La or Ce
End, W in composite powder：88-97wt%, rare earth oxide 0.02-0.8wt%, remaining is Ni and Fe.Composite powder is pressed into
Shape is prepared into high-performance fine grain containing trace rare-earth W-Ni- after solid phase and liquid phase two-step sintering in reducing atmosphere after pre-burning
Fe alloys.The deficiency of the present invention is：（1）The compression strength of the grain-refining W-Ni-Fe alloy containing trace rare-earth is relatively low, as armor-piercing bullet
The material for preparing be not easy to realize secondary blasting；（2）The tensile strength of the grain-refining W-Ni-Fe alloy containing trace rare-earth is in 1000-
1300MPa, the armor-piercing bullet more than 1000MPa are the effect that anticipation is not achieved in secondary blasting, caused by later stage explosion
Effect is inadequate.
Invention content
In order to solve the problems of the above-mentioned prior art, it is an object of the invention to propose a kind of tungsten alloy and its preparation
Method.
A kind of tungsten alloy, which is characterized in that following components composition in percentage by weight：
Ni powder 1.1%-1.3%
Fe powder 1.1%-1.4%
Re0.8%-1.0%
Tungsten basal body 96.3%-97%.
In this tungsten alloy of the present invention, the preparation method of the tungsten basal body is reduction method, and Fisher particle size is 3.0 μm,
Purity is 99.9%.
In this tungsten alloy of the present invention, the preparation method of the Ni powder is carbonyl process, and Fisher particle size is 3.66 μm, pure
Degree is 99.5%.
In this tungsten alloy of the present invention, the preparation method of the Fe powder is carbonyl process, and Fisher particle size is 3.97 μm, pure
Degree is 99.3%.
In this tungsten alloy of the present invention, the preparation method of the Re powder is hydrogen reduction method, and Fisher particle size is 3.54 μm,
Purity is 99.99%.
In this tungsten alloy of the present invention, the tungsten basal body, which is W powder, coated composite powder and nickel powder composition, the coated composite powder, is
For preparing the steel alloy of comminuted steel shot, the main component of the coated composite powder is Fe, Si and Mn.
The present invention also provides a kind of preparation methods of tungsten alloy, include the following steps：
Step 1: wet mixing：According to weight percent tungsten basal body 96.3%-97%, Ni powder 1.1%-1.3%, Fe powder 1.1%-1.4%,
Al is added according to the 3% of weight ratio in the powder mixed by Re0.8%-1.0%2O3, remix to be put into three-dimensional mixer and be mixed
It closing, then the ball milling in steel ball grinding cylinder, ball-milling medium is absolute alcohol, and ball milling is sintered carbide ball with ball, ratio of grinding media to material 2: 1,
Ball-milling Time is 8h-12h, rotating speed 200r-350r/min；
Step 2: drying and screening：The good slurry of wet mixing in step 1 is dried in vacuum drying chamber, drying temperature is
100-120 DEG C, drying time 2h, 80 mesh sieve is crossed after dry；
Step 3: mixing wax：Additive selects paraffin gasoline solution, and solution is prepared with the molten 10g paraffin of 50ml gasoline, when additive amount
100g raw material powder mixes paraffin 2g；
Step 4: drying and screening：It mixes wax and will produce the agglomerating phenomenon of raw material powder bonding in the process, and impurity may be introduced, therefore to mixing
Material after wax is dried, and crosses the sieve of 80 mesh；
Step 5: forming：Using common mould compression moulding, the powder mixture in step 4 is pressed into steel pressing mold
Shape, forming pressing pressure are 150-200MPa, and pressing mode is unidirectional compacting；
Step 6: dewaxing/pre-burning：Dewaxing/pre-burning is in H2Reduction furnace in carry out；
Step 7: sintering：Sintering uses microwave sintering or discharge plasma sintering；
Step 8: being heat-treated after sintering：Using vacuum annealing process or solution hardening technique, the tungsten alloy is obtained.
In the preparation method of this tungsten alloy of the present invention, the vacuum annealing process heating rate of the step 8 is 10
DEG C/min, 1150-1250 DEG C keeps the temperature furnace cooling after 2h-4h, vacuum degree 0.5-5Pa.
