CN100411779C - Prepn process of composite W-Cu powder for preparing high density alloy - Google Patents
Prepn process of composite W-Cu powder for preparing high density alloy Download PDFInfo
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- CN100411779C CN100411779C CNB2006101247670A CN200610124767A CN100411779C CN 100411779 C CN100411779 C CN 100411779C CN B2006101247670 A CNB2006101247670 A CN B2006101247670A CN 200610124767 A CN200610124767 A CN 200610124767A CN 100411779 C CN100411779 C CN 100411779C
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Abstract
The preparation process of composite W-Cu powder for preparing high density alloy includes the following steps: spray pyrolyzing or spray drying W-Cu material and calcining to prepare composite W-Cu oxide powder of size 0.1-10 micron; and twice reducing the composite W-Cu oxide powder in a multiple atmosphere inclined rotary furnace to obtain composite W-Cu powder. The composite W-Cu powder has the features of adjustable size, homogeneous components, high purity and high dispersivity, and possesses grain size of 50 nm to 1 micron, oxygen content lower than 0.1 wt% and excellent sintering activity. It may be used in preparing high density W-Cu alloy with excellent thermal and mechanical performance.
Description
Technical field
The invention belongs to a kind of preparation method who is used to prepare the composite W-Cu powder of heavy alloy.
Background technology
Two-phase structure's material that tungsten-copper alloy is made up of tungsten (W) and the widely different metal of two physical properties of copper (Cu), its performance changes with the variation of tissue.Tungsten has high fusing point, high density, low thermal coefficient of expansion and high intensity, and copper has good heat conduction, electric conductivity.The fusing point of tungsten and copper differs too big (3380 ℃ of tungsten fusing points, 1083 ℃ of copper fusing points), two kinds of metallic elements are immiscible, the composite that W and Cu form is a kind of typical counterfeit formula alloy, this alloy can be given full play to tungsten, copper intrinsic property separately, mechanical property is preferably arranged, anti-ablative, combination properties such as thermal shock resistance, can be widely used in machinery (spark machined, the electrical contact of welding and electrode etc.), electric power (extra-high voltage contact material, contact material and electrode material, the super-pressure switch of power industry etc.), electronics is (in large scale integrated circuit and the HIGH-POWERED MICROWAVES device, substrate, electronic package material such as connector and heat dissipation element and heat sink material, CPU, the tungsten-copper alloy material of IC microelectric technique, device in the high-tech areas such as electron beam target etc.), metallurgical (finishing rolling mill group oval groove guide and guard etc.), industry (the guide material of magnetic artillery such as military affairs and Aero-Space, the broken first property of medicine cover of high explosive anti-tank cartridge, high accuracy and highdensity weight material, radioactive source is made shielding part, the high temperature resistance combustion gas is ablated and the high-temperature component that washes away etc. in rocket and the guided missile), in the nuclear fusion device towards the divertor material of plasma, traffic fields such as (electric locomotive guide blocks etc.).
The preparation of conventional tungsten copper alloy generally adopts copper to blend liquid-phase sintering process, but because tungsten copper is immiscible, its sintering character is relatively poor, is difficult to realize sintering densification and the microstructure that forms homogenising completely, the highest relative density generally only is 92-95%, and conduction, heat conductivility are poor.Adopt powder ultra-fine or that nano-diffusion distributes, can improve the sintering character of tungsten-copper alloy preferably, obtain comparatively ideal material; Other adds elements such as nickel, cobalt, iron, palladium, but activated sintering also can obtain effect preferably, can obtain higher relative density, hardness, fracture strength etc.But the adding of activator has significantly reduced conduction, the thermal conductivity of composite, has limited the scope of application of material.
