CN102433480A - Tungsten-copper alloy with low skeleton connectivity and preparation method thereof - Google Patents
Tungsten-copper alloy with low skeleton connectivity and preparation method thereof Download PDFInfo
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- CN102433480A CN102433480A CN2011103905488A CN201110390548A CN102433480A CN 102433480 A CN102433480 A CN 102433480A CN 2011103905488 A CN2011103905488 A CN 2011103905488A CN 201110390548 A CN201110390548 A CN 201110390548A CN 102433480 A CN102433480 A CN 102433480A
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Abstract
The invention discloses a tungsten-copper alloy with low skeleton connectivity and a preparation method thereof. The tungsten-copper alloy contains 60 to 80 percent of W and 20 to 40 percent of Cu. The method comprises the following steps of: 1, selecting the particle diameter of tungsten powder; 2, pre-treating the tungsten powder, namely calculating the mass of the tungsten according to the mass percentage of the prepared tungsten-copper alloy, weighing the tungsten powder according to the particle diameter selected in the step 1, and performing surface pretreatment on the tungsten powder; 3, preparing composite powder: preparing copper-coated tungsten composite powder by adopting a chemical plating method; 4, mixing powder, namely mixing the copper-coated tungsten composite powder and copper powder in a certain ratio by using a planetary ball mill; and 5, performing final sintering, namely sintering the mixed powder obtained in the step 4 by adopting a spark plasma sintering technology, and thus obtaining the tungsten-copper alloy with low skeleton connectivity. The prepared tungsten-copper alloy has the advantages of uniform components, fine tissues, good electric conductivity and thermal conductivity, low thermal expansion coefficient and good tensile property, and is applied in the fields of electric spark machining, electronic encapsulation and aerospace material preparation.
Description
Technical field
The invention belongs to the powder technology field of metallurgy, relate in particular to a kind of preparation method of low skeleton interconnectedness tungsten-copper alloy.
Background technology
Tungsten-copper alloy has good electrical conductivity, resistance fusion welding and advantages such as HS, high firmness by the pseudo-alloy that copper constituted of the tungsten of HMP, high firmness and high conduction, thermal conductivity, has a wide range of applications in fields such as electronics, military project, space flight at present.Along with science and technology development, industry practice use to the W-Cu material property require increasingly high.
Traditional tungsten-copper alloy is generally by high-temperature liquid-phase sintering process and infiltration method preparation.It is to make its densification through the high-temperature liquid-phase sintering more than the copper fusing point that the high-temperature liquid-phase sintering process prepares tungsten-copper alloy.Be characterized in that production process is simple and easy to control.But that shortcoming is a sintering temperature is higher, sintering time is long, sintered density lower (only for theoretical density 90%～95%) and sintering character are relatively poor, is difficult to satisfy request for utilization.Infiltration method is that tungsten powder is pressed into briquet, and pre-burning at a certain temperature is prepared into the W skeleton with certain density and intensity, and then that fusing point is lower metallic copper fusing penetrates in the W skeleton, thereby obtains the method for fine and close tungsten-copper alloy.But the tungsten-copper alloy that copper content is lower utilizes infiltration method to be difficult to preparation, and uneven distribution takes place copper easily, influences the electrical and thermal conductivity performance and the mechanical property of material.
Along with the development of large-scale integrated circuit, high-power electronic device and aerospace material, the performance of tungsten-copper alloy is also had higher requirement, require material to have: density that (1) is high and density; (2) higher conduction and heat conductivility; (3) better high temperature resistant ablation resistance; (4) better mechanical property, especially tensile strength and toughness.Utilize the tungsten-copper alloy of traditional method preparation to be difficult to satisfy these special requirements.
Utilizing W-Cu composite powder to prepare tungsten-copper alloy can improve the problems referred to above on the part degree, and for example mechanize alloyage, sol-gel method etc. fundamentally are not resolved but composition mixes uneven problem.
Adopt the method for electroless plating to prepare the W-Cu composite powder, coat even, the fine and close copper coating of one deck at tungsten powder surface.Utilize the tungsten-copper alloy of copper cladding tungsten composite powder preparation can avoid the direct contact between the tungsten particle, for the tungsten-copper alloy for preparing low skeleton interconnectedness provides good basis.Principle problems such as the tungsten powder surface processing in the electroless copper process, sedimentation rate have been advanced and originally have been resolved, like Chinese patent ZL200910083113.1.But how significantly to improve thickness of coating in the middle of the actual production tungsten-copper alloy; Make exposure level between the tungsten particle low as far as possible, how the ratio through different powder in the control mixed powder and plasma agglomeration temperature obtain having low skeleton interconnectedness and high stretch can tungsten-copper alloy, also all belong to open question still.