In the preparation method of this tungsten alloy of the present invention, solution hardening technique is to be protected in argon gas in the step 8
Download water quenching after 1150 DEG C of -1250 DEG C of heat preservation 2h-4h in molybdenum wire furnace.
In the preparation method of this tungsten alloy of the present invention, the Al2O3A diameter of 0.6 μm, 3 μm and 7 μm.
The beneficial effects of the invention are as follows：（1）, Re close to W in periodic table, addition Re can improve the intensity of tungsten alloy,
The density of tungsten alloy can also be improved simultaneously.It is more effective solution strengthening element to add Re, it is strengthening the conjunction of tungsten base high density
While golden, moreover it is possible to it is a degree of to improve the density of alloy, and keep preferable plasticity.
（2）, work as Al2O3Grain size from when increasing to 7 μm for 0.67 μm, the tensile strength of alloy is respectively 503,555 and
583MPa；Elongation percentage is respectively 7.10%, 7.55% and 8.12%, can obtain Al2O3Grain size it is larger, the tensile strength of tungsten alloy
All declined with elongation percentage.
（3）, with Al2O3The increase of particle diameter, tungsten grain shape is kept not substantially in microwave sintering W-Ni-Fe alloys
Become；With Al2O3The increase of content, Al2O3Interfacial fracture between second phase particles and Binder Phase, tungsten particle gradually increases, tungsten
The average grain diameter of particle continuously decreases.
（4）, tungsten alloy fracture mode be mostly W-W fracture, with Al2O3The increase of graininess, the tensile property meeting of tungsten alloy
There are prodigious decline, tensile strength and elongation percentage also to be declined；In addition, with Al2O3The increase of content, the surrender of tungsten alloy
Intensity is increased, and the compressive property of tungsten alloy is enhanced.
（5）, the Al of different-grain diameter is added in the tungsten alloy2O3Powder prepares a kind of novel fragile tungsten heavy alloy material.
The tungsten alloy reduces tensile strength in the case where ensureing the precondition of certain dynamic compressive strength and plasticity, improves the easy of material
Fragility, it is ensured that tungsten alloy material forms fragmentation to achieve the purpose that secondary injure after armour-piercing.
（6）, tungsten particle is oval or round is evenly distributed in Binder Phase.Since sintering process is plasma discharging
Sintering, ferronickel Binder Phase exists with liquid phase in entire sintering process, and hole is completely filled between tungsten particle, hole between tungsten particle
Liquid phase in gap is formed by capillary force and the liquid matrix mutually VISCOUS FLOW of itself, makes tungsten particle adjustment position, again
It is uniformly distributed.Its Binder Phase is mainly the coated composite powder of powdered alloy steel, and adds nickel element and ferro element, makes the tungsten alloy material
The physical property and mechanical property of material all meet the basic demand as armor-piercing bullet, the tungsten particle average diameter obtained after measured
About between 20-30 μm.
Description of the drawings
Fig. 1 is to add Al in tungsten alloy of the present invention2O3A diameter of 0.67 μm of dynamic compression sample section microscopic structure；
Fig. 2 is to add Al in tungsten alloy of the present invention2O3A diameter of 3 μm of dynamic compression sample section microscopic structure；
Fig. 3 is to add Al in tungsten alloy of the present invention2O3A diameter of 7 μm of dynamic compression sample section microscopic structure；
Fig. 4 is the microstructure picture of tungsten alloy of the present invention；
Fig. 5 is tungsten alloy energy spectral position photo.
Specific implementation mode
The present invention is described further with reference to embodiment.
Tungsten basal body in the present invention is W powder, coated composite powder and nickel powder composition, and coated composite powder is the steel alloy for preparing comminuted steel shot,
The main component of coated composite powder is Fe, Si and Mn.Wherein, the thermal coefficient of Fe is 52W/（m·K）, the thermal coefficient of Si is 84W/
（m·K）, the thermal coefficient of Mn is 7.8W/（m·K）.The preparation of coated composite powder is made using second-rate gas atomization.Tungsten basal body has
Steps are as follows for system work：
Step 1: weighing W powder, coated composite powder and nickel powder according to proportioning, the powder weighed is mixed into 48h in three-dimensional material mixer.
