Method for analyzing content and distribution of Cr in Cr-doped zinc sulfide crystalline material

A crystal material, zinc sulfide technology, applied in the field of analytical chemistry, can solve the problems of unavailability, easy pollution, tedious and time-consuming, etc., achieve accurate quantitative analysis, high sensitivity, and avoid the effect of sample pretreatment process

Inactive Publication Date: 2016-05-04
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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Problems solved by technology

[0004] In order to overcome the shortcomings of the chemical pretreatment process, such as tedious and time-consuming, easy to pollute, and unable to provide element distribution information, the present invention provides a practical Cr:ZnS crystal material with laser ablation-inductive coupling for the quantification and distribution of doped element Cr. Plasma mass spectrometry method

Method used

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  • Method for analyzing content and distribution of Cr in Cr-doped zinc sulfide crystalline material
  • Method for analyzing content and distribution of Cr in Cr-doped zinc sulfide crystalline material
  • Method for analyzing content and distribution of Cr in Cr-doped zinc sulfide crystalline material

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preparation example Construction

[0024] Regarding the preparation of solid standard substances, the ZnS matrix material can be grown by vapor deposition, and the surface of the ZnS matrix material can be plated with a uniform thickness and dense Cr film by the magnetic filtration ion plating method. The ZnS matrix material plated with Cr film is diffused at 950° C. for more than 14 days in the tube, and it is obtained by grinding and polishing after the diffusion is completed. Specifically, the above preparation method refers to FangZhenyietal (FangZhenyi, ChaiYichao, HaoYongliang, YangYaoyuan, DongYanping, YanZewu, TianHongchang, XiaoHongtao, WangHeming.JournalofCrystalGrowth, 2002, 237-239:1707-1710), A.F.Shchurov. Ikonnikov, E.V.Yashina, A.N.Sysoev, D.N.Shevarenkov. Inorganic Materials, 2004, 40(4):336–339), Zhu Tufu et al (Zhu Tufu, Shen Liru, Xu Guidong, Jin Fanya. China Surface Engineering, 2008, 4( 21): 27-35) and other methods. In the solid standard substance, there is the following relationship betw...

Embodiment 1

[0037] (1) Preparation of Cr:ZnS solid standard substance

[0038] Solid standard substances were prepared by thermal diffusion method. The preparation steps include: first growing a ZnS matrix material by a vapor deposition (CVD) method, and then plating a uniform and dense Cr film on the surface of the ZnS matrix by using a magnetic filter ion plating (FAD) method. The material is then encapsulated in vacuum quartz tubes (-1 Pa), diffused at a high temperature of 950°C for more than 2 weeks to obtain a uniformly doped crystal material. Polishing is performed after the diffusion process.

[0039] (2) LA-ICP-MS instrument parameters and joint analysis

[0040] The optimized instrument parameters are as follows: laser ablation adopts Cetac213nm Nd:YAG laser sampling system, laser wavelength is 213nm, laser energy is 50%, laser frequency is 10Hz, laser beam spot is 1000μm, scan rate is 50μm / s, helium gas flow rate is 0.6L / min; ICP-MS is a ThermoXseries II CCT quadrupole, arg...

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Abstract

The invention relates to a method for analyzing the content and distribution of Cr in a Cr-doped zinc sulfide crystalline material. According to the method, laser denudation inductively coupled plasma massspectrometry is utilized for analyzing the content and distribution of Cr in the Cr-doped zinc sulfide crystalline material. The method comprises the step that 1, the surface of a ZnS matrix material is plated with a Cr film to prepare a plurality of Cr:ZnS solid standard substances with different Cr contents, wherein Cr is evenly distributed in the Cr:ZnS solid standard substances; 2, the contents of Cr in the solid standard substances are obtained through inductively coupled plasma atomic emission spectrometry or the inductively coupled plasma massspectrometry, the response signal strength of Cr in the solid standard substances is measured through the laser denudation inductively coupled plasma massspectrometry, and a Cr standard work curve is drawn; 3, laser denudation inductively coupled plasma mass spectrometric detection is carried out on a Cr-doped zinc sulfide crystalline material sample to be detected, and the content and distribution of Cr in the sample to be detected are obtained.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a laser ablation-inductively coupled plasma mass spectrometry analysis method for analyzing Cr content and distribution in a Cr-doped zinc sulfide (Cr:ZnS) crystal material by introducing a solid sample. Background technique [0002] As a tunable mid-infrared solid-state laser material at room temperature, Cr:ZnS crystal material has a wide range of applications in the fields of environmental monitoring, atmospheric remote sensing, medical treatment, and laser communication. The content and uniformity of the doping element Cr are important indicators for evaluating the properties of crystals. The inhomogeneous / gradient distribution of doping elements in the material preparation process has always been an important problem that plagues material preparation. Therefore, accurate determination of Cr content and distribution is of great significance for crystal preparation and perform...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N1/28G01N27/626
CPCG01N1/28G01N27/628
Inventor 朱燕汪正李超宇张国震屈海云寇华敏
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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