Summary of the invention
In order to overcome the above problems, the object of the present invention is to provide a kind of preparation method with tungsten-copper alloy of low skeleton interconnectedness and high stretch ability.
The composition quality per-cent of low skeleton interconnectedness tungsten-copper alloy of the present invention is: Cu content is 20%～40%, and surplus is W; Preferred 80W%, 20%Cu or 75%W, 25%Cu or 70%W, 30%Cu or 65%W, 35%Cu or 60%W, 40%Cu.
The preparation method of the above-mentioned tungsten-copper alloy with low skeleton interconnectedness and high stretch ability is following:
Step 1: select the tungsten powder (2～6 μ m) of suitable grain size, utilize HCl, SnCl
2, PdCl
2Original tungsten powder is carried out activation and sensitization, and acvator is HCl and SnCl
2, concentration is 5%～30%, soak time is 30～50min; Sensitizing agent is PdCl
2, sensitization time is 30～50min;
Step 2: adopt the method for electroless plating to prepare the copper cladding tungsten composite powder; Bath pH value is 12～14, and temperature is 50～60 ℃, utilizes planetary ball mill that the copper cladding tungsten composite powder is mixed with a certain proportion of copper powder again; Process mixed powder; Massfraction per-cent in the final blending powder is 20%～40% for Cu content, and W content is 60%～80%, ball milling time 1～10h;
Step 3: adopt discharge plasma sintering technique mixed powder to be carried out sintering, 800～1100 ℃ of sintering temperatures, 50～150 ℃/min of temperature rise rate, soaking time 5min, the tungsten-copper alloy that finally obtains having high-compactness and low skeleton interconnectedness.
The composition of above-mentioned chemical plating bath is one or more in the middle of cupric sulfate pentahydrate, Seignette salt, formaldehyde, sodium hydroxide, the second bipyridine.
The present invention it is advantageous that with respect to existing tungsten-copper alloy:
(1) the present invention at first carries out surface preparation to tungsten powder, makes tungsten powder have catalytic activity preferably.Electroless plating master's salt is CuSO
45H
2O, reductive agent are formaldehyde.PH value and temperature of reaction through the adjustment plating bath; Improve the stability of plating bath; And guarantee certain reaction speed, to obtain tissue distribution low copper cladding tungsten composite powder of exposure level evenly and between tungsten-tungsten, this provides good basis for the tungsten-copper alloy that preparation has low skeleton interconnectedness.
(2) in order further to reduce exposure level between the tungsten particle; Before sintering, composite powder is mixed with a certain proportion of copper powder again, mixed powder is put into special mould carry out discharge plasma sintering, discharge plasma sintering is a solid state sintering; Can strengthen tungsten copper two activity of self mutually; Improve two mutually between wetting conditions, effectively utilize the inner self-heating effect of powder and carry out sintering, thereby obtain having the tungsten-copper alloy of low skeleton interconnectedness.
(3) low skeleton interconnectedness tungsten-copper alloy has favorable tissue homogeneity and higher density, satisfies the requirement of electrode with tungsten-copper alloy high-compactness, high uniformity, electric-conductivity heat-conductivity high property and good high temperature resistant ablation resistance; Simultaneously, low skeleton interconnectedness tungsten-copper alloy is main in plastic history to rely on the slippage of copper phase to coordinate bulk deformation, thereby has good plastic deformation ability, satisfies tungsten-copper alloy and is applied to mechanics requirement specific in space flight and the mechanical field.
Description of drawings
Fig. 1 is the whole pattern of copper cladding tungsten composite powder;
Fig. 2 is a copper cladding tungsten composite powder granule-morphology;
Fig. 3 is the whole pattern of low skeleton interconnectedness tungsten-copper alloy;
Fig. 4 is the local pattern that amplifies of low skeleton interconnectedness tungsten-copper alloy.