Step 2: the mixed-powder in step 1 is ground with the speed of 200-600r/min under an argon atmosphere, grinding
Time 20-48h, and ethyl alcohol is added, 10-60min is dried under infrared lamp in the powder after grinding.
Step 3: the powder mixed in step 2 is pressed into blank under the pressure of 200MPa-350MPa.
Step 4: the mixed-powder of compression moulding in step 3 is packed into graphite jig, graphite jig is put into liquid
It is sintered in phase sintering stove, it is to be ensured that the center of powder is directed at temperature measuring point, and it is Φ 5- that graphite mo(u)ld, which has densely covered internal diameter,
20, it is separated among powder and graphite jig, graphite jig is put in preformer, two pressure heads above and below graphite jig with carbon paper
Between apply 5-20MPa pressure, then release, complete pre-compaction process, then adjust graphite jig up and down two pressure heads position,
So that powder is placed in the centre position of graphite jig, graphite jig is put into the sintering chamber of sintering furnace, starts to be sintered, sintering pressure
For 20-70MPa, temperature-rise period is to rise to 500 DEG C or so from 20 DEG C in 1min, is then risen to the rate of 0-200 DEG C/min
800-1200 DEG C or so, then 1000-1250 DEG C of sintering temperature is risen to the rate of 0-200 DEG C/min, it is sintered chamber in sintering process
0.0001-0.09Pa is inside remained, after sintering, with sintering furnace temperature natural cooling, then by the tungsten base in graphite jig
Body takes out.
Embodiment one
According to weight percent：
Tungsten basal body 97.8%, Fisher particle size are 3.0 μm, purity 99.9%；
Ni powder 1.1%, Fisher particle size are 3.66 μm, purity 99.5%；
Fe powder 1.1%, Fisher particle size are 3.97 μm, purity 99.3%.
Above-mentioned powder is mixed to be put into three-dimensional mixer and is mixed, then the ball milling in steel ball grinding cylinder, ball-milling medium
For absolute alcohol, ball milling is sintered carbide ball, ratio of grinding media to material 2: 1, Ball-milling Time 10h, rotating speed 300r/min with ball.
The good slurry of wet mixing is dried in vacuum drying chamber, drying temperature is 100-120 DEG C, and drying time is
2h crosses 80 mesh sieve after dry.
Additive is added, additive selects paraffin gasoline solution, and solution, additive amount are prepared with the molten 10g paraffin of 50ml gasoline
When 100g raw material powder mix paraffin 2g.
Drying and screening mixes and will produce raw material powder during wax and bond agglomerating phenomenon, and may introduce impurity, thus to mixing wax after
Material be dried, and cross 80 mesh sieve.
Again with common mould compression moulding, by powder mixture compression moulding in steel pressing mold, forming pressing pressure is
150-200MPa, pressing mode are unidirectional compacting.
In H2Reduction furnace in dewax, sintering use microwave sintering or discharge plasma sintering.The burning of microwave sintering
Junction temperature is low, energy saving, safety non-pollution, heating rate is fast, sintering time is short, homogeneous heating, can realize that spatial selectivity is burnt
Knot.With the raising of sintering temperature, the stomata in alloy, which gradually decreases, even to be eliminated, and W particles are thicker, and crystallite dimension gradually increases
Greatly, and distribution of the W particles in matrix phase becomes more uniformly, and interface binding intensity is also enhanced.
The heating rate of discharge plasma sintering is fast, sintering temperature is relatively low, sintering time is short, institutional framework is controllable, energy saving
Environmental protection, under lower sintering temperature and smaller briquetting pressure it is sinterable go out high performance material.With the raising of sintering temperature, alloy
Macrohardness continue to decline, and bending strength is continuously increased, and discharge plasma sintering can strictly control the same of W grain growths
When, and W/W Connected degrees are reduced as far as possible, the fine grain even nanocrystalline W-Ni-Fe alloys for having high-strength and high ductility performance can be made.
It is heat-treated after sintering：Using vacuum annealing process or solution hardening technique.Vacuum annealing process heating rate is 10
DEG C/min, 1150-1250 DEG C keeps the temperature furnace cooling after 2h-4h, vacuum degree 0.5-5Pa.Solution hardening technique is under protection of argon gas
Carry water quenching after 1150 DEG C of -1250 DEG C of heat preservation 2h-4h in molybdenum wire furnace.