Prepare the required ultra-fine/nanoscale composite W-Cu powder of ultra-fine/nanocrystal W-Cu alloy and mainly contain following method:
(1) pure tungsten powder and copper powder are mixed by theory requirement ratio, and carry out high-energy ball milling, obtain ultra-fine/nanometer composite W-Cu powder (Ryu S S through ma process, Kim Y D, Moon I H.Dilatometric analysis onthe sintering behavior of nanocrystalline W-Cu prepared by mechanical alloying[J] .Journal of Alloys and Compounds, 335 (2002) 233-240);
(2) pure W powder and CuO powder are mixed by theory requirement ratio, and carry out high-energy ball milling, through H
2Reduction process obtains nanometer composite W-Cu powder (Kim D G, Kim G S, Oh S T, Kim Y D.The initial stage ofsintering for the W-Cu nanocomposite powder prepared from W-CuO mixuure[J] .MaterialsLetters, 58 (2004) 578-581);
(3) wet chemical technology---the ammonia still process homogeneous precipitation method prepares nanometer CuWO in employing
42H
2O/Cu
2WO
4(OH)
2The precipitation from homogeneous solution thing is calcined then, is reduced, and obtains tungsten-copper composite powder (Cheng Jigui, Lei Chunpeng, Jiang Yang etc., the homogeneous precipitation method preparation and the sintering character thereof of nanometer W-Cu powder, China YouSe Acta Metallurgica Sinica, 15 (2005) 89-93);
(4) each metal salts in proportion is taken by weighing preparation salting liquid and mixing salt solution; Add small amount of acid or alkali and surfactant and obtain the colloidal sol body, nano oxidized composite powder of spray-dried preparation or complex salt composite powder presoma through once reducing and secondary reduction, obtain nanometer tungsten base composite powder (Fan Jinglian, Ma Yunzhu, Huang Baiyun, Wang Denglong, Chen Zhongbai, Wu Enxi, prepare the method for nanoscale tungsten base composite powder, Chinese invention patent ZL03143136.4, on June 12nd, 2003 with colloidal sol-spray-drying-thermal reduction);
(5) tungstenic, the copper compound of solubility is dissolved in makes precursor solution in the solvent, the precursor solution atomization drying is become precursor powder, other ion that precursor powder is removed in the soluble-salt by roasting is made the intermediate oxide powder, oxide powder is made nano-class composite W-Cu powder body (Yang Mingchuan by thermal chemical reaction under reducing atmosphere, Xu Jian, Lu Ke.A kind of preparation method of ultra-fine composite W-Cu powder, Chinese invention patent ZL 01114123.9, June 22 calendar year 2001);
(6) with ammonium metatungstate, copper nitrate or Schweinfurt green take by weighing the preparation mixing salt solution in proportion, spray-dried system, the nano oxidized composite powder of calcining preparation, ammonium paratungstate is prepared the tungsten oxide powder through calcining, require the ratio ball milling to mix according to theory both, after once reducing, obtain nano-class composite W-Cu powder end (Yong Won Woo, Seong Hyeon Hong, Byoung Kee Kim.Method of producing tungsten-copper basedcomposite powder and sintered alloys, US Pat.6914032, Oct.16,2002).
Wherein, ultra-fine/nano composite powder method that method (1) prepares tungsten-copper is introduced impurity easily in the high-energy ball milling; Method (2) has obtained certain improvement with respect to (1), but still has the shortcoming of introducing impurity easily; Method (3) exists cost height, shortcoming that the industrialization difficulty is big.Compare with said method, method (4), (5), (6) it is low to have a cost, be fit to advantages such as production continuously, has industrial prospect, but the too complicated repeatability that will increase production cost and reduce product of method (4) technology, simultaneously owing to exist the ball milling dispersing technology may introduce ball milling impurity, preparation technology is simple for method (5), but do not consider that the preparation tungsten-copper composite powder is last, breaking and scattering problem of powder agglomerates, in the process of preparation alloy, will inevitably influence the performance of alloy, method (6) has been considered the spherical agglomerated problem of tungsten-copper presoma composite oxide power that spray-drying forms, but reckon without the problem that ball milling disperses impurity to be incorporated into composite powder, the final performance that influences W-Cu alloy, the controllable granularity scope that other three kinds of methods prepare powder is narrower.