Embodiment
Embodiment 1
1, selecting diameter is the tungsten powder of 4 μ m, utilizes HCl, SnCl
2, PdCl
2Original tungsten powder is carried out activation and sensitization, and acvator is HCl and SnCl
2, concentration is 10%, soak time is 30min; Sensitizing agent is PdCl
2, sensitization time is 30min;
2, adopt the method for electroless plating to prepare the copper cladding tungsten composite powder; Bath pH value is 13, and temperature is 50 ℃, utilizes planetary ball mill that the copper cladding tungsten composite powder is mixed with a certain proportion of copper powder again; Process mixed powder; Massfraction per-cent in the final blending powder is 20% for Cu content, and W content is 80%, ball milling time 4h;
3, adopt discharge plasma sintering technique mixed powder to be carried out sintering, 800 ℃ of sintering temperatures, 50 ℃/min of temperature rise rate, soaking time 5min, the tungsten-copper alloy that finally obtains having high-compactness and low skeleton interconnectedness.This tungsten-copper alloy density reaches more than 98%, and microstructure is tiny and even, has lower skeleton interconnectedness.
Embodiment 2
1, selecting diameter is the tungsten powder of 4 μ m, utilizes HCl, SnCl
2, PdCl
2Original tungsten powder is carried out activation and sensitization, and acvator is HCl and SnCl
2, concentration is 10%, soak time is 35min; Sensitizing agent is PdCl
2, sensitization time is 35min;
2, adopt the method for electroless plating to prepare the copper cladding tungsten composite powder; Bath pH value is 13, and temperature is 55 ℃, utilizes planetary ball mill that the copper cladding tungsten composite powder is mixed with a certain proportion of copper powder again; Process mixed powder; Massfraction per-cent in the final blending powder is 25% for Cu content, and W content is 75%, ball milling time 4h;
3, adopt discharge plasma sintering technique mixed powder to be carried out sintering, 850 ℃ of sintering temperatures, 100 ℃/min of temperature rise rate, soaking time 5min, the tungsten-copper alloy that finally obtains having high-compactness and low skeleton interconnectedness.This tungsten-copper alloy density reaches more than 98%, and microstructure is tiny and even, has lower skeleton interconnectedness.
Embodiment 3
1, selecting diameter is the tungsten powder of 3 μ m, utilizes HCl, SnCl
2, PdCl
2Original tungsten powder is carried out activation and sensitization, and acvator is HCl and SnCl
2, concentration is 10%, soak time is 40min; Sensitizing agent is PdCl
2, sensitization time is 40min;
2, adopt the method for electroless plating to prepare the copper cladding tungsten composite powder; Bath pH value is 13, and temperature is 60 ℃, utilizes planetary ball mill that the copper cladding tungsten composite powder is mixed with a certain proportion of copper powder again; Process mixed powder; Massfraction per-cent in the final blending powder is 30% for Cu content, and W content is 70%, ball milling time 4h;
3, adopt discharge plasma sintering technique mixed powder to be carried out sintering, 900 ℃ of sintering temperatures, 150 ℃/min of temperature rise rate, soaking time 5min, the tungsten-copper alloy that finally obtains having high-compactness and low skeleton interconnectedness.This tungsten-copper alloy density reaches more than 98.5%, and microstructure is tiny and even, has low skeleton interconnectedness.
Embodiment 4
1, selecting diameter is the tungsten powder of 3 μ m, utilizes HCl, SnCl
2, PdCl
2Original tungsten powder is carried out activation and sensitization, and acvator is HCl and SnCl
2, concentration is 10%, soak time is 45min; Sensitizing agent is PdCl
2, sensitization time is 45min;
2, adopt the method for electroless plating to prepare the copper cladding tungsten composite powder; Bath pH value is 13, and temperature is 60 ℃, utilizes planetary ball mill that the copper cladding tungsten composite powder is mixed with a certain proportion of copper powder again; Process mixed powder; Massfraction per-cent in the final blending powder is 35% for Cu content, and W content is 65%, ball milling time 4h;
3, adopt discharge plasma sintering technique mixed powder to be carried out sintering, 950 ℃ of sintering temperatures, 150 ℃/min of temperature rise rate, soaking time 5min, the tungsten-copper alloy that finally obtains having high-compactness and low skeleton interconnectedness.This tungsten-copper alloy density reaches more than 99%, and microstructure is tiny and even, has low skeleton interconnectedness.
Claims (9)
1. one kind low skeleton interconnectedness tungsten-copper alloy material, it is characterized in that: the composition of tungsten-copper alloy is: W content is 60～80%, and Cu content is 20～40%, and this alloy material combines discharge plasma sintering to prepare through electroless plating.
2. material as claimed in claim 1 is characterized in that: material composition is by mass percentage: 80%W, 20%Cu.