The tensile strength of obtained tungsten alloy, the tungsten alloy is 849MPa, elongation percentage 15.45%.
Embodiment two
According to weight percent：
Tungsten basal body 97%, Fisher particle size are 3.0 μm, purity 99.9%；
Ni powder 1.1%, Fisher particle size are 3.66 μm, purity 99.5%；
Fe powder 1.1%, Fisher particle size are 3.97 μm, purity 99.3%；
Re powder 0.8%, Fisher particle size are 3.54 μm, purity 99.99%.
Above-mentioned powder is mixed to be put into three-dimensional mixer and is mixed, then the ball milling in steel ball grinding cylinder, ball-milling medium
For absolute alcohol, ball milling is sintered carbide ball, ratio of grinding media to material 2: 1, Ball-milling Time 10h, rotating speed 300r/min with ball.
The good slurry of wet mixing is dried in vacuum drying chamber, drying temperature is 100-120 DEG C, and drying time is
2h crosses 80 mesh sieve after dry.
Additive is added, additive selects paraffin gasoline solution, and solution, additive amount are prepared with the molten 10g paraffin of 50ml gasoline
When 100g raw material powder mix paraffin 2g.
Drying and screening mixes and will produce raw material powder during wax and bond agglomerating phenomenon, and may introduce impurity, thus to mixing wax after
Material be dried, and cross 80 mesh sieve.
Again with common mould compression moulding, by powder mixture compression moulding in steel pressing mold, forming pressing pressure is
150-200MPa, pressing mode are unidirectional compacting.
The tensile strength of obtained tungsten alloy, the tungsten alloy is 774MPa, elongation percentage 10.76%.
Embodiment three
According to weight percent：
Tungsten basal body 97%, Fisher particle size are 3.0 μm, purity 99.9%；
Ni powder 1.1%, Fisher particle size are 3.66 μm, purity 99.5%；
Fe powder 1.1%, Fisher particle size are 3.97 μm, purity 99.3%；
Re powder 0.8%, Fisher particle size are 3.54 μm, purity 99.99%.
Al is added according to the 3% of weight ratio in the powder mixed2O3, Al2O3A diameter of 0.67 μm, then by above-mentioned powder
Mixing, which is put into three-dimensional mixer, to be mixed, then the ball milling in steel ball grinding cylinder, ball-milling medium are absolute alcohol, ball milling ball
For sintered carbide ball, ratio of grinding media to material 2: 1, Ball-milling Time 10h, rotating speed 300r/min.
The good slurry of wet mixing is dried in vacuum drying chamber, drying temperature is 100-120 DEG C, and drying time is
2h crosses 80 mesh sieve after dry.
Additive is added, additive selects paraffin gasoline solution, and solution, additive amount are prepared with the molten 10g paraffin of 50ml gasoline
When 100g raw material powder mix paraffin 2g.
Drying and screening mixes and will produce raw material powder during wax and bond agglomerating phenomenon, and may introduce impurity, thus to mixing wax after
Material be dried, and cross 80 mesh sieve.
Again with common mould compression moulding, by powder mixture compression moulding in steel pressing mold, forming pressing pressure is
150-200MPa, pressing mode are unidirectional compacting.
The tensile strength of obtained tungsten alloy, the tungsten alloy is 583MPa, elongation percentage 8.12%.
Example IV
According to weight percent：
Tungsten basal body 97%, Fisher particle size are 3.0 μm, purity 99.9%；
Ni powder 1.1%, Fisher particle size are 3.66 μm, purity 99.5%；
Fe powder 1.1%, Fisher particle size are 3.97 μm, purity 99.3%；
Re powder 0.8%, Fisher particle size are 3.54 μm, purity 99.99%.
Al is added according to the 3% of weight ratio in the powder mixed2O3, Al2O3A diameter of 3 μm, then above-mentioned powder is mixed
Conjunction is put into three-dimensional mixer and is mixed, then the ball milling in steel ball grinding cylinder, and ball-milling medium is absolute alcohol, and ball milling is with ball
Sintered carbide ball, ratio of grinding media to material 2: 1, Ball-milling Time 10h, rotating speed 300r/min.