Summary of the invention
The objective of the invention is to propose a kind of preparation method who prepares composite W-Cu powder.This method can be good at solving spray pyrolysis or spray-drying and adds breaking and scattering problem of the presoma tungsten copper composite oxide power aggregate that is prepared into tungsten copper powder after the calcining, need not ball milling or other dispersion treatment, adopt many atmosphere tilting rotary furnace (Shao Gangqin, Duan Xinglong, Yi Zhong comes, Sun Peng, Wang Cong, Shi Xiaoliang, Xie Jiren, a kind of many atmosphere tilting rotary furnace, Chinese utility model patent on March 26th, 200420017540.2,2004) can guarantee that tungsten copper composite oxide power aggregate is broken and disperseed in the process of reduction continuously, guarantee the subsequent preparation W-Cu alloy can not influence the segregation of copper in the packing of base substrate and the sintered body and influence the performance of alloy because of the existence of aggregate, guarantee the even distribution of copper in composite powder and alloy, and simplified production technology, more help industrialization.
Be illustrated below in conjunction with 1 pair of implementation procedure of the present invention of accompanying drawing:
1, raw material:
The tungsten copper raw material is selected mixing of tungsten compound and copper compound for use, and choosing by following requirement of raw material undertaken:
(1) compound of tungsten can be selected a kind of in following for use: ammonium metatungstate AMT ((NH
4)
6(H
2W
12O
40) 4H
2O), ammonium paratungstate APT ((NH
4)
10(H
2W
12O
42) 4H
2O), positive ammonium tungstate (NH
4)
2WO
4, wolframic acid H
2WO
4, metatungstic acid H
6(H
2W
12O
40) etc.;
(2) compound of copper can be selected a kind of in following for use: nitric hydrate copper Cu (NO
3)
23H
2O, hydrated copper acetate Cu (CH
3COO)
2H
2O, ethanedioic acid copper C
2CuO
41/2H
2O, hydration copper chloride CuCl
22H
2O, hydrated copper sulfate [Cu (H
2O)
4] SO
4H
2O, basic copper carbonate Cu
2(OH)
2CO
3Deng;
(3) reducibility gas is hydrogen H
2
2, spray pyrolysis:
The concentration of aqueous solution of tungsten copper mixed material is 30～70wt.%, and the spray pyrolysis temperature is controlled at 600～900 ℃, and ambiance is air or inert gas;
3, spray-drying:
The concentration of aqueous solution of tungsten copper mixed material is 30～70wt.%, and the spray-drying temperature is controlled at 100～200 ℃, and ambiance is air or inert gas;
4, calcining:
Be reflected in rotary furnace or the micro-wave oven and carry out, ambiance is air, inert gas or vacuum, and temperature is controlled at 300～1200 ℃, 0.5～24 hour reaction time;
5, reducing process:
(Yi Zhong comes for Shao Gangqin, Duan Xinglong to be reflected at many atmosphere tilting rotary furnace, Sun Peng, Wang Cong, Shi Xiaoliang, Xie Jiren, a kind of many atmosphere tilting rotary furnace, Chinese utility model patent 200420017540.2, on March 26th, 2004) carry out in, ambiance is a hydrogen, and one time reduction temperature is controlled at 250～400 ℃, 2～5 hours reaction time, the secondary reduction temperature is controlled at 750～1200 ℃, 1～4 hour reaction time.
Wherein:
1, material composition is by the quality proportioning, and tungsten is 55～92wt.%, and copper is 8～45wt.%; Make the tungsten copper composite oxide power after the tungsten copper raw material added calcine technology through spray pyrolysis or spray-drying.
Adopt reducing atmosphere reduction combined oxidation powder technology to prepare the W-Cu composite powder: mixed oxide powder to be put into many atmosphere tilting rotary furnace under the ambiance, contain the reducing gases scale of construction, reduction temperature and reaction time by control and make the W-Cu composite powder.
2, the technological parameter of spray pyrolysis, spray-drying, calcining is as follows:
(1) spray pyrolysis: the concentration of aqueous solution of tungsten copper mixed material is 30～70wt.%, and the spray pyrolysis temperature is controlled at 600～900 ℃, and ambiance is air or inert gas;
(2) spray-drying: the concentration of aqueous solution of tungsten copper mixed material is 30～70wt.%, and the spray-drying temperature is controlled at 100～200 ℃, and ambiance is air or inert gas;
(3) calcining: temperature is controlled at 300～1200 ℃, and in 0.5～24 hour reaction time, ambiance is air, inert gas or vacuum;
3, reducing process is: the ambiance of reaction is a reductive hydrogen atmosphere, and one time reduction temperature is controlled at 250～400 ℃, and in 2～5 hours reaction time, the secondary reduction temperature is controlled at 750～1200 ℃, 1～4 hour reaction time.