3. material as claimed in claim 1 is characterized in that: material composition is by mass percentage: 75%W, 25%Cu.
4. material as claimed in claim 1 is characterized in that: material composition is by mass percentage: 70%W, 30%Cu.
5. material as claimed in claim 1 is characterized in that: material composition is by mass percentage: 65%W, 35%Cu.
6. material as claimed in claim 1 is characterized in that: material composition is by mass percentage: 60%W, 40%Cu.
7. material as claimed in claim 1; It is characterized in that: said material prepares through following process: (1) adopts the method for electroless plating to prepare the copper cladding tungsten composite powder; Wherein the tungsten powder diameter is 2～6 μ m; Utilize planetary ball mill that the copper cladding tungsten composite powder is mixed with a certain proportion of copper powder again, process mixed powder, ball milling time 1～10h;
(2) adopt discharge plasma sintering technique that mixed powder is carried out sintering, 800～1100 ℃ of sintering temperatures, temperature rise rate is 50～150 ℃/min, soaking time 5min finally obtains having the tungsten-copper alloy of high-compactness and low skeleton degree of connection.
8. a kind of low skeleton interconnectedness tungsten-copper alloy preparation methods as claimed in claim 1 is characterized in that:
(1) tungsten powder (2～6 μ m) of the suitable grain size of selection utilizes HCl, SnCl
2, PdCl
2Original tungsten powder is carried out activation and sensitization, and acvator is HCl and SnCl
2, concentration is 5%～30%, soak time is 30～50min; Sensitizing agent is PdCl
2, sensitization time is 30～50min;
(2) adopt the method for electroless plating to prepare the copper cladding tungsten composite powder; Bath pH value is 12～14, and temperature is 50～60 ℃, utilizes planetary ball mill that the copper cladding tungsten composite powder is mixed with a certain proportion of copper powder again; Process mixed powder; Massfraction per-cent in the final blending powder is 20%～40% for Cu content, and W content is 60%～80%, ball milling time 1～10h;
(3) adopt discharge plasma sintering technique mixed powder to be carried out sintering, 800～1100 ℃ of sintering temperatures, 50～150 ℃/min of temperature rise rate, soaking time 5min, the tungsten-copper alloy that finally obtains having high-compactness and low skeleton interconnectedness.
9. a kind of low skeleton interconnectedness tungsten-copper alloy preparation methods as claimed in claim 8, it is characterized in that: the composition of plating bath is cupric sulfate pentahydrate, Seignette salt, formaldehyde, sodium hydroxide and second bipyridine in the above-mentioned electroless plating process.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103418786A (en) * | 2013-09-10 | 2013-12-04 | 北京理工大学 | Preparation method of W-Cu-Ni alloy material with low W-W connectivity |
| CN104014792A (en) * | 2014-06-20 | 2014-09-03 | 阮秀仕 | Method for adopting spark plasma for sintering high-performance copper tungsten electrical contact materials |
| CN105441764A (en) * | 2015-12-29 | 2016-03-30 | 常熟市良益金属材料有限公司 | Tungsten-based high-density alloy |
| CN103882423B (en) * | 2013-12-25 | 2016-08-17 | 华侨大学 | A kind of method at Cu matrix surface microwave cladding CuW alloy |
| CN106180654A (en) * | 2016-08-05 | 2016-12-07 | 陕西斯瑞新材料股份有限公司 | Discharge plasma sintering prepares the method for infiltration copper-chromium contact material |
| CN106180653A (en) * | 2016-08-05 | 2016-12-07 | 陕西斯瑞新材料股份有限公司 | Discharge plasma sintering prepares the method for copper tungsten contact material |
| CN110699676A (en) * | 2019-11-20 | 2020-01-17 | 哈尔滨工业大学（深圳） | High-strength high-conductivity metal glass composite material and preparation method thereof |
| CN112359236A (en) * | 2020-10-16 | 2021-02-12 | 陕西斯瑞新材料股份有限公司 | Process for preparing high-density tungsten-copper alloy metal material by using tungsten powder |
| CN113025859A (en) * | 2021-03-05 | 2021-06-25 | 北京理工大学 | High-strength high-plasticity tungsten alloy material and preparation method thereof |
