CN103418786A - Preparation method of W-Cu-Ni alloy material with low W-W connectivity - Google Patents
Preparation method of W-Cu-Ni alloy material with low W-W connectivity Download PDFInfo
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- CN103418786A CN103418786A CN2013104105173A CN201310410517A CN103418786A CN 103418786 A CN103418786 A CN 103418786A CN 2013104105173 A CN2013104105173 A CN 2013104105173A CN 201310410517 A CN201310410517 A CN 201310410517A CN 103418786 A CN103418786 A CN 103418786A
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Abstract
The invention discloses a preparation method of a W-Cu-Ni alloy material with low W-W connectivity. The specific process includes the steps that a nickel coating layer is arranged on the surface of micro order tungsten powder in a plating mode through a chemical plating method, the tungsten powder with the surface coated with the nickel layer and copper powder are dispensed and mixed, then spark plasma sintering is conducted on the evenly-mixed powder, and the W-Cu-Ni alloy material with the high density and low W-W connectivity can be prepared. The preparation method of the W-Cu-Ni alloy material with the low W-W connectivity has the advantages that first, the nickel coating layer can improve the interface bonding strength of a tungsten phase and a copper phase, the activated sintering function is further achieved, sintering temperatures are lowered, and meanwhile the density of the material can be better improved; second, by means of the preparation method, the W-Cu-Ni alloy material with the density being larger than 97.5% and the low W-W connectivity being smaller than 30% can be prepared, and the material has excellent tensile mechanical performance. The W-Cu-Ni alloy material has excellent mechanical performance, and is suitable for the fields of aviation and weapons.
Description
Technical field
The invention belongs to metallurgical technology field, relate to the preparation technology of refractory metal, especially a kind of preparation method of W-Cu-Ni alloy of low W-W connection degree.
Background technology
The tungsten-copper alloy material had both had the characteristics 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, therefore was 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, especially the 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, there is no metallurgical binding between W-Cu, bond strength is also very weak, so easily ftracture in W-W interface and W-Cu interface under the stretching loading environment, cause tungsten-copper alloy tensile strength extreme difference.Therefore, in order to improve the tensile strength of tungsten-copper alloy, at first to suppress the formation at W-W interface, reduce W-W connection degree, will realize the metallurgical binding between W-Cu simultaneously, improve the 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, the tungsten alloy of the powder sintered preparation of copper cladding tungsten that utilizes the method to prepare has been avoided the direct contact of W-W, but the bond strength at W-Cu interface does not improve yet.Therefore, how to improve the bond strength at W-Cu interface in W-W connection degree in reducing the W-Cu alloy, the tensile mechanical properties that further improves material becomes problem demanding prompt solution.
Because dissolving each other fully, Ni and Cu can form unlimited solid solution, can form limit solid solution by partial miscibility with W, therefore can coat the Ni layer by W particle top layer mixes with copper powder again, 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, Ni layer and W phase and copper form solid solution between mutually, and the metallurgical junction that can improve between the W-Cu interface is made a concerted effort, and then improves the 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 by said method, can prepare there is good W-Cu interface bond strength, low W-W connections degree and well the high-compactness tungsten copper of tensile mechanical properties be associated gold copper-base alloy.
Summary of the invention
The tungsten-bast alloy the present invention relates to is the W-Cu-Ni alloy material.
The present invention has improved the tensile property of existing tungsten-copper alloy, provides a kind of and has had 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 in conjunction with chemical nickel plating and discharge plasma sintering preparation.
The technical scheme that the present invention takes is: the method by chemical nickel plating coats one deck nickel on the tungsten particle surface, adopt the method for mechanical mixture that the 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, low W-W connection degree and the tiny W-Cu-Ni alloy of crystal grain.Wherein in the W-Cu-Ni alloy, the computing formula of W-W connection degree is:
In formula, C
SSW-W connection degree, N
SSW-W interface number, N
SLIt is W-Cu interface number.N
SSAnd N
SLComputational 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 along this line of horizontal line (vertical curve) number, pass, 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 N
SSAnd N
SL.
For above-mentioned nickel process, its process parameters range is as follows:
The 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 ℃, the pH value is 8～10, and the chemical plating plating time is 20～40min.
