CN105177633A - W-Ni-Cu gradient material and preparation method thereof - Google Patents
W-Ni-Cu gradient material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a W-Ni-Cu gradient material and a preparation method thereof. The method comprises the following steps: taking a molten salt system of NaCl-KCl-NaF-NiO as an Ni leakage source and taking a copper-plating aqueous solution as a Cu leakage source; electrically depositing and leaking nickel on a pure W plate through molten salt, electrically depositing and leaking Cu through an aqueous solution; and finally diffusing and annealing to obtain the W-Ni-Cu gradient material. The material is high in thermal shock resistance and thermal fatigue resistance; all the components of the material are combined closely; the material surface structure is compact and smooth; the material has high electrical conductivity, high thermal conductivity and high mechanical performance. The method is capable of simultaneously carrying out mutual diffusion between W and Ni and carrying out mutual diffusion between Ni and Cu under the action of an electric field and a temperature field by using an electric deposition method according to the basic diffusion theory (the electric field can accelerate the diffusion of solid metals, and the diffusion speed of the opposite party can also be mutually improved when carrying out multi-element diffusion in the solid diffusion); the thickening of gradient layers can be accelerated; the W-Ni-Cu gradient material has the characteristics of rapid forming speed of the gradient layers, short preparation time, randomly controllable thickness of the gradient layers, compact surface structure of the material, high thermal conductivity and simple process.
Description
Technical field
The present invention relates to a kind of gradient material and preparation method thereof, especially a kind of W-Ni-Cu gradient material and preparation method thereof.
Background technology
Gradient material is applied to the fields such as nuclear energy, biomedicine, machinery, petrochemical complex, information, civilian and aerospace as a kind of type material.The key features of gradient material is the consecutive variations by control inerface composition and tissue, the different material of two or more performances is well coupled together, thus reaches the object improved materials'use performance He increase the service life.W-Cu gradient material has excellent characteristic because having special construction model, and in nuclear industry, electronic industry, mechanical engineering, is widely applied in the fields such as aerospace.
The preparation research of W-Ni-Cu gradient material rarely has report both at home and abroad at present, but has certain report both at home and abroad in the preparation of W-Cu gradient material.At present, the preparation method of domestic and international W-Cu gradient material mainly contains and moltenly oozes method, powder metallurgic method, plasma spraying method and fused salt electrodip process etc.
Infiltration method prepares W-Cu gradient material, is W powder (or the W powder containing a little Cu powder) is pressed into base, under preset temp, is then fired into the porous W base skeleton with certain density and intensity, finally in reducing atmosphere or vacuum, oozes Cu.Adopt the W-Cu gradient material prepared in this way, thermal conductivity is low, mainly because the void distribution of W skeleton is wayward, be difficult to obtained 0 ~ 100% proper gradient material, cause when oozing Cu, Cu Entropy density deviation is uneven, easily there is closed pore in W base, space can not be filled up completely.In addition, be difficult to preparation W volume fraction lower than the gradient material of 50%, limit the composition range of W-Cu gradient material.In addition, remove unnecessary metallic cementation Cu, also can increase cost.
Powder metallurgic method (PM) prepares W-Cu gradient material, that particulate state W, Cu starting material are mixed by pre-designed proportioning, pavement layer by layer, be pressed into gradient-structure prefabricated section, then adopt normal pressure-sintered, the sintering method such as hot pressed sintering, HIP sintering, reaction sintering to make sintering gradient material body.Adopt the W-Cu gradient material prepared in this way, density is lower, mainly because W, Cu density and fusing point difference are comparatively large, and any reaction does not occur between the two.In addition, manufacture craft more complicated, comparatively strict to the requirement of holding temperature, time and speed of cooling.
The direction that plasma spraying method prepares W-Cu gradient material mainly contains two kinds: a kind of be select thermal expansivity between W, Cu material as transition layer; Another kind selects the gradient layer of W, Cu to be transition layer, can eliminate the thermal stress issues existed because W, Cu thermal expansivity difference is comparatively large to greatest extent.Adopt gradient material bonding strength prepared by plasma spraying method lower, coating structure is uneven, coating porosity is high, and inter-layer bonding force is low, easily peels off, and major cause is that coating and matrix are based on mechanical bond.
