CN103418786B - A kind of low W-W connection degree W-Cu-Ni alloy material - Google Patents
A kind of low W-W connection degree W-Cu-Ni alloy material Download PDFInfo
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Abstract
The invention discloses the alloy material of a kind of low W-W connection degree W-Cu-Ni, its concrete preparation technology is: use the method for chemical plating at micron order tungsten powder surface nickel plating clad, the tungsten powder of surface cladded with nickel layer is prepared burden, mixed with copper powder, again the powder after mixing is carried out to discharge plasma sintering (SPS), prepare the low W-W connection degree W-Cu-Ni alloy material with high-compactness. Its advantage is: 1. nickel clad can improve the interface bond strength of tungsten phase and copper phase, and plays activated sintering, reduces the effect of sintering temperature, is conducive to improve the density of material simultaneously; 2. can prepare by preparation method of the present invention the W-Cu-Ni alloy material that density is less than 30% with W-W degree of connection more than 97.5%, material has good tensile mechanical properties. W-Cu-Ni alloy material of the present invention has excellent mechanical property, is applicable to Aero-Space and weapons field.
Description
Technical field
The invention belongs to metallurgical technology field, relate to the preparation technology of refractory metal, especially a kind of W-Cu-Ni alloy of low W-W connection degree.
Background technology
Tungsten-copper alloy material had both had the features such as the high strength, high rigidity, low-expansion coefficient of tungsten, had again high conduction, heat conductivility and the good plasticity of copper simultaneously, was therefore widely used in the fields such as Aero-Space, spark machined and electronic package material. Along with scientific and technical development, tungsten-copper alloy also shows good application potential as warhead with material, but the mechanical property of tungsten-copper alloy is had higher requirement simultaneously, the especially tensile mechanical properties of material.
Comprise tearing of W-W Interface Cracking, W-Cu Interface Cracking, W particle cleavage fracture and Binder Phase for its failure mode of tungsten-copper alloy, wherein due to a little less than W-W interface bond strength in tungsten-copper alloy, between W-Cu, there is no metallurgical binding, bond strength is also very weak, so easily ftracture in W-W interface and W-Cu interface under stretching loading environment, cause tungsten-copper alloy tensile strength extreme difference. Therefore, in order to improve the tensile strength of tungsten-copper alloy, first to suppress the formation at W-W interface, reduce W-W connection degree, will realize the metallurgical binding between W-Cu simultaneously, improve W-Cu interface bond strength.
At present, there is method to solve the high problem of W-W connection degree. As Chinese patent ZL201010607044.2 provides a kind of preparation method of copper-coated tungsten composite powder, utilize the tungsten alloy of the powder sintered preparation of copper cladding tungsten prepared by the method to avoid the direct contact of W-W, but the bond strength at W-Cu interface improve not yet. Therefore, how in reduction W-Cu alloy, in W-W connection degree, to improve the bond strength at W-Cu interface, the tensile mechanical properties that further improves material becomes problem demanding prompt solution.
Because dissolving each other completely, Ni and Cu can form unlimited solid solution, can form limit solid solution by partial miscibility with W, therefore can mix with copper powder again by the coated Ni layer in W particle top layer, then adopt the method for discharge plasma sintering (SPS) to prepare tungsten-copper-nickel alloy, improve the tensile strength of tungsten-copper alloy. In this preparation method, between Ni layer and W phase and copper phase, form solid solution, the metallurgical junction that can improve between W-Cu interface is made a concerted effort, and then improves W-Cu boundary strength, and nickel dam can also be avoided the direct contact between tungsten particle simultaneously, reduces W-W connection degree. In addition, Ni and Cu form solid solution, play the effect of solution strengthening, have improved the intensity of alloy. Therefore can prepare by said method there is good W-Cu interface bond strength, the high-compactness tungsten copper of low W-W connection degree and good tensile mechanical properties is associated gold copper-base alloy.