The good slurry of wet mixing is dried in vacuum drying chamber, drying temperature is 100-120 DEG C, and drying time is
2h crosses 80 mesh sieve after dry.
Additive is added, additive selects paraffin gasoline solution, and solution, additive amount are prepared with the molten 10g paraffin of 50ml gasoline
When 100g raw material powder mix paraffin 2g.
Drying and screening mixes and will produce raw material powder during wax and bond agglomerating phenomenon, and may introduce impurity, thus to mixing wax after
Material be dried, and cross 80 mesh sieve.
Again with common mould compression moulding, by powder mixture compression moulding in steel pressing mold, forming pressing pressure is
150-200MPa, pressing mode are unidirectional compacting.
The tensile strength of obtained tungsten alloy, the tungsten alloy is 555MPa, elongation percentage 7.55%.
Embodiment five
According to weight percent：
Tungsten basal body 97%, Fisher particle size are 3.0 μm, purity 99.9%；
Ni powder 1.1%, Fisher particle size are 3.66 μm, purity 99.5%；
Fe powder 1.1%, Fisher particle size are 3.97 μm, purity 99.3%；
Re powder 0.8%, Fisher particle size are 3.54 μm, purity 99.99%.
Al is added according to the 3% of weight ratio in the powder mixed2O3, Al2O3A diameter of 7 μm, then above-mentioned powder is mixed
Conjunction is put into three-dimensional mixer and is mixed, then the ball milling in steel ball grinding cylinder, and ball-milling medium is absolute alcohol, and ball milling is with ball
Sintered carbide ball, ratio of grinding media to material 2: 1, Ball-milling Time 10h, rotating speed 300r/min.
The good slurry of wet mixing is dried in vacuum drying chamber, drying temperature is 100-120 DEG C, and drying time is
2h crosses 80 mesh sieve after dry.
Additive is added, additive selects paraffin gasoline solution, and solution, additive amount are prepared with the molten 10g paraffin of 50ml gasoline
When 100g raw material powder mix paraffin 2g.
Drying and screening mixes and will produce raw material powder during wax and bond agglomerating phenomenon, and may introduce impurity, thus to mixing wax after
Material be dried, and cross 80 mesh sieve.
Again with common mould compression moulding, by powder mixture compression moulding in steel pressing mold, forming pressing pressure is
150-200MPa, pressing mode are unidirectional compacting.
The tensile strength of obtained tungsten alloy, the tungsten alloy is 503MPa, elongation percentage 7.10%.
Tungsten particle is oval or round is evenly distributed in Binder Phase.Since sintering process is that plasma discharging is burnt
Knot, ferronickel Binder Phase exists with liquid phase in entire sintering process, and hole is completely filled between tungsten particle, hole between tungsten particle
In liquid phase be formed by capillary force and the liquid matrix mutually VISCOUS FLOW of itself, make tungsten particle adjustment position, again
Even distribution.
The corner angle and boss on tungsten particle surface also preferentially dissolve, and small tungsten particle tends to reduce, and surface tends to smooth light
It is sliding；The saturation solubility of big tungsten particle is relatively low, keeps a part of oversaturated tungsten atom in liquid matrix phase heavy in large particle surface
Product is precipitated, and ultimately forms the larger spherical tungsten particle of particle size.
Its Binder Phase is mainly the coated composite powder of powdered alloy steel, and adds nickel element and ferro element, makes the tungsten alloy material
The physical property and mechanical property of material all meet the basic demand as armor-piercing bullet, the tungsten particle average diameter obtained after measured
About between 20-30 μm.
The tungsten alloy material for using this alloy steel material to be prepared as main binding phase, although being shown after dynamic compressive test
The phenomenon that no in micro-assembly robot apparent Adiabatic Shear Bands occur, but tungsten grain deforms, clearly, shows to use
This tungsten alloy material is very favorable as armor-piercing bullet warhead material.
Two white bright spot positions are original powdered alloy steel position in Fig. 4, by matter after powdered alloy steel partial melting
Amount transmission is fused together with ferronickel Binder Phase, and non-diffused part and the part not melted form residual core.May be used also from Fig. 4
To see the black region for there are a large amount of very littles between tungsten particle, hole is turned out to be after energy spectrum analysis.This is because being formed
The Binder Phase of liquid phase is more, it can also be seen that Binder Phase proportion is very big from figure, and the connection between tungsten particle is with tungsten-
Tungsten contact is in the majority, thus has enough liquid phase wetting removal tungsten particles, a large amount of hole is finally formd between tungsten particle.