Fused salt electrodip process prepares W-Cu gradient material, is to utilize electrochemical principle the W ion deposition in fused salt to negative electrode Cu substrate will to be formed the process of Cu-W gradient layer.Adopt the gradient material prepared in this way there is Thickness of Gradient Layer easily to control, process parameter control wide ranges, easy to operate, material surface compact structure, the feature such as smooth, but the bonding strength of material is low, mainly because W, Cu are immiscible under normal conditions, both can not form sosoloid, can not be reacted generation compound, and the W-Cu gradient material formed is a kind of pseudo-alloy of typical case.
Analysis above shows, W-Ni-Cu gradient material rarely having heat shock resistance and heat-resistant anti-fatigue performance at present and preparation method thereof, even if also there is following deficiency in W-Cu gradient material like material type therewith preparing: the defect such as hole, cavity of (1) gradient layer is more, and mechanical property is relatively poor; (2) processing condition are complicated, and production cost is high; (3) the proper gradient material of preparation 0 ~ 100% is difficult to.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of W-Ni-Cu gradient material with graded; Present invention also offers the preparation method of the W-Ni-Cu gradient material of a kind of resistance to sudden heating and heat-resistant anti-fatigue performance.
For solving the problems of the technologies described above, the technical solution used in the present invention is: it is with pure W plate for matrix, and matrix both sides are W-Ni-Cu gradient layers; Described gradient layer raises gradually for Cu content from inside to outside, and Ni content first raises rear reduction, and W content reduces gradually.
From inside to outside, the composition Changing Pattern of phase is gradient material of the present invention: W-NiW
2+ NiW+Ni
4w-Cu.
NiW of the present invention
2+ NiW+Ni
4the thickness of W-Cu gradient layer is 25 μm ~ 45 μm.
The inventive method is: described method oozes source using the molten salt system of NaCl-KCl-NaF-NiO as Ni, oozes source using the copper facing aqueous solution as Cu; Pure W plate oozes nickel through fused salt galvanic deposit, Cu is oozed in aqueous solution galvanic deposit, last diffusion annealing, can obtain described W-Ni-Cu gradient material.
Further, the processing step of the inventive method is: negative electrode W plate and anode Ni plate insert in the fused salt of NaCl-KCl-NaF-NiO by (1) simultaneously, then carry out galvanic deposit;
(2) after galvanic deposit terminates, take out negative electrode W plate, after removing fused salt dirt settling, flushing, W-Ni gradient material can be obtained;
(3) negative electrode W-Ni gradient material and positive C u plate are inserted in the copper facing aqueous solution simultaneously, then carry out galvanic deposit;
(4) after galvanic deposit terminates, take out negative electrode W-Ni gradient material, after removing fused salt dirt settling, flushing, W-Ni-Cu alloy material can be obtained;
(5) W-Ni-Cu alloy material is carried out diffusion annealing process in the annealing furnace of inert atmosphere protection, described W-Ni-Cu gradient material can be obtained.
Further, in step described in the inventive method (1), at temperature 700 ~ 800 DEG C, current density 50 ~ 100mAcm
-2condition under galvanic deposit 10 ~ 30min.
Further, in step described in the inventive method (3), at current density 30 ~ 70mAcm
-2condition under galvanic deposit 80 ~ 100min.
Further, the diffusion annealing in step described in the inventive method (5) is treated to: at 800 ~ 1000 DEG C of insulation 60 ~ 180min.In described diffusion annealing treating processes, after W-Ni-Cu alloy material is put into annealing furnace, elder generation to preset temp 800 ~ 1000 DEG C with 3 ~ 8 DEG C/min ramp, is incubated afterwards, is finally cooled to room temperature with identical speed range again.
The technological principle of the inventive method is: in NaCl-KCl-NaF-NiO molten salt system, take metal W as negative electrode, and W metal is anode, galvanic deposit under the effect of DC pulse current, and described W negative electrode can form W-Ni gradient material; Afterwards in the copper facing aqueous solution, with W-Ni gradient material for negative electrode, Ni metal is anode, galvanic deposit under the effect of DC pulse current, and described W-Ni negative electrode can form W-Ni-Cu alloy; Last annealing DIFFUSION TREATMENT of passing through in the annealing furnace of inert atmosphere protection can form W-Ni-Cu gradient material.
Adopt the beneficial effect that produces of technique scheme to be: material of the present invention has good resistance to sudden heating and heat-resistant anti-fatigue performance, material each several part combines closely, material surface compact structure, smooth, has good conduction, thermal conductivity and mechanical property.