Summary of the invention
The tungsten-bast alloy the present invention relates to is W-Cu-Ni alloy material.
The present invention has improved the tensile property of existing tungsten-copper alloy, provides a kind of combination chemical nickel plating and discharge plasma sintering preparation to have the preparation method of the W-Cu-Ni alloy material of higher W-Cu interface bond strength, low W-W connection degree, high-compactness, better tensile property.
The technical scheme that the present invention takes is: the method by chemical nickel plating is coated one deck nickel on tungsten particle surface, adopt the method for mechanical mixture that nickel coated tungsten powder is mixed with copper powder, adopt discharging plasma sintering equipment to carry out sintering to mixing rear powder, obtain thering is high-compactness, the W-Cu-Ni alloy that low W-W connection degree and crystal grain are tiny. Wherein in W-Cu-Ni alloy, the computing formula of W-W connection degree is:
In formula, CSSW-W connection degree, NSSW-W interface number, NSLIt is W-Cu interface number. NSSAnd NSLComputational methods as follows: gridding on the section shape appearance figure of W-Cu-Ni alloy, then the W-W interface number and the W-Cu interface number that pass along this line of horizontal line (vertical curve) number, until all horizontal lines (vertical curve) and the intersection point at W-W interface and W-Cu interface are counted up to, corresponding number of hits is respectively NSSAnd NSL。
For above-mentioned nickel process, its process parameters range is as follows:
Six hydration nickel sulfate concentration range is that 20～40g/L, hypophosphorous acid hydrogen na concn scope are that 20～40g/L, ammonium chloride concentration scope are that 30～40g/L, sodium pyrophosphate concentration range are that 50～70g/L, sodium citrate concentration scope are that 5～10g/L, triethanolamine concentration range are 90～120g/L, bath temperature is 35～40 DEG C, pH value is 8～10, and chemical plating plating time is 20～40min.
For the preparation method of above-mentioned W-Cu-Ni alloy material, comprise the steps:
(1) adopt the method for chemical nickel plating to prepare the composite powder of the coated tungsten of nickel, coated nickel tungsten composite powder is mixed 1～2 hour (wet mixing) with a certain proportion of copper powder by recycling planetary ball mill (without abrading-ball), dry under vacuum condition, each element mass percent is: W content 65%～80%, Cu content 15%～25%, Ni content 5%～10%.
(2) alloying element powder (1) gained being mixed reduces 0.5～1h in nitrogen atmosphere, and reduction temperature scope is 200 DEG C～300 DEG C, obtains mixing fully and the mechanical impurity of the metal dust of non-oxidation.
(3) adopt discharge plasma sintering technique to carry out sintering to gained mixed-powder in (2); sintering temperature is 850～950 DEG C, and exerting pressure is 20～50MPa, and heating rate is 50～150 DEG C/min; temperature retention time is 5～10min, and sintering atmosphere is vacuum protection.
Brief description of the drawings
Fig. 1 is the overall pattern of the coated tungsten composite powder of nickel;
Fig. 2 is the section pattern of the coated tungsten composite powder of the nickel inlayed of dental base acrylic resin powder;
Fig. 3 is the overall pattern of low W-W connection degree W-Cu-Ni alloy;
Fig. 4 is that pattern is amplified in the part of low W-W connection degree W-Cu-Ni alloy;
Fig. 5 is the XRD collection of illustrative plates of low W-W connection degree W-Cu-Ni alloy.
Detailed description of the invention
Below in conjunction with five specific embodiments, the present invention is further understood in exemplary illustration and help. But embodiment detail is only for the present invention is described, do not represent the whole technical schemes of the present invention under conceiving, therefore can not be interpreted as the restriction to technical solution of the present invention. Some do not depart from the unsubstantiality of the present invention's design changes, for example, to have simple the change or replacement of technical characterictic of same or similar technique effect, all belong to rights protection scope of the present invention.