For EDAX results as shown in figure 5, in liquid sintering process, phase has occurred with the atom in Binder Phase in tungsten atom
Counterdiffusion, but the concentration of three kinds of components has no apparent difference at position 2 and position 3, without apparent concentration gradient, illustrates to close
Golden inside forms relatively uniform Binder Phase.
Comparative example one and embodiment two, data therein for as make armor-piercing bullet material be possible, but
It is that utilize high injury caused by secondary blasting at it be worthless.Embodiment two is prolonged due to being added to Re, tungsten alloy
The rate of stretching is significantly improved, but tensile strength not how many decline.
Comparative example two and embodiment three are compared, due to being added to Re and Al2O3, wherein Re reduces prolonging for tungsten alloy
Stretch rate, the Al of addition2O3Particle distribution is inside Binder Phase, when tungsten alloy is stretched stress, due to Binder Phase plasticity compared with
It is good, it deforms first, stress is then passed into Al2O3On particle；Due to Al2O3The intensity of particle is very high, cannot be with Binder Phase
Occur to coordinate to be plastically deformed, and Al2O3The interface bond strength of particle and Binder Phase is very low, under stress, Al2O3Particle
Micro-crack is germinated in interface between Binder Phase first, and crack propagation makes interfacial separation, ultimately forms Al2O3Particle with it is viscous
Tie the separation fracture of phase.
Comparative example three, example IV and embodiment five, work as Al2O3From when increasing to 7 μm for 0.6 μm, alloy resists grain size
Tensile strength is respectively 583,555 and 503MPa；Elongation percentage is respectively 8.12%, 7.55% and 7.10%.It can obtain with Al2O3Grain
The increase of diameter, the tensile strength and elongation percentage of tungsten alloy are all declined.Such tungsten alloy material can be used as to prepare and wear
First bullet tungsten alloy prepares material,
Tungsten alloy fracture mode is mostly W-W fractures, with Al2O3The tensile property of the increase of graininess, tungsten alloy has very greatly
Decline, tensile strength and elongation percentage are also declined；In addition, with Al2O3The yield strength of the increase of content, tungsten alloy has
Increased, enhances the compressive property of tungsten alloy.And the tungsten alloy is in the premise for ensureing certain dynamic compressive strength and plasticity
Under the conditions of reduce tensile strength, improve the fragility of material, it is ensured that tungsten alloy material forms fragmentation to reach after armour-piercing
To the secondary purpose injured.
In short, the foregoing is merely a prefered embodiment of the invention, it is all according to equivalent change made by scope of the present invention patent
With modification, it should all belong to the covering scope of patent of the present invention.
Claims (10)
1. a kind of tungsten alloy, which is characterized in that following components composition in percentage by weight：
Ni powder 1.1%-1.3%
Fe powder 1.1%-1.4%
Re0.8%-1.0%
Tungsten basal body 96.3%-97%.
2. tungsten alloy according to claim 1, it is characterised in that：The preparation method of the tungsten basal body is reduction method, Fei Shi
Granularity is 3.0 μm, purity 99.9%.
3. tungsten alloy according to claim 1, it is characterised in that：The preparation method of the Ni powder be carbonyl process, Fei Shi
Degree is 3.66 μm, purity 99.5%.
4. tungsten alloy according to claim 1, it is characterised in that：The preparation method of the Fe powder be carbonyl process, Fei Shi
Degree is 3.97 μm, purity 99.3%.
5. tungsten alloy according to claim 1, it is characterised in that：The preparation method of the Re powder is hydrogen reduction method, Fei Shi
Granularity is 3.54 μm, purity 99.99%.
6. tungsten alloy according to claim 1, it is characterised in that：The tungsten basal body is that W powder, coated composite powder and nickel powder form,
The coated composite powder is the steel alloy for preparing comminuted steel shot, and the main component of the coated composite powder is Fe, Si and Mn.