The inventive method is for the characteristic of existing W-Ni and Cu-Ni alloy, according to diffusion basic theories, adopt electrodip process, under the effect in electric field and temperature field, between W, Ni and between Ni, Cu, mutual diffusion occurring simultaneously, (electric field can accelerate the diffusion of solid metal, also the velocity of diffusion of the other side mutually can be improved during multielement diffusion in solid-state diffusion), accelerating gradient layer thickens.The inventive method has gradient layer and forms that speed is fast, preparation time is short, Thickness of Gradient Layer can arbitrarily control, material surface compact structure, thermal conductivity are good, the features such as technique is simple.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is W-Ni-Cu distribution diagram of element in the embodiment of the present invention 1 gained gradient material;
Fig. 2 is W-Ni-Cu distribution diagram of element in the embodiment of the present invention 2 gained gradient material;
Fig. 3 is W-Ni-Cu distribution diagram of element in the embodiment of the present invention 3 gained gradient material.
Embodiment
This W-Ni-Cu gradient material is with pure W plate for matrix, and matrix both sides are W-Ni-Cu gradient layers; Described gradient layer raises gradually for Cu content from inside to outside, and Ni content first raises rear reduction, and W content reduces gradually; From inside to outside, the composition Changing Pattern of phase is: W-NiW
2+ NiW+Ni
4w-Cu; Wherein, NiW
2+ NiW+Ni
4the thickness of W-Cu gradient layer is 25 μm ~ 45 μm.This W-Ni-Cu gradient material adopts following preparation method to produce:
(1) by NaCl-KCl-NaF-NiO(mol ratio be: 0.36:0.36:0.25:0.03) reagent mixing is poured in plumbago crucible; again the plumbago crucible being stamped graphite cover is put into resistance furnace electrified regulation; and pass into shielding gas argon gas; stir after being warming up to 700 ~ 800 DEG C, insulation 40 ~ 80min reaches stable to make melting molten salt system.
(2) by pure for negative electrode W plate (20 × 20 × 2mm), the pure Ni plate (20 × 20 × 2mm) of anode puts into the plumbago crucible of cvd furnace, at 700 ~ 800 DEG C, 50 ~ 100mAcm
-2condition under galvanic deposit 10 ~ 30min.
(3) take out negative electrode W plate after deposition, first with boiling water boiling 10 ~ 30min to remove fused salt dirt settling, then to rinse successively with deionized water and alcohol, W-Ni gradient material can be obtained.
(4) by CuSO
45H
2the concentration of O(in mix reagent is 90g/L), CuCl
2(concentration in mix reagent is 7g/L), H
2sO
4(concentration in mix reagent is 30ml/L) mix reagent is put into glass dish, and is added in distilled water, at room temperature dissolves, and is mixed with the copper facing aqueous solution, leaves standstill 20 ~ 40min and makes molten salt system reach stable.
(5) negative electrode W-Ni gradient material and the pure Cu plate (20 × 20 × 2mm) of anode being put into the coating bath that the copper facing aqueous solution is housed, make pulse electroplating power supply, is 30 ~ 70mAcm in current density
-2condition under galvanic deposit 80 ~ 100min, deposit the W-Ni-Cu alloy of surfacing.
(6) take out negative electrode W-Ni gradient material after deposition, first with boiling water boiling 10 ~ 30min to remove fused salt dirt settling, then to rinse successively with deionized water and alcohol, W-Ni-Cu alloy can be obtained.
(7) W-Ni-Cu alloy is placed in high-temperature annealing furnace, controls annealing furnace with 3 ~ 8 DEG C/min ramp, occur crackle to prevent W, Cu because thermal diffusivity difference is comparatively large; Be warming up to 800 ~ 1000 DEG C, annealing (insulation) 60 ~ 180min; Finally be cooled to room temperature with the rate of temperature fall scope identical with temperature rise rate scope again; Omnidistance inert atmosphere protection, is preferably argon gas atmosphere, to prevent material oxidized; Described W-Ni-Cu gradient material can be obtained.