Preparation method for above-mentioned W-Cu-Ni alloy material, comprise the steps:
(1) adopt the method for chemical nickel plating to prepare the composite powder that nickel coats tungsten, recycling planetary ball mill (without abrading-ball) coats tungsten composite powder by nickel and mixes 1～2 hour (wet mixing) with a certain proportion of copper powder, 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 mixed reduces 0.5～1h in nitrogen atmosphere, and the reduction temperature scope is 200 ℃～300 ℃, 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 ℃, and exerting pressure is 20～50MPa, and heating rate is 50～150 ℃/min; temperature retention time is 5～10min, and the sintering atmosphere is vacuum protection.
The accompanying drawing explanation
Fig. 1 is the whole pattern that nickel coats tungsten composite powder;
Fig. 2 is the section pattern that the nickel inlayed of dental base acrylic resin powder coats tungsten composite powder;
Fig. 3 is the whole pattern of low W-W connection degree W-Cu-Ni alloy;
Pattern is amplified in the part that Fig. 4 is 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.
The specific embodiment
Below in conjunction with five specific embodiments, the present invention is further understood in exemplary illustration and help.But the 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, and for example simple the change or replacement of technical characterictic to have 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, select the tungsten powder 20g that average grain diameter is 6 μ m, at first utilizes 60mL/LHCl to carry out alligatoring alligatoring 12h, recycling 30g/LSnCl
2Carry out sensitization with 50mL/LHCl, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl
2With 10mL/LHCl, activated, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, by tungsten nickel weight ratio, 16:1 takes six hydration nickel sulfate, and the 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 ℃ of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 400r/min, and after plating completes, tungsten powder surface coats the thick nickel dam of one deck 0.1 μ m;
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 that coats nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 1h, then by mixed-powder drying under vacuum condition;
Step 5, be encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 950 ℃ of sintering temperatures, and temperature retention time 5min, programming rate is 150 ℃/min, exerts pressure as 50MPa, vacuum protection.
The density of the W-Cu-Ni alloy made 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, select the tungsten powder 20g that average grain diameter is 6 μ m, at first utilizes 60mL/LHCl to carry out alligatoring alligatoring 12h, recycling 30g/LSnCl
2Carry out sensitization with 50mL/LHCl, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl
2With 10mL/LHCl, activated, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, by tungsten nickel weight ratio, 15:1 takes six hydration nickel sulfate, and the 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 ℃ of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 400r/min, and after plating completes, tungsten powder surface coats the thick nickel dam of one deck 0.2 μ m;
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 that coats nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 1h, then by mixed-powder drying under vacuum condition;
Step 5, be encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 950 ℃ of sintering temperatures, and temperature retention time 5min, programming rate is 150 ℃/min, exerts pressure as 50MPa, vacuum protection.
The density of the W-Cu-Ni alloy made 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, select the tungsten powder 20g that average grain diameter is 5 μ m, at first utilizes 60mL/LHCl to carry out alligatoring alligatoring 12h, recycling 30g/LSnCl
2Carry out sensitization with 50mL/LHCl, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl
2With 10mL/LHCl, activated, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, by tungsten nickel weight ratio, 14:1 takes six hydration nickel sulfate, and the 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 ℃ of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 350r/min, and after plating completes, tungsten powder surface coats the thick nickel dam of one deck 0.3 μ m;
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 that coats nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 1.5h, then by mixed-powder drying under vacuum condition;
Step 5, be encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 900 ℃ of sintering temperatures, and temperature retention time 8min, programming rate is 100 ℃/min, exerts pressure as 30MPa, vacuum protection.
The density of the W-Cu-Ni alloy made by the method is that 97.51%, W-W connection degree is 26%.
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, select the tungsten powder 20g that average grain diameter is 4 μ m, at first utilizes 60mL/LHCl to carry out alligatoring alligatoring 12h, recycling 30g/LSnCl
2Carry out sensitization with 50mL/LHCl, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl
2With 10mL/LHCl, activated, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, by tungsten nickel weight ratio, 13:2 takes six hydration nickel sulfate, and the 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 ℃ of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 300r/min, and after plating completes, tungsten powder surface coats the thick nickel dam of one deck 0.4 μ m;
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 that coats nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 2h, then by mixed-powder drying under vacuum condition;
Step 5, be encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 850 ℃ of sintering temperatures, and temperature retention time 10min, programming rate is 50 ℃/min, exerts pressure as 40MPa, vacuum protection.
