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Method for preparing nano tungsten-copper-rare earth composite powder

A technology of copper rare earth and composite powder is applied in the field of preparation of nanometer tungsten copper rare earth composite powder, which can solve the problems of complex steps of nanometer tungsten copper composite powder, reducing the electrical conductivity and thermal conductivity of materials, and long time of decomposition and reduction process, so as to avoid The effect of copper concentration gradient, compactness and comprehensive performance improvement of materials, inhibiting grain growth

Inactive Publication Date: 2010-11-03
YUNTAI CEMENTED CARBIDE GANZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mechanical alloying method will introduce a certain amount of impurity elements in the powder preparation stage (ball milling stage), and the powder preparation time is long, generally more than 10h, or even 60h; compared with the mechanical alloying method, the mechanochemical method can shorten the powder preparation time and prevent pollution. However, the preparation of nano-tungsten-copper composite powder by this method is complicated, the reduction temperature is high, and the energy consumption is large; the solution of the spray drying method is uniformly dispersed, preventing component segregation, and the obtained oxide particles are mostly spherical, with good fluidity and easy handling. , but there is a relatively long time for the decomposition and reduction process, which takes about 10 hours
In addition, some scholars add additives such as Ni and Pd to improve the wettability of the powder, but reduce the electrical and thermal conductivity of the material.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Weigh 630g Cu(NO 3 ) 2 ·3H 2 O, 356g ammonium metatungstate dissolved in 1830g H 2 In O, a mixed solution with a concentration of about 30% is prepared;

[0023] 2) Add a nitric acid solution with a concentration of 50% to adjust the pH value of the above solution to 3;

[0024] 3) Add 2g of yttrium nitrate and stir evenly to obtain a higher saturation solution or near colloid;

[0025] 4) The solution or sol pressure spray dryer is spray-dried, the inlet air temperature of the spray drying is 200°C ~ 250°C, the outlet air temperature is 180°C ~ 200°C, and the feed flow rate is 300ml / min to obtain the precursor powder;

[0026] 5) The precursor powder is calcined in a high-temperature rapid decomposition furnace, which uses a fluidized bed to fluidize the precursor solid powder and transport it through a heat-resistant pipeline. A heating device is installed outside the pipeline to calcin the precursor powder Then enter a receiving device, the calcination temperature is 800 ...

Embodiment 2

[0029] 1) Weigh 236g Cu(NO 3 ) 2 ·3H 2 O, 356g ammonium metatungstate dissolved in 755g H 2 In O, prepare a mixed solution with a concentration of about 40%;

[0030] 2) Add a 50% hydrochloric acid solution to adjust the pH of the above solution to 4;

[0031] 3) Add 3g of cerium nitrate and stir evenly to obtain a higher saturation solution or near colloid;

[0032] 4) Spray drying the solution or sol. The inlet air temperature of the spray drying is 200°C ~ 250°C, the outlet air temperature is 180°C ~ 200°C, and the feed flow rate is 200ml / min to obtain the precursor powder;

[0033] 5) The precursor powder is calcined in a high-temperature rapid decomposition furnace, the calcining temperature is 1100°C, and the calcining time is 7 minutes to obtain nano-scale tungsten copper rare earth oxide composite powder;

[0034] 6) Reduce the tungsten-copper rare-earth oxide composite powder in a reduction device with "hydrogen + nitrogen" at 750°C for 50 minutes to obtain a copper-containing ...

Embodiment 3

[0036] 1) Weigh 630g Cu(NO 3 ) 2 ·3H 2 O, 60g ammonium metatungstate dissolved in 2055g H 2 In O, prepare a mixed solution with a concentration of about 20%;

[0037] 2) Adding a 50% concentration of nitric acid + hydrochloric acid mixed solution to adjust the pH value of the above solution to 5;

[0038] 3) Add 1g of gadolinium nitrate and stir evenly to obtain a solution or near colloid with higher saturation;

[0039] 4) Spray drying the solution or sol. The inlet air temperature of spray drying is 250℃~300℃, the outlet temperature is 180℃~200℃, and the feed flow rate is 400ml / min to obtain the precursor powder;

[0040] 5) Calcining the precursor powder in a high-temperature rapid decomposition furnace at a calcination temperature of 1200°C and a calcination time of 5 minutes to obtain nano-scale tungsten copper rare earth oxide composite powder;

[0041] 6) The tungsten copper rare earth oxide composite powder is reduced with pure hydrogen at 900° C. for 30 min in a reduction devic...

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Abstract

The invention discloses a method for preparing nano tungsten-copper-rare earth composite powder, in particular a method for preparing nano tungsten-copper-rare earth composite powder by adopting gelling-spraying drying-high-temperature instant decomposition technology. In the invention, in order to improve the granularity, uniformity and compactness of the tungsten-copper composite powder and the comprehensive performance of the material, reduce the power consumption of the production and shorten the production period, micro rare earth alloy elements are added into a mixing process of the original solution of the invention to thin the crystal particles and improve the compactness of the sintered powder, and the novel high-temperature instant decomposition technology is used to restrain the growth of the crystal particles, reduce the energy consumption and copper consumption and improve the uniformity of the tungsten-copper composite powder. The method for preparing the nano tungsten-copper-rare earth composite powder has the characteristics of short production period, low energy consumption and copper consumption, improved granularity, uniformity and compactness of a product and improved comprehensive performance of the material.

Description

Technical field [0001] The invention relates to a method for preparing nano tungsten copper rare earth composite powder, in particular to a method for preparing nano tungsten copper rare earth composite powder by adopting a high-temperature instantaneous decomposition technology. Background technique [0002] Nano-tungsten-copper composite materials have both the excellent characteristics of tungsten and copper, and are widely used in electrode materials, electrical contact materials, electronic packaging materials and heat sink materials, etc. However, tungsten and copper elements do not dissolve each other, have large melting points, poor wettability and The shortcomings of low density after sintering lead to the reduction of the performance of the tungsten copper composite material and the increase of the production cost. [0003] In recent years, the preparation methods of nano-tungsten copper composite powder at home and abroad mainly include mechanical alloying method, mechan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/26
Inventor 钟守正龚云生刘飞飞林静章
Owner YUNTAI CEMENTED CARBIDE GANZHOU
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