In aforesaid method, Cu, Ni, W content distribution of described gradient layer, the control of thickness and thermal conductivity, realize mainly through parameters such as adjustment electrodeposition time, electrodeposition temperature, current density, annealing times.Present method working mechanism is as follows: due to electric field and temperature field, W-Ni-Cu content concn gradient and the chemical diffusion of W-Ni-Cu and the effect of physical diffusion, and accelerating to be formed along matrix W to top layer phase composite Changing Pattern is W trace NiW
2+ NiW+Ni
4the gradient material of W Cu weave construction, shortens the formation time of gradient layer, accelerating gradient layer thicken speed.Through inspection, gradient material has good resistance to sudden heating and thermal fatigue resistance; The purer W plate of thermal conductivity of W-Ni-Cu gradient material (45 μm) reduces 1 times; Gradient material surface has high copper content (100%), and gradient material inwardly foreign object is a small amount of NiW mutually gradually
2, NiW, Ni
4w, can improve the hot strength of gradient material, extends the life-span of material.
The concrete production technique of embodiment 1: this W-Ni-Cu gradient material is as described below.
NaCl-KCl-NaF-NiO molten salt system is loaded plumbago crucible, puts into electric furnace and be warming up to 700 DEG C, constant temperature 40min; Negative electrode W plate (20 × 20 × 2mm) and anode Ni plate (20 × 20 × 2mm) are put into simultaneously the NaCl-KCl-NaF-NiO fused salt of melting, apply DC pulse current, current density is 50mAcm
-2time, after 700 DEG C of galvanic deposit 10min, from the NaCl-KCl-NaF-NiO molten salt system of melting, take out cathode material, put into boiling water and boil 10min, make without obvious fused salt dirt settling on W board substrate, then use deionized water, alcohol rinse sample, W-Ni gradient material can be obtained.By CuSO
45H
2o, CuCl
2, H
2sO
4mix reagent puts into glassware, adds in distilled water, at room temperature dissolves, and leaves standstill 20min; Negative electrode W-Ni gradient material and positive C u plate (20 × 20 × 2mm) are inserted in the copper facing aqueous solution, apply DC pulse current, current density is 30mAcm simultaneously
-2, after galvanic deposit 80min, from the copper facing aqueous solution, take out cathode material, put into boiling water and boil 10min, make without obvious fused salt dirt settling on W-Ni board substrate, then use deionized water, alcohol rinse sample, W-Ni-Cu alloy material can be obtained.W-Ni-Cu alloy material is put into high-temperature annealing furnace; be 800 DEG C with stove with the ramp of 3 DEG C/min to preset temp; insulation 60min; room temperature is cooled to the speed of 3 DEG C/min again with stove; annealing process should be carried out under the environment of Ar protective atmosphere, finally can obtain W-Ni-Cu gradient material.
Show coating surface morphology, section thickness and W, Ni, Cu content distribution, Surface Phases analytical results, the surface compact of the present embodiment gained gradient material is smooth, and gradient layer surface is pure Cu.With GDA750 glow discharge spectrometry to material analysis, the results are shown in Figure 1, show: material both side surface is Ni metal, middle layer is metal W, and gradient layer raises gradually for Cu content from inside to outside, and Ni content first raises rear reduction, W content reduces gradually, and Thickness of Gradient Layer is 25 μm.
The concrete production technique of embodiment 2: this W-Ni-Cu gradient material is as described below.
NaCl-KCl-NaF-NiO molten salt system is loaded plumbago crucible, puts into electric furnace and be warming up to 750 DEG C, constant temperature 60min; Negative electrode W plate (20 × 20 × 2mm) and anode Ni plate (20 × 20 × 2mm) are put into simultaneously the NaCl-KCl-NaF-NiO fused salt of melting, apply DC pulse current, current density is 70mAcm
-2time, after 750 DEG C of galvanic deposit 20min, from the NaCl-KCl-NaF-NiO molten salt system of melting, take out cathode material, put into boiling water and boil 20min, make without obvious fused salt dirt settling on W board substrate, then use deionized water, alcohol rinse sample, W-Ni gradient material can be obtained.By CuSO
45H
2o, CuCl
2, H
2sO
4mix reagent puts into glassware, adds in distilled water, at room temperature dissolves, and leaves standstill 30min; Negative electrode W-Ni gradient material and positive C u plate (20 × 20 × 2mm) are inserted in the copper facing aqueous solution, apply DC pulse current, current density is 50mAcm simultaneously
-2, after galvanic deposit 90min, from the copper facing aqueous solution, take out cathode material, put into boiling water and boil 20min, make without obvious fused salt dirt settling on W-Ni board substrate, then use deionized water, alcohol rinse sample, W-Ni-Cu alloy material can be obtained.W-Ni-Cu alloy material is put into high-temperature annealing furnace; be 900 DEG C with stove with 5 DEG C/min ramp to preset temp; insulation 120min; room temperature is cooled to the speed of 8 DEG C/min again with stove; annealing process should be carried out under the environment of Ar protective atmosphere, finally can obtain W-Ni-Cu gradient material.