Embodiment 1
A kind of tungsten-copper-nickel alloy material, alloying component and content (mass percent): 80%W-15%Cu-5%Ni, its preparation method comprises the following steps:
Step 1, selecting average grain diameter is the tungsten powder 20g of 6 μ m, first utilizes 60mL/LHCl to carry out alligatoring, alligatoring 12h, recycling 30g/LSnCl2Carry out sensitization with 50mL/LHCl, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl2Activate with 10mL/LHCl, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, takes six hydration nickel sulfate by tungsten nickel weight ratio at 16: 1, and preparation solution composition is six hydration nickel sulfate 40g/L, sodium hypophosphite 30g/L, ammonium chloride 30g/L, natrium hydrocitricum 7g/L, sodium pyrophosphate 60g/L, triethanolamine 90g/L, bath pH value is 8,35 DEG C of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 400r/min, the coated thick nickel dam of one deck 0.1 μ m of tungsten powder surface after plating completes;
Step 3, took according to tungsten copper nickel content the copper powder that average grain diameter is 1 μ m than 16: 3: 1, by the tungsten powder of coated nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 1h, then mixed-powder is dried under vacuum condition;
Step 4 is reduced 0.5h by the mixed-powder of gained in step 3 in nitrogen atmosphere, and reduction temperature is 200 DEG C, obtains mixing fully and the mechanical impurity of the metal dust of non-oxidation;
Step 5, is encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 950 DEG C of sintering temperatures, and temperature retention time 5min, programming rate is 150 DEG C/min, exerts pressure as 50MPa, vacuum protection.
The density of the W-Cu-Ni alloy making by the method is that 97.55%, W-W connection degree is 27%.
Embodiment 2
A kind of tungsten-copper-nickel alloy material, alloying component and content (mass percent): 75%W-20%Cu-5%Ni, its preparation method comprises the following steps:
Step 1, selecting average grain diameter is the tungsten powder 20g of 6 μ m, first utilizes 60mL/LHCl to carry out alligatoring, alligatoring 12h, recycling 30g/LSnCl2Carry out sensitization with 50mL/LHCl, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl2Activate with 10mL/LHCl, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, takes six hydration nickel sulfate by tungsten nickel weight ratio at 15: 1, and preparation solution composition is six hydration nickel sulfate 40g/L, sodium hypophosphite 30g/L, ammonium chloride 30g/L, natrium hydrocitricum 7g/L, sodium pyrophosphate 60g/L, triethanolamine 90g/L, bath pH value is 8,35 DEG C of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 400r/min, the coated thick nickel dam of one deck 0.2 μ m of tungsten powder surface after plating completes;
Step 3, took according to tungsten copper nickel content the copper powder that average grain diameter is 1 μ m than 15: 4: 1, by the tungsten powder of coated nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 1h, then mixed-powder is dried under vacuum condition;
Step 4 is reduced 0.5h by the mixed-powder of gained in step 3 in nitrogen atmosphere, and reduction temperature is 200 DEG C, obtains mixing fully and the mechanical impurity of the metal dust of non-oxidation;
Step 5, is encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 950 DEG C of sintering temperatures, and temperature retention time 5min, programming rate is 150 DEG C/min, exerts pressure as 50MPa, vacuum protection.
The density of the W-Cu-Ni alloy making by the method is that 97.65%, W-W connection degree is 29%.