7. a kind of method preparing tungsten alloy, which is characterized in that include the following steps：
Step 1: wet mixing：According to weight percent tungsten basal body 96.3%-97%, Ni powder 1.1%-1.3%, Fe powder 1.1%-1.4%,
Al is added according to the 3% of weight ratio in the powder mixed by Re0.8%-1.0%2O3, remix to be put into three-dimensional mixer and be mixed
It closing, then the ball milling in steel ball grinding cylinder, ball-milling medium is absolute alcohol, and ball milling is sintered carbide ball with ball, ratio of grinding media to material 2: 1,
Ball-milling Time is 8h-12h, rotating speed 200r-350r/min；
Step 2: drying and screening：The good slurry of wet mixing in step 1 is dried in vacuum drying chamber, drying temperature is
100-120 DEG C, drying time 2h, 80 mesh sieve is crossed after dry；
Step 3: mixing wax：Additive selects paraffin gasoline solution, and solution is prepared with the molten 10g paraffin of 50ml gasoline, when additive amount
100g raw material powder mixes paraffin 2g；
Step 4: drying and screening：It mixes wax and will produce the agglomerating phenomenon of raw material powder bonding in the process, and impurity may be introduced, therefore to mixing
Material after wax is dried, and crosses the sieve of 80 mesh；
Step 5: forming：Using common mould compression moulding, the powder mixture in step 4 is pressed into steel pressing mold
Shape, forming pressing pressure are 150-200MPa, and pressing mode is unidirectional compacting；
Step 6: dewaxing/pre-burning：Dewaxing/pre-burning is in H2Reduction furnace in carry out；
Step 7: sintering：Sintering uses microwave sintering or discharge plasma sintering；
Step 8: being heat-treated after sintering：Using vacuum annealing process or solution hardening technique, the tungsten alloy is obtained.
8. the method for preparing tungsten alloy according to claim 7, it is characterised in that：The vacuum annealing process liter of the step 8
Warm speed is 10 DEG C/min, and 1150 DEG C -1250 DEG C keep the temperature furnace cooling after 2h-4h, vacuum degree 0.5-5Pa.
9. the method for preparing tungsten alloy according to claim 7, it is characterised in that：Solution hardening technique is in the step 8
Water quenching after 1150 DEG C of -1250 DEG C of heat preservation 2h-4h in molybdenum wire furnace is carried under protection of argon gas.
10. the method for preparing tungsten alloy according to claim 7, it is characterised in that：The Al2O3A diameter of 0.6 μm, 3 μm
With 7 μm.
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| CN109680173A (en) * | 2019-01-11 | 2019-04-26 | 重庆文理学院 | A kind of preparation method of tungsten tantalum rhenium refractory alloy |
| CN112047794A (en) * | 2020-09-14 | 2020-12-08 | 中北大学 | Anti-sintering treatment method for heavy metal particles |
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| CN109680173A (en) * | 2019-01-11 | 2019-04-26 | 重庆文理学院 | A kind of preparation method of tungsten tantalum rhenium refractory alloy |
| CN109680173B (en) * | 2019-01-11 | 2020-02-07 | 重庆文理学院 | Preparation method of tungsten-tantalum-rhenium refractory alloy |
| CN112047794A (en) * | 2020-09-14 | 2020-12-08 | 中北大学 | Anti-sintering treatment method for heavy metal particles |
| CN112047794B (en) * | 2020-09-14 | 2021-10-15 | 中北大学 | Anti-sintering treatment method for heavy metal particles |
| CN112958770A (en) * | 2021-02-02 | 2021-06-15 | 合肥工业大学 | Preparation method of WRe/TZM composite material |
| CN113462942A (en) * | 2021-07-02 | 2021-10-01 | 西安华力装备科技有限公司 | Preparation method of high-yield tungsten alloy material |
| CN114147233A (en) * | 2022-02-10 | 2022-03-08 | 北京煜鼎增材制造研究院有限公司 | Missile warhead shell and additive manufacturing method thereof |
| CN114147233B (en) * | 2022-02-10 | 2022-04-12 | 北京煜鼎增材制造研究院有限公司 | Missile warhead shell and additive manufacturing method thereof |
| CN117646142A (en) * | 2024-01-30 | 2024-03-05 | 江西翔鹭钨业有限公司 | Nickel-doped tungsten alloy wire and preparation method and application thereof |
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