Show coating surface morphology, section thickness and W, Ni, Cu content distribution, Surface Phases analytical results, the gradient layer surface compact obtained is smooth, and gradient layer surface is pure Cu.With GDA750 glow discharge spectrometry to material analysis, the results are shown in Figure 2, show: material both side surface is Ni metal, middle layer is metal W, and gradient layer raises gradually for Cu content from inside to outside, and Ni content first raises rear reduction, W content reduces gradually, and Thickness of Gradient Layer is 35 μm.
The concrete production technique of embodiment 3: this W-Ni-Cu gradient material is as described below.
NaCl-KCl-NaF-NiO molten salt system is loaded plumbago crucible, puts into electric furnace and be warming up to 800 DEG C, constant temperature 80min; Negative electrode W plate (20 × 20 × 2mm) and anode Ni plate (20 × 20 × 2mm) are put into simultaneously the NaCl-KCl-NaF-NiO fused salt of melting, apply DC pulse current, current density is 100mAcm
-2, after 800 DEG C of galvanic deposit 30min, from the NaCl-KCl-NaF-NiO molten salt system of melting, take out cathode material, put into boiling water and boil 30min, make without obvious fused salt dirt settling on W board substrate, then use deionized water, alcohol rinse sample, W-Ni gradient material can be obtained.By CuSO
45H
2o, CuCl
2, H
2sO
4mix reagent puts into glassware, adds in distilled water, at room temperature dissolves, and leaves standstill 40min; Negative electrode W-Ni gradient material and positive C u plate (20 × 20 × 2mm) are inserted in the copper facing aqueous solution, apply DC pulse current, current density is 70mAcm simultaneously
-2, after galvanic deposit 100min, from the copper facing aqueous solution, take out cathode material, put into boiling water and boil 30min, make without obvious fused salt dirt settling on W-Ni board substrate, then use deionized water, alcohol rinse sample, W-Ni-Cu alloy material can be obtained.W-Ni-Cu alloy material is put into high-temperature annealing furnace; be 1000 DEG C with stove with the ramp of 8 DEG C/min to preset temp; insulation 180min; room temperature is cooled to the speed of 5 DEG C/min again with stove; annealing process should be carried out under the environment of Ar protective atmosphere, finally can obtain W-Ni-Cu gradient material.
Show coating surface morphology, section thickness and W, Ni, Cu content distribution, Surface Phases analytical results, the specimen surface densification obtained is smooth, and gradient layer surface is pure Cu.With GDA750 glow discharge spectrometry to material analysis, the results are shown in Figure 3, show: material both side surface is Ni metal, middle layer is metal W, and gradient layer raises gradually for Cu content from inside to outside, and Ni content first raises rear reduction, W content reduces gradually, and Thickness of Gradient Layer is 45 μm.
The concrete production technique of embodiment 4: this W-Ni-Cu gradient material is as described below.
NaCl-KCl-NaF-NiO molten salt system is loaded plumbago crucible, puts into electric furnace and be warming up to 780 DEG C, constant temperature 50min; Negative electrode W plate (20 × 20 × 2mm) and anode Ni plate (20 × 20 × 2mm) are put into simultaneously the NaCl-KCl-NaF-NiO fused salt of melting, apply DC pulse current, current density is 85mAcm
-2, after 780 DEG C of galvanic deposit 20min, from the NaCl-KCl-NaF-NiO molten salt system of melting, take out cathode material, put into boiling water and boil 15min, make without obvious fused salt dirt settling on W board substrate, then use deionized water, alcohol rinse sample, W-Ni gradient material can be obtained.By CuSO
45H
2o, CuCl
2, H
2sO
4mix reagent puts into glassware, adds in distilled water, at room temperature dissolves, and leaves standstill 35min; Negative electrode W-Ni gradient material and positive C u plate (20 × 20 × 2mm) are inserted in the copper facing aqueous solution, apply DC pulse current, current density is 60mAcm simultaneously
-2, after galvanic deposit 85min, from the copper facing aqueous solution, take out cathode material, put into boiling water and boil 25min, make without obvious fused salt dirt settling on W-Ni board substrate, then use deionized water, alcohol rinse sample, W-Ni-Cu alloy material can be obtained.W-Ni-Cu alloy material is put into high-temperature annealing furnace; being warming up to preset temp with stove with the speed of 6 DEG C/min is 850 DEG C; insulation 150min; room temperature is cooled to the speed of 4 DEG C/min again with stove; annealing process should be carried out under the environment of Ar protective atmosphere, finally can obtain W-Ni-Cu gradient material.
