Method for preparing ultra-fine crystal grain tungsten-copper alloy and tungsten-copper alloy

A tungsten-copper alloy and ultra-fine grain technology is applied in the field of preparing ultra-fine-grain tungsten-copper alloy and ultra-fine-grain tungsten-copper alloy, which can solve the problems of coarse grain, low degree of densification and poor alloy performance. , to achieve the effect of improving mechanical properties, uniform product organization, and improving electrical and thermal conductivity.

Inactive Publication Date: 2007-11-28
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the problems of coarse grains, low degree of densification and poor alloy properties in traditional alloys, the technical solution of the present invention is to combine concentrated HNO 3 Add Cu(NO 3 ) 2 solution, and then the mixed solution was added to (NH 4 ) 2 WO 4 Chemical precipitation reaction in solution in a magnetic stirrer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] First, weigh 320 g of ammonium tungstate solution (ammonium tungstate content 28.2%) and place it in an electronic stirrer. Under stirring conditions (rotation speed: 1000 rpm, stirring time: 60 min.), Cu(NO 3 ) 2 Mixture of solution and concentrated nitric acid (concentration 68%) (55gCu(NO 3 ) 2 ·5H 2 O, 75g concentrated nitric acid) was added to ammonium tungstate solution for chemical precipitation reaction, and then the precipitate was calcined at 150°C for 3 hours, ground and crushed, and the resulting tungsten copper oxide composite powder was placed in a gas-permeable strong drainage tube furnace H 2 Reduction in atmosphere (reduction temperature: 650℃, reduction time: 1.5h, hydrogen flow rate: 45ml·min -1 cm -2 ) Obtain nano-tungsten-copper mixed powder (average crystal grain≤40nm). The mixed powder is loaded into a steel mold for compression under a pressure of 150MPa, and the compact is sintered in a hydrogen furnace at a heating rate of 10°C / min, a sintering tem...

Embodiment 2

[0027] First, weigh 320g of ammonium tungstate solution (28.2% ammonium tungstate) and place it in an electronic stirrer, and add Cu(NO 3 ) 2 Mixture of solution and concentrated nitric acid (concentration 68%) (55gCu(NO 3 ) 2 ·5H 2 O, 75g concentrated nitric acid was added to the ammonium tungstate solution under stirring conditions (rotation speed: 1500rpm, stirring time: 90min.) for chemical precipitation reaction. Then, the precipitate was dried at 200°C for 2.3 hours and then ground and crushed. The resulting tungsten copper oxide composite powder was placed in a gas-permeable and strong drainage tube furnace H 2 Reduction in atmosphere (reduction temperature: 700℃, reduction time: 1.3h, hydrogen flow rate: 40ml·min-1 cm -2 ) Obtain nano-tungsten-copper mixed powder (average crystal grain≤50nm). The mixed powder is loaded into a steel mold for compression under a pressure of 180MPa, and the compact is sintered in a hydrogen furnace at a heating rate of 10°C / min, a sintering t...

Embodiment 3

[0029] Weigh 320g of ammonium tungstate solution (ammonium tungstate content 28.2%) and place it in an electronic stirrer. Under stirring conditions (rotation speed: 1700rpm, stirring time: 90min), add Cu(NO 3 ) 2 Mixture of solution and concentrated nitric acid (concentration 68%) (55gCu(NO 3 ) 2 ·5H 2 O, 75g concentrated nitric acid) was added to the above ammonium tungstate solution for chemical precipitation reaction. Then, the precipitate was dried at 300°C for 1.8 hours and then crushed by grinding. The obtained tungsten copper oxide composite powder was placed in a gas-permeable and strong-draining tube furnace H 2 Reduction in atmosphere (reduction temperature: 750℃, reduction time: 1h, hydrogen flow rate: 35ml·min -1 cm -2 ) Obtain nano-tungsten-copper mixed powder (average crystal grain≤50nm). The mixed powder is loaded into a steel mold and pressed under a pressure of 230MPa. The compact is sintered in a hydrogen furnace at a heating rate of 10°C / min, a sintering temper...

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Abstract

A method to prepare ultra-fine grain tungsten-copper alloy and the tungsten-copper alloy, it belongs to powder metallurgy technology field. The solution of concentrated HNO3 and solution of Cu (NO3)2 will be added into the solution of (NH4)2WO4 at the condition that they are blended, the chemical deposition reaction will occur in the agitator. And then the deposit will be burned and grinded to produce the composite powder of tungsten-copper oxidate. The composite powder will be reduced at low temperature in the pipe furnace, and nanometer tungsten-copper composite powder can be gained, and then they will be pressed to take shape, the pressed compact will be sintered at the protection of H2 and ultra-fine grain tungsten-copper alloy can be gained. The weight percent of copper in a kind of tungsten-copper alloy produced according to the above method is 20%, the relative density of the alloy is 98.0%-99.7%, the average crystal grain size of the tungsten in the alloy is 0.5-1.5 mu m, the electrical resistance of the alloy is 0.035-0.041X10-6omega .m, the heat-transmit index is 200-223W.m-1.k-1. The advantage of it is that. The densification degree of the alloy is high, the tungsten crystal grain is small and uniform, the copper is highly dispersed to compose a compact net. And the flow of it is short, the technology operation is easy and reliable, the production efficiency is high, the energy and production cost is lower, and an industrial production can be carried on according the method.

Description

Technical field [0001] The invention belongs to the technical field of powder metallurgy, and in particular relates to a method for preparing ultrafine grained tungsten-copper alloy and its tungsten-copper alloy. Nano-level tungsten-copper composite oxide powder is prepared by chemical precipitation, and then reduced by hydrogen to obtain nano-tungsten-copper composite Powder, and finally formed and sintered to obtain ultra-fine grained tungsten copper alloy. Background technique [0002] W-Cu composite materials are widely used as electrical contact materials and electrode materials due to their high hardness, good thermal conductivity, electrical conductivity and small thermal expansion coefficient. With the development of microelectronic information technology, in large-scale integrated circuits and high-power microwave devices, W-Cu composite materials have more extensive uses as electronic packaging materials and heat sink materials such as substrates, connectors, and heat d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22C1/04B22F9/18B22F3/16C22C27/04C22C45/10
Inventor 林涛姚惠龙刘祥庆邵慧萍罗骥郭志猛郝俊杰
Owner UNIV OF SCI & TECH BEIJING
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