The composite W-Cu powder of the present invention preparation has that granularity is adjustable, the characteristics of distributed components, purity height, good dispersion, and the tungsten grain degree of powder can be controlled in 50nm～1 μ m, and oxygen content is lower than 0.1wt.%.This powder has good sintering activity, can be used for preparing the high density W-Cu alloy with good mechanics and thermal property.Presoma tungsten copper composite oxide power of the present invention need not ball milling or other dispersion treatment, thereby technology is simple and direct, easy to control, do not pollute, cost of investment is low, is suitable for industrial-scale production.
The present invention can be generalized to the research and the production field of materials such as compound tungsten-bast alloy, cermet.
Description of drawings
Fig. 1: preparation technology's flow chart of composite W-Cu powder;
Fig. 2: the X ray diffracting spectrum of W-20Cu composite powder;
Fig. 3: the sem photograph of W-20Cu composite powder;
Fig. 4: the transmission electron microscope picture of W-20Cu composite powder.
Specific measures for implementation
Embodiment 1:
With 179 gram ammonium metatungstate AMT ((NH
4)
6(H
2W
12O
40) 4H
2O) and 121 gram nitric hydrate copper Cu (NO
3)
23H
2The O raw material is miscible in 500 milliliters distilled water, makes the tungsten copper composite oxide power through 120 ℃ of air atmosphere spray-dryings, puts into 750 ℃ of silicon-carbon stove air atmospheres calcination 3 hours, and the composite oxide power that obtains is at H
2Through 400 ℃ of reduction 4 hours, be warming up to 850 ℃ again in many atmosphere tilting rotary furnace under the atmosphere, be incubated 4 hours and carry out secondary reduction, subsequently in high-purity N
2Be cooled to room temperature in the atmosphere.
Embodiment 2:
With 155 gram ammonium paratungstate APT ((NH
4)
10(H
2W
12O
42) 4H
2O) and 145 gram hydrated copper acetate Cu (CH
3COO)
2H
2The O raw material is miscible in 500 milliliters distilled water, makes the tungsten copper composite oxide power through 180 ℃ of air atmosphere spray-dryings, puts into 750 ℃ of vacuum drying oven calcinations after 3 hours, and the powder that obtains is at H
2Through 300 ℃ of reduction 4 hours, be warming up to 800 ℃ again in many atmosphere tilting rotary furnace under the atmosphere, be incubated 2 hours and carry out secondary reduction, subsequently in high-purity N
2Be cooled to room temperature in the atmosphere, make the W-30Cu composite powder thus.
Embodiment 3:
With 128 positive ammonium tungstate (NH
4)
2WO
4With 172 gram ethanedioic acid copper C
2CuO
41/2H
2The O raw material is miscible in 500 milliliters distilled water, makes the tungsten copper composite oxide power through 700 ℃ of air atmosphere spray pyrolysis; The powder that obtains in many atmosphere tilting rotary furnace at H
2Through 260 ℃ of reductase 12s hour, be warming up to 850 ℃ of insulations again and carried out secondary reduction in 4 hours in the atmosphere, in high-purity Ar atmosphere, be cooled to room temperature subsequently, make the W-45Cu composite powder thus.
Embodiment 4:
With 258 gram ammonium metatungstate AMT ((NH
4)
6(H
2W
12O
40) 4H
2O) and 42 gram hydration copper chloride CuCl
22H
2The O raw material is miscible in 500 milliliters distilled water, makes the tungsten copper composite oxide power through 190 ℃ of air atmosphere spray-dryings, puts into micro-wave oven through 500 ℃ of calcinations 0.5 hour, and the powder that obtains is at H
2Through 300 ℃ of reduction 4 hours, be warming up to 1000 ℃ of secondary reductions again 0.5 hour in many atmosphere tilting rotary furnace under the atmosphere, in high-purity Ar atmosphere, be cooled to room temperature subsequently, make the W-8Cu composite powder thus.