Embodiment 3
A kind of tungsten-copper-nickel alloy material, alloying component and content (mass percent): 70%W-25%Cu-5%Ni, its preparation method comprises the following steps:
Step 1, selecting average grain diameter is the tungsten powder 20g of 5 μ m, first utilizes 60mL/LHCl to carry out alligatoring, alligatoring 12h, recycling 30g/LSnCl2Carry out sensitization with 50mL/LHCl, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl2Activate with 10mL/LHCl, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, takes six hydration nickel sulfate by tungsten nickel weight ratio at 14: 1, and preparation solution composition is six hydration nickel sulfate 30g/L, sodium hypophosphite 40g/L, ammonium chloride 30g/L, natrium hydrocitricum 10g/L, sodium pyrophosphate 50g/L, triethanolamine 120g/L, bath pH value is 9,40 DEG C of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 350r/min, the coated thick nickel dam of one deck 0.3 μ m of tungsten powder surface after plating completes;
Step 3, took according to tungsten copper nickel content the copper powder that average grain diameter is 0.5 μ m than 14: 5: 1, by the tungsten powder of coated nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 1.5h, then mixed-powder is dried under vacuum condition;
Step 4 is reduced 0.5h by the mixed-powder of gained in step 3 in nitrogen atmosphere, and reduction temperature is 240 DEG C, obtains mixing fully and the mechanical impurity of the metal dust of non-oxidation;
Step 5, is encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 900 DEG C of sintering temperatures, and temperature retention time 8min, programming rate is 100 DEG C/min, exerts pressure as 30MPa, vacuum protection.
The density of the W-Cu-Ni alloy making by the method is that 97.51%, W-W connection degree is 26%.
Embodiment 4
A kind of tungsten-copper-nickel alloy material, alloying component and content (mass percent): 65%W-25%Cu-10%Ni, its preparation method comprises the following steps:
Step 1, selecting average grain diameter is the tungsten powder 20g of 4 μ m, first utilizes 60mL/LHCl to carry out alligatoring, alligatoring 12h, recycling 30g/LSnCl2Carry out sensitization with 50mL/LHCl, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl2Activate with 10mL/LHCl, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, takes six hydration nickel sulfate by tungsten nickel weight ratio at 13: 2, and preparation solution composition is six hydration nickel sulfate 20g/L, sodium hypophosphite 20g/L, ammonium chloride 40g/L, natrium hydrocitricum 5g/L, sodium pyrophosphate 70g/L, triethanolamine 100g/L, bath pH value is 10,35 DEG C of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 300r/min, the coated thick nickel dam of one deck 0.4 μ m of tungsten powder surface after plating completes;
Step 3, took according to tungsten copper nickel content the copper powder that average grain diameter is 1 μ m than 13: 5: 2, by the tungsten powder of coated nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 2h, then mixed-powder is dried under vacuum condition;
Step 4 is reduced 0.75h by the mixed-powder of gained in step 3 in nitrogen atmosphere, and reduction temperature is 270 DEG C, obtains mixing fully and the mechanical impurity of the metal dust of non-oxidation;
Step 5, is encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 850 DEG C of sintering temperatures, and temperature retention time 10min, programming rate is 50 DEG C/min, exerts pressure as 40MPa, vacuum protection.
The density of the W-Cu-Ni alloy making by the method is that 97.85%, W-W connection degree is 28%.
Embodiment 5
A kind of tungsten-copper-nickel alloy material, alloying component and content (mass percent): 65%W-25%Cu-10%Ni, its preparation method comprises the following steps:
Step 1, selecting average grain diameter is the tungsten powder 20g of 4 μ m, first utilizes 60mL/LHCl to carry out alligatoring 12h, recycling 30g/LSnCl2Carry out sensitization with 50mL/LHCl, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl2Activate with 10mL/LHCl, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, takes six hydration nickel sulfate by tungsten nickel weight ratio at 13: 2, and preparation solution composition is six hydration nickel sulfate 30g/L, sodium hypophosphite 30g/L, ammonium chloride 35g/L, natrium hydrocitricum 7g/L, sodium pyrophosphate 60g/L, triethanolamine 100g/L, bath pH value is 10,35 DEG C of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 300r/min, the coated thick nickel dam of one deck 0.4 μ m of tungsten powder surface after plating completes;
Step 3, took according to tungsten copper nickel content the copper powder that average grain diameter is 0.5 μ m than 13: 5: 2, by the tungsten powder of coated nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 2h, then mixed-powder is dried under vacuum condition;
Step 4 is reduced 1h by the mixed-powder of gained in step 3 in nitrogen atmosphere, and reduction temperature scope is 300 DEG C, obtains mixing fully and the mechanical impurity of the metal dust of non-oxidation;
Step 5, is encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 850 DEG C of sintering temperatures, and temperature retention time 10min, programming rate is 50 DEG C/min, exerts pressure as 20MPa, vacuum protection.
