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Wolfram-copper composite powder preparation method

A technology of composite powder and mixed liquid, which is applied in the field of powder preparation, can solve problems such as poor sintering performance and difficulty in reducing preparation costs, and achieve good sintering stability, low degree of agglomeration, and scientific preparation methods.

Inactive Publication Date: 2013-06-05
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, both the preparation method and the obtained tungsten-copper composite powder have shortcomings. First, the preparation method requires both spray drying and hydrogen reduction, which makes it difficult to reduce the preparation cost; secondly, the obtained tungsten-copper composite powder by Cu 0.4 W 0.6 phase and Cu phase composition, rather than the uniform distribution of W and Cu phases, due to the Cu in the tungsten-copper composite powder 0.4 W 0.6 The existence of the phase makes its sintering performance poor, which can be caused by Cu 0.4 W 0.6 The size of the primary grains of the phase is only 33nm, and the particle size of W after sintering into a bulk is close to 0.8μm, which is confirmed

Method used

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  • Wolfram-copper composite powder preparation method
  • Wolfram-copper composite powder preparation method
  • Wolfram-copper composite powder preparation method

Examples

Experimental program
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Embodiment 1

[0020] The concrete steps of preparation are:

[0021] Step 1, first mix water, copper nitrate, tartaric acid, ammonium paratungstate and citric acid according to the molar ratio of 440:0.9:2:0.067:1.620, and stir at 50°C for 7h; wherein, the water is deionized water, and Mixture. Then add polyethylene glycol to the mixture, and stir at 60°C until it forms a gel; wherein, the molar ratio of polyethylene glycol to copper nitrate in the mixture is 0.0022:0.9, and polyethylene glycol is polyethylene glycol. Ethylene glycol 20000.

[0022] In step 2, the gel was first dried at 100°C for 16 hours to obtain a dry gel, and then the dry gel was placed at 290°C for 4.5 hours and 540°C for 5.5 hours to obtain an intermediate product. Next, the intermediate product was placed in a reducing gas atmosphere, and reduced at 760 ° C for 5 h; wherein, the reducing gas was hydrogen, and the following figure 1 c. Approximate to image 3 and Figure 4 shown, and as figure 2 The tungsten-co...

Embodiment 2

[0024] The concrete steps of preparation are:

[0025] Step 1, first mix water, copper nitrate, tartaric acid, ammonium paratungstate and citric acid according to the molar ratio of 445:0.95:2:0.115:2.781, and then stir at 53°C for 6.5h; wherein, the water is deionized water, to obtain a mixture. Add polyethylene glycol to the mixture, and stir at 63°C until it forms a gel; wherein, the molar ratio of polyethylene glycol to copper nitrate in the mixture is 0.0023:0.95, and polyethylene glycol is polyethylene glycol. Ethylene glycol 20000.

[0026] In step 2, the gel was dried at 105°C for 15 hours to obtain a dry gel, and then the dry gel was placed at 295°C for 4.3 hours and 545°C for 5.3 hours to obtain an intermediate product. Next, put the intermediate product in a reducing gas atmosphere, and reduce it at 770°C for 4.5 hours; wherein, the reducing gas is hydrogen, and the obtained product is approximately figure 1 b. image 3 and Figure 4 shown, and as figure 2 Th...

Embodiment 3

[0028] The concrete steps of preparation are:

[0029] Step 1, first mix water, copper nitrate, tartaric acid, ammonium paratungstate and citric acid according to the molar ratio of 450:1:2:0.164:3.942, and then stir at 55°C for 6h; wherein, the water is deionized water to obtain Mixture. Then add polyethylene glycol to the mixed solution, and stir it at 65°C until it forms a gel; wherein, the molar ratio of polyethylene glycol to copper nitrate in the mixed solution is 0.0024:1, and polyethylene glycol is polyethylene glycol. Ethylene glycol 20000.

[0030] In step 2, the gel was first dried at 110° C. for 14 hours to obtain a dry gel, and then the dry gel was placed at 300° C. for 4 hours and 550° C. for 5 hours to obtain an intermediate product. Next, the intermediate product is placed in a reducing gas atmosphere, and reduced at 780 ° C for 4 h; wherein, the reducing gas is hydrogen, and the following figure 1 b. image 3 and Figure 4 shown, and as figure 2 The tun...

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Abstract

The invention discloses a wolfram-copper composite powder preparation method. Water, copper nitrate, tartaric acid, ammonium paratungstate and citric acid are mixed according to the molar ratio of 440-460: 0.9-1.1: 2: 0.067-0.26: 1.620-6.264 and are stirred for at least five hours under the condition of 50 DEG C-60 DEG C, and mixed liquor is obtained. Polyethylene glycol is added into the mixed liquor. The polyethylene glycol and the mixed liquor are stirred to form gel under the condition of 60 DEG C-70 DEG C, wherein the molar ratio between the polyethylene glycol and the mixed liquor is 0.0022-0.0026: 0.9-1.1. After that, the gel is put under 100 DEG C-200 DEG C and is dried for at least twelve hours, and xerogel is obtained. The xerogel is put under 290 DEG C-310 DEG C for 3.5h-4.5 h, 540 DEG C-560 DEG C for 4.5h-5.5 h and intermediate products are obtained. Then, the intermediate products are put in reducing gas atmosphere and are reduced at least 3h, granular wolfram-copper composite powders are obtained, wherein the weight percentage of the wolfram and the copper is 70-90 wt% : 10-30 wt%. Grain sizes of the wolfram and the copper are 100nm-1Mum. The wolfram-copper composite powders can be used as nuclear fusion plasma facing materials.

Description

technical field [0001] The invention relates to a method for preparing powder, in particular to a method for preparing tungsten-copper composite powder. Background technique [0002] Tungsten-copper functional composite materials have excellent comprehensive properties such as high melting point of tungsten, low thermal expansion coefficient, low sputtering rate and high electrical and thermal conductivity of copper, and are considered to be the most promising plasma materials for nuclear fusion. Recently, people have made unremitting efforts in order to obtain it, as in "Preparation and Sintering of W-20wt% Cu Ultrafine Composite Powder (Nano Processing Technology, Volume 4, Issue 5, October 2007, Fan Jinglian et al. ) the 36th to 38th pages of the article discloses a preparation method of tungsten-copper composite powder. The preparation method mentioned in the paper adopts the spray drying-hydrogen reduction method; the composite powder obtained is composed of tungsten an...

Claims

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Application Information

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IPC IPC(8): B22F9/26
Inventor 周燕孙钦星刘瑞郝汀张涛王先平方前锋
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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