Standard sample for analyzing trace elements of high-purity tungsten and preparation method of standard sample

A standard sample and trace element technology, which is applied in the preparation of test samples, material analysis, material analysis by electromagnetic means, etc., can solve the problems of fewer types of elements covered, increase the types of elements, reduce costs, etc., and achieve composition Good uniformity, high accuracy and good stability

Active Publication Date: 2021-10-22
国合通用测试评价认证股份公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Aiming at the problems that the existing high-purity tungsten standard samples are expensive and cover few types of elements, the present invention has deve

Method used

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  • Standard sample for analyzing trace elements of high-purity tungsten and preparation method of standard sample
  • Standard sample for analyzing trace elements of high-purity tungsten and preparation method of standard sample
  • Standard sample for analyzing trace elements of high-purity tungsten and preparation method of standard sample

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Experimental program
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Effect test

Embodiment 1

[0032] Weigh 23kg of ammonium tungstate (purity 4N), high-quality pure manganese nitrate, barium nitrate, cobalt nitrate, cadmium nitrate, chromium nitrate, nickel nitrate, magnesium nitrate, bismuth nitrate, lead nitrate, antimony trioxide, tetrachloride Weigh 3.0g of tin, titanium powder, zinc chloride and strontium chloride.

[0033] Put the above reagents into an evaporating stirrer, evaporate and crystallize while stirring at 103°C for 12 hours, and obtain crude ammonium tungstate crystals with uniform composition. The obtained crystals are subjected to hydrogenation reduction (reduction temperature is 940°C, hydrogen flow rate is 5m3 / h) to obtain pure tungsten powder. The obtained tungsten powder is mechanically stirred, and then mechanically stirred for 150 hours after being crushed by a ball mill, and finally a tungsten powder precursor with a concentrated particle size distribution and uniform chemical composition is obtained.

[0034] The homogenized high-purity tun...

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Abstract

The invention relates to a standard sample for analyzing trace elements of high-purity tungsten and a preparation method of the standard sample, and belongs to the field of analysis and detection of high-purity metals. The standard sample comprises elements of Al, As, B, Ba, Bi, Ca, Cd, Cu, Cr, Co, Fe, Hf, K, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Si, Sn, Sr, Ta, Ti, Zn and Zr, the content of each element is 0.1 ppm to 500 ppm, and the balance is W. The method comprises following steps of: putting the raw materials into an evaporation stirrer to obtain crude ammonium tungstate crystals; performing hydrogenation reduction to obtain tungsten powder; performing mechanical stirring, performing ball-milling crushing, and performing mechanical stirring and mixing again; detecting the content of impurity elements; briquetting and sintering the material; and performing component uniformity inspection and valuing on the chemical standard sample. The high-purity tungsten standard sample obtained by the method disclosed by the invention is regular in shape, uniform in component, good in stability and accurate in fixed value, and can be used for correcting a high-purity tungsten trace element measurement result and monitoring an instrument and equipment state.

Description

technical field [0001] The invention relates to a high-purity tungsten standard sample and a preparation method thereof, in particular to a high-purity tungsten trace element analysis standard sample and a preparation method thereof, belonging to the field of high-purity metal analysis and detection. Background technique [0002] With the development and progress of modern high technology, the demand for key basic materials such as ultra-high-purity rare / precious metals is increasing day by day in the fields of aviation, aerospace, integrated circuits, and high-performance semiconductor lighting. The demand of researchers for the ability to detect trace impurity elements in ultra-high-purity metals is also gradually increasing. To improve the detection ability, the research and development of supporting standard samples is essential. At present, the standard sample of high-purity tungsten can be found to be BAM S002 developed in Germany, with 15 fixed value elements and the...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/38G01N27/626G01N27/68C22C27/04C22C1/04B22F9/22
CPCG01N1/28G01N1/286G01N1/38G01N27/626G01N27/68C22C27/04C22C1/045B22F9/22Y02P10/20
Inventor 李甜陈雄飞张芳张晓孙海峰徐青刘美子张力久李凤艳
Owner 国合通用测试评价认证股份公司
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