The density of the W-Cu-Ni alloy making by the method is that 97.66%, W-W connection degree is 29%.
Claims (4)
1. a low W-W connection degree W-Cu-Ni alloy material, is characterized in that: the one-tenth of W-Cu-Ni alloyDivide and be by mass percentage: W content 65%, Cu content 25%, Ni content 10% or W content 80%,Cu content 15%, Ni content 5%;
The density of prepared W-Cu-Ni alloy is more than 97.5%, and W-W connection degree is less than 30%.
2. material as claimed in claim 1, is characterized in that: described material is to be prepared into by following processArrive:
(1) adopt the method for chemical nickel plating to prepare the coated tungsten composite powder of nickel, recycling is planetary without abrading-ballBall mill is by coated nickel tungsten composite powder and copper powder wet mixing 1～2h;
(2) alloying element powder mixing in (1) is reduced in hydrogen atmosphere to 0.5～1h, reductionTemperature range is 200～300 DEG C, obtains mixing fully and the mechanical impurity of the metal dust of non-oxidation;
(3) adopt discharge plasma sintering technique to carry out sintering, sintering temperature to gained mixed-powder in (2)Degree is 850～950 DEG C, and exerting pressure is 20～50MPa, and temperature retention time is 5～10min, and sintering atmosphere is trueSky, finally obtains density more than 97.5%, the W-Cu-Ni alloy that W-W connection degree is less than 30%.
3. material as claimed in claim 2, is characterized in that: six hydration nickel sulfate concentration in chemical plating bathScope is that 20～40g/L, hypophosphorous acid hydrogen na concn scope are that 20～40g/L, ammonium chloride concentration scope are30～40g/L, sodium pyrophosphate concentration range are that 50～70g/L, sodium citrate concentration scope are 5～10g/L, three secondHydramine concentration range is 90～120g/L, and bath temperature is 35～40 DEG C, and pH value is 8～10, chemical plating platingTime is 20～40min.
4. material as claimed in claim 2, is characterized in that: selecting Tungsten Powder Size is 4～6 μ m, copper powder grainFootpath is 0.5～1 μ m.
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| CN104174854B (en) * | 2014-07-14 | 2016-08-24 | 昆山安泰美科金属材料有限公司 | A kind of method preparing miniature tungsten-bast alloy part |
| CN105057681B (en) * | 2015-07-29 | 2018-03-30 | 昆山德泰新材料科技有限公司 | A kind of preparation method of tungsten-copper-nickel alloy powder |
| CN104999077B (en) * | 2015-08-05 | 2017-10-31 | 北京科技大学 | A kind of high-density alloy composite granule and preparation method thereof |
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| CN109454229B (en) * | 2019-01-07 | 2019-12-10 | 广东省材料与加工研究所 | Pomegranate type tungsten alloy powder and preparation method and application thereof |
| CN111390195B (en) * | 2020-03-27 | 2022-05-24 | 陕西理工大学 | Micro-interface quantum scattering-free tungsten-copper alloy and preparation method and application thereof |
| CN114393211B (en) * | 2021-12-15 | 2024-04-05 | 西安理工大学 | Method for preparing CuW/low carbon steel integral material by using copper-nickel powder interlayer |
| CN116652179B (en) * | 2023-07-28 | 2023-10-13 | 安徽诺星航空科技有限公司 | Tungsten-copper alloy composite material and preparation process thereof |
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| CN102433480A (en) * | 2011-12-01 | 2012-05-02 | 北京理工大学 | Tungsten-copper alloy with low skeleton connectivity and preparation method thereof |
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