Embodiment 5:
With 216 gram wolframic acid H
2WO
4With 84 gram hydrated copper sulfate [Cu (H
2O)
4] SO
4H
2The O raw material is miscible in 500 milliliters distilled water, makes the tungsten copper composite oxide power through 750 ℃ of air atmosphere spray pyrolysis; The tungsten copper composite oxide power that obtains is at H
2Through 280 ℃ of reduction 4 hours, be raised to 900 ℃ again in many atmosphere tilting rotary furnace under the/Ar atmosphere at H
2Secondary reduction is 1.5 hours in the atmosphere, in high-purity N
2Cool to room temperature in the atmosphere with the furnace, make the W-12Cu composite powder thus.
Embodiment 6:
With 242 gram metatungstic acid H
6(H
2W
12O
40) and 58 gram basic copper carbonate Cu
2(OH)
2CO
3Raw material is miscible in 500 milliliters distilled water, makes the tungsten copper composite oxide power through 150 ℃ of air atmosphere spray-dryings, through 950 ℃ of calcinations 1.5 hours, when reducing to 400 ℃, feeds H in the many atmosphere tilting rotary furnace under Ar atmosphere
2Gas carries out reductase 12 hour, is warming up to 850 ℃ again at H
2Insulation was carried out secondary reduction in 3 hours in the atmosphere, was cooled to room temperature subsequently in high-purity Ar atmosphere, made the W-15Cu composite powder thus.
Claims (1)
1. the preparation method of a composite W-Cu powder, it is characterized in that at first the tungsten copper mixed material being made composite oxide power through spray pyrolysis, make composite oxide power after perhaps adding calcining through spray-drying, the composite oxide power granularity is controlled at 0.1～10 μ m; Many atmosphere tilting rotary furnace of the composite oxides powder being put under the reducing atmosphere reacts then, by the control reducing gases scale of construction, reduction temperature and reaction time, makes composite W-Cu powder through secondary reduction, wherein:
(1) the tungsten copper mixed material is a tungsten compound and the mixing of copper compound, wherein:
Tungsten compound is selected a kind of in following for use: ammonium metatungstate AMT (NH
4)
6(H
2W
12O
40) 4H
2O, ammonium paratungstate APT (NH
4)
10(H
2W
12O
42) 4H
2O, positive ammonium tungstate (NH
4)
2WO
4, wolframic acid H
2WO
4, metatungstic acid H
6(H
2W
12O
40);
Copper compound is selected a kind of in following for use: nitric hydrate copper Cu (NO
3)
23H
2O, hydrated copper acetate Cu (CH
3COO)
2H
2O, ethanedioic acid copper C
2CuO
41/2H
2O, hydration copper chloride CuCl
22H
2O, hydrated copper sulfate [Cu (H
2O)
4] SO
4H
2O, basic copper carbonate Cu
2(OH)
2CO
3
(2) spray pyrolysis process: the concentration of aqueous solution of tungsten copper mixed material is 30～70wt.%, and pyrolysis temperature is controlled at 600～900 ℃, and ambiance is air or inert gas;
(3) spray-drying adds calcine technology: the concentration of aqueous solution of tungsten copper mixed material is 30～70wt.%, and the spray-drying temperature is controlled at 100～200 ℃, and ambiance is air or inert gas; Calcining heat is controlled at 300～1200 ℃, and in 0.5～24 hour reaction time, ambiance is air, inert gas or vacuum;
(4) reducing process: the ambiance of reaction is a reductive hydrogen atmosphere, and one time reduction temperature is controlled at 250～400 ℃, and in 2～5 hours reaction time, the secondary reduction temperature is controlled at 750～1200 ℃, and in 1～4 hour reaction time, ambiance is a hydrogen.
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| CN114833348A (en) * | 2022-05-07 | 2022-08-02 | 合肥工业大学 | Large-scale preparation method of controllable high-quality W-Cu composite powder |
| CN115446323B (en) * | 2022-09-22 | 2024-03-22 | 西北有色金属研究院 | Method for preparing tungsten-molybdenum powder by utilizing waste target scraps of tungsten and molybdenum |
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