Show coating surface morphology, section thickness and W, Ni, Cu content distribution, Surface Phases analytical results, the specimen surface densification obtained is smooth, and gradient layer surface is pure Cu.With GDA750 glow discharge spectrometry to material analysis: material both side surface is Ni metal, and middle layer is metal W, and gradient layer raises gradually for Cu content from inside to outside, and Ni content first raises rear reduction, and W content reduces gradually, Thickness of Gradient Layer is 30 μm.
Claims (9)
1. a W-Ni-Cu gradient material, is characterized in that: it is with pure W plate for matrix, and matrix both sides are W-Ni-Cu gradient layers; Described gradient layer raises gradually for Cu content from inside to outside, and Ni content first raises rear reduction, and W content reduces gradually.
2. a kind of W-Ni-Cu gradient material according to claim 1, is characterized in that: from inside to outside, the composition Changing Pattern of phase is described gradient material: W-NiW
2+ NiW+Ni
4w-Cu.
3. a kind of W-Ni-Cu gradient material according to claim 2, is characterized in that: described NiW
2+ NiW+Ni
4the thickness of W-Cu gradient layer is 25 μm ~ 45 μm.
4. a preparation method for W-Ni-Cu gradient material, is characterized in that: described method oozes source using the molten salt system of NaCl-KCl-NaF-NiO as Ni, oozes source using the copper facing aqueous solution as Cu; Pure W plate oozes nickel through fused salt galvanic deposit, Cu is oozed in aqueous solution galvanic deposit, last diffusion annealing, can obtain described W-Ni-Cu gradient material.
5. the preparation method of a kind of W-Ni-Cu gradient material according to claim 4, is characterized in that, the processing step of described method is: negative electrode W plate and anode Ni plate insert in the fused salt of NaCl-KCl-NaF-NiO by (1) simultaneously, then carry out galvanic deposit;
(2) after galvanic deposit terminates, take out negative electrode W plate, after removing fused salt dirt settling, flushing, W-Ni gradient material can be obtained;
(3) negative electrode W-Ni gradient material and positive C u plate are inserted in the copper facing aqueous solution simultaneously, then carry out galvanic deposit;
(4) after galvanic deposit terminates, take out negative electrode W-Ni gradient material, after removing fused salt dirt settling, flushing, W-Ni-Cu alloy material can be obtained;
(5) W-Ni-Cu alloy material is carried out diffusion annealing process in the annealing furnace of inert atmosphere protection, described W-Ni-Cu gradient material can be obtained.
6. the preparation method of a kind of W-Ni-Cu gradient material according to claim 5, is characterized in that: in described step (1), at temperature 700 ~ 800 DEG C, current density 50 ~ 100mAcm
-2condition under galvanic deposit 10 ~ 30min.
7. the preparation method of a kind of W-Ni-Cu gradient material according to claim 5, is characterized in that: in described step (3), at current density 30 ~ 70mAcm
-2condition under galvanic deposit 80 ~ 100min.
8. the preparation method of a kind of W-Ni-Cu gradient material according to claim 5,6 or 7, is characterized in that, the diffusion annealing in described step (5) is treated to: at 800 ~ 1000 DEG C of insulation 60 ~ 180min.
9. the preparation method of a kind of W-Ni-Cu gradient material according to claim 8, it is characterized in that: in described diffusion annealing treating processes, after W-Ni-Cu alloy material is put into annealing furnace, first with 3 ~ 8 DEG C/min ramp to preset temp 800 ~ 1000 DEG C, be incubated afterwards, be finally cooled to room temperature with identical speed range again.
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| CN105177633B (en) | 2017-09-01 |
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