| CN113070478A (en) * | 2021-03-26 | 2021-07-06 | 深圳市注成科技股份有限公司 | Tungsten-copper alloy feed, preparation method, tungsten-copper alloy workpiece and manufacturing method |
| CN114086013A (en) * | 2021-11-09 | 2022-02-25 | 北京工业大学 | High-strength high-conductivity ultrafine-grained tungsten-copper composite material and preparation method thereof |
| CN114850471A (en) * | 2022-04-21 | 2022-08-05 | 北京工业大学 | Discontinuous layered bimetal composite material and preparation method thereof |
| CN115161567A (en) * | 2022-07-20 | 2022-10-11 | 内蒙古科技大学 | Preparation method of interface control tungsten filament bundle reinforced copper-based composite material and composite material |
| 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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Cited By (22)
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| CN103418786A (en) * | 2013-09-10 | 2013-12-04 | 北京理工大学 | Preparation method of W-Cu-Ni alloy material with low W-W connectivity |
| CN103882423B (en) * | 2013-12-25 | 2016-08-17 | 华侨大学 | A kind of method at Cu matrix surface microwave cladding CuW alloy |
| CN104014792A (en) * | 2014-06-20 | 2014-09-03 | 阮秀仕 | Method for adopting spark plasma for sintering high-performance copper tungsten electrical contact materials |
| CN104014792B (en) * | 2014-06-20 | 2016-09-28 | 阮秀仕 | The method using discharge plasma sintering high-performance copper tungsten electric contact material |
| CN105441764A (en) * | 2015-12-29 | 2016-03-30 | 常熟市良益金属材料有限公司 | Tungsten-based high-density alloy |
| CN106180654A (en) * | 2016-08-05 | 2016-12-07 | 陕西斯瑞新材料股份有限公司 | Discharge plasma sintering prepares the method for infiltration copper-chromium contact material |
| CN106180653A (en) * | 2016-08-05 | 2016-12-07 | 陕西斯瑞新材料股份有限公司 | Discharge plasma sintering prepares the method for copper tungsten contact material |
| CN106180654B (en) * | 2016-08-05 | 2018-01-12 | 陕西斯瑞新材料股份有限公司 | The method that discharge plasma sintering prepares infiltration copper-chromium contact material |
| CN106180653B (en) * | 2016-08-05 | 2018-01-12 | 陕西斯瑞新材料股份有限公司 | The method that discharge plasma sintering prepares copper tungsten contact material |
| CN110699676A (en) * | 2019-11-20 | 2020-01-17 | 哈尔滨工业大学（深圳） | High-strength high-conductivity metal glass composite material and preparation method thereof |
| CN112359236A (en) * | 2020-10-16 | 2021-02-12 | 陕西斯瑞新材料股份有限公司 | Process for preparing high-density tungsten-copper alloy metal material by using tungsten powder |
| CN112359236B (en) * | 2020-10-16 | 2021-11-02 | 陕西斯瑞新材料股份有限公司 | Process for preparing high-density tungsten-copper alloy metal material by using tungsten powder |
| CN113025859A (en) * | 2021-03-05 | 2021-06-25 | 北京理工大学 | High-strength high-plasticity tungsten alloy material and preparation method thereof |
| CN113025859B (en) * | 2021-03-05 | 2021-12-14 | 北京理工大学 | High-strength high-plasticity tungsten alloy material and preparation method thereof |
| CN113070478A (en) * | 2021-03-26 | 2021-07-06 | 深圳市注成科技股份有限公司 | Tungsten-copper alloy feed, preparation method, tungsten-copper alloy workpiece and manufacturing method |
| CN113070478B (en) * | 2021-03-26 | 2023-08-08 | 深圳市注成科技股份有限公司 | Tungsten-copper alloy feed, preparation method, tungsten-copper alloy workpiece and manufacturing method |
| CN114086013A (en) * | 2021-11-09 | 2022-02-25 | 北京工业大学 | High-strength high-conductivity ultrafine-grained tungsten-copper composite material and preparation method thereof |
| CN114086013B (en) * | 2021-11-09 | 2023-02-07 | 北京工业大学 | High-strength high-conductivity ultrafine-grained tungsten-copper composite material and preparation method thereof |
| CN114850471A (en) * | 2022-04-21 | 2022-08-05 | 北京工业大学 | Discontinuous layered bimetal composite material and preparation method thereof |
| CN115161567A (en) * | 2022-07-20 | 2022-10-11 | 内蒙古科技大学 | Preparation method of interface control tungsten filament bundle reinforced copper-based composite material and composite material |
| 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 |
| 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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Application publication date: 20120502 |