The density of the W-Cu-Ni alloy made 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, select the tungsten powder 20g that average grain diameter is 4 μ m, at first utilize 60mL/LHCl to carry out alligatoring 12h, recycling 30g/LSnCl2 and 50mL/LHCl carry out sensitization, sensitization adopts ultrasonic simultaneously and stirs, and the time is 5min, finally utilizes 0.5g/LPdCl2 and 10mL/LHCl to be activated, activation adopts ultrasonic simultaneously and stirs, and the time is 100min;
Step 2, take six hydration nickel sulfate by tungsten nickel weight ratio at 13: 2, and the 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 ℃ of temperature, and tungsten powder is scattered in plating solution with stirring by ultrasonic in plating solution, mixing speed is 300r/min, and after plating completes, tungsten powder surface coats the thick nickel dam of one deck 0.4 μ m;
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 that coats nickel dam with copper powder at planetary ball mill (without abrading-ball) wet mixing 2h, then by mixed-powder drying under vacuum condition;
Step 5, be encased in the metal powder mixture in step 4 in graphite jig, carries out sintering in discharging plasma sintering equipment, 850 ℃ of sintering temperatures, and temperature retention time 10min, programming rate is 50 ℃/min, exerts pressure as 20MPa, vacuum protection.
The density of the W-Cu-Ni alloy made by the method is that 97.66%, W-W connection degree is 29%.
Claims (6)
1. one kind low W-W connection degree W-Cu-Ni alloy material, it is characterized in that: the composition of W-Cu-Ni alloy is by mass percentage: W content 65%～80%, Cu content 15%～25%, Ni content 5%～10%.
2. material as claimed in claim 1, it is characterized in that: described material prepares by following process:
(1) adopt the method for chemical nickel plating to prepare nickel coating tungsten composite powder, recycling planetary ball mill (without abrading-ball) coats tungsten composite powder and copper powder wet mixing 1～2h by nickel;
(2) alloying element powder mixed in (1) is reduced in hydrogen atmosphere to 0.5～1h, the reduction temperature scope is 200～300 ℃, 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 ℃, exerting pressure is 20～50MPa, temperature retention time is 5～10min, the sintering atmosphere is vacuum, finally obtains having the W-Cu-Ni alloy of high-compactness and low W-W degree of connection.
3. preparation method as claimed in claim 2, it is characterized in that: in chemical plating bath, the 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 ℃, the pH value is 8～10, and the chemical plating plating time is 20～40min.
4. preparation method as claimed in claim 2, it is characterized in that: selecting Tungsten Powder Size is 4～6 μ m, and copper powder size is 0.5～1 μ m.
5. preparation method as claimed in claim 2, it is characterized in that: chemical deposit is nickel dam, and the nickel coating thickness is 0.1～0.5 μ m, and the nickel clad can reduce W-W connection degree; Utilize between nickel and copper the effect that forms partial miscibility between unlimited solid solution and nickel and tungsten simultaneously, make tungsten phase and copper produce metallurgical binding between mutually, the interface bond strength of raising tungsten phase and Cu phase; Nickel can also improve sintering activity, plays the effect that reduces sintering temperature.
6. preparation method as claimed in claim 2, it is characterized in that: the density of prepared W-Cu-Ni alloy is more than 97.5%, and W-W connection degree is less than 30%.
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| CN104174854A (en) * | 2014-07-14 | 2014-12-03 | 昆山安泰美科金属材料有限公司 | Method for manufacturing miniature tungsten-based alloy part |
| CN104999077A (en) * | 2015-08-05 | 2015-10-28 | 北京科技大学 | Composite powder for high gravity alloy and preparation method thereof |
| CN105057681A (en) * | 2015-07-29 | 2015-11-18 | 昆山德泰新材料科技有限公司 | Preparation method for tungsten copper nickel alloy powder |
| CN105861980A (en) * | 2016-05-25 | 2016-08-17 | 广州新莱福磁电有限公司 | Anti-corrosion method for high-gravity alloy |
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| CN114393211A (en) * | 2021-12-15 | 2022-04-26 | 西安理工大学 | Method for preparing CuW/low-carbon steel integral material by utilizing copper-nickel powder interlayer |
| 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 |
| CN116652179A (en) * | 2023-07-28 | 2023-08-29 | 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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