CN102854178B - Method for measuring atomic ratio of tellurium elements to cadmium elements in cadmium telluride - Google Patents
Method for measuring atomic ratio of tellurium elements to cadmium elements in cadmium telluride Download PDFInfo
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- CN102854178B CN102854178B CN201210342108.XA CN201210342108A CN102854178B CN 102854178 B CN102854178 B CN 102854178B CN 201210342108 A CN201210342108 A CN 201210342108A CN 102854178 B CN102854178 B CN 102854178B
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Abstract
The invention discloses a method for measuring the atomic ratio of tellurium elements to cadmium elements in cadmium telluride. The method includes dissolving a sample by liquor with HNO3 of 50% in volume percent; testing the mixture by ICP (inductively coupled plasma)-OES (optical emission spectrometry); and comparing signal intensity of the sample with signal intensity of a prepared standard sample by internal standard and increasing sampling frequency and sampling quantity to correct errors caused by signal drifting of an instrument, random change of the signal intensity and unevenness of sampling. By the method, measurement accuracy for the atomic ratio of the tellurium elements to the cadmium elements in the cadmium telluride is greatly improved, relative standard deviation can be controlled to be within 2%, accuracy of a measurement result obtained by the quantitative measuring method is obviously higher than that of a measurement result obtained by an XRF (X-ray fluorescence spectrometry) method or an SEM (scanning electron microscope)-EDS (energy disperse spectroscopy) method conveniently adopted in the industry currently, accordingly, concentration of high-content tellurium in the cadmium telluride can be accurately detected and controlled, and the quality of solar thin-film cells can be guaranteed.
Description
Technical field
The present invention relates to a kind of method measuring tellurium in cadmium telluride, cadmium element atomic ratio.
Background technology
Cadmium telluride is the semiconductor material by II B race Elements C d and VI A race element T e chemical combination, and molecular formula is CdTe.Cadmium telluride can be used for spectral analysis, CO
2the Q modulation, making solar film battery, infrared modulator etc. of laser instrument.
When adopting cadmium telluride to manufacture solar film battery plate, cadmium telluride rete should be rich tellurium autodoping P type, and suitable rich tellurium concentration is one of key factor affecting solar film battery conversion ratio.The Elements Atom of the cadmium telluride of acceptable quality than scope should be:
Cd：Te＝1：（1.000129－1.012856）
So carry out the detection control of the rich tellurium concentration of cadmium telluride, the quality for solar film battery is most important.That is, for tellurium in cadmium telluride, that cadmium element atomic ratio carries out Accurate Measurement is most important.
At present, the popular approach measured tellurium, cadmium element atomic ratio in cadmium telluride mainly contains XRF method and SEM-EDS method.
Wherein, XRF(X fluorescent x ray spectroscopy x) be that the characteristic X-ray energies that sends for different element and wavelength are different, by judging that to the energy of X ray or the measurement of wavelength it is which kind of element sends, carry out the qualitative analysis of element, the intensity of the characteristic X-ray of each element is except outside the Pass the energy and intensity with excitaton source have, also relevant with this element content in the sample to which.According to the intensity of the characteristic X-ray of each element, also the content information of each element can be obtained, thus carry out semi-quantitative analysis, X-ray fluorescence spectra has nothing to do with the chemical binding state of sample, can Direct solid sampling, but the precision of the method is not high, easily by the impact of sample unevenness, especially lower to the sensitivity of light element, the relative standard deviation of the method is generally about 5%.
SEM-EDS(X gamma ray spectrometer) inner electron produces transition under X ray effect, unnecessary energy discharges with the form of X ray, characteristic X-ray has the intrinsic energy of element, after they are launched into power spectrum, energy value according to it just can determine element kind, intensive analysis according to spectrum just can determine its content, owing to lacking standard model, generally can only carry out sxemiquantitative test.When measuring major component content, may be subject to the interference of impurity scattered radiation, the precision of the method is reduced, and its relative standard deviation is generally about 5%.
In sum, in existing mensuration cadmium telluride all there is the larger defect of relative standard deviation in the method for tellurium, cadmium element atomic ratio, all about 5%, can not meet measuring the more and more higher requirement of precision.。
Summary of the invention
Goal of the invention of the present invention is: for above-mentioned Problems existing, provides the assay method of tellurium in the cadmium telluride that a kind of degree of accuracy is high, cadmium element atomic ratio.
The technical solution used in the present invention is such: a kind of method measuring tellurium in cadmium telluride, cadmium element atomic ratio, comprises the following steps:
(1) sample: accurately take testing sample, be accurate to 0.01mg;
(2) sample dissolution constant volume: by taken sample dissolution in percent by volume be the HNO of 50%
3dissolve in solution, then add Sc as internal standard compound and add deionized water, shake up, get part previous solu, add the HNO that percent by volume is 5%
3solution carries out dilution constant volume, obtains testing sample.
(3) test: adopt ICP-OES to test,
Its condition of work is:
Analytical element parameter: Cd – 228.8 nm, Te – 214.2 nm, Sc – 361.3nm;
Carrier gas flux: 0.6-0.7MPa;
Camera temperature≤-45 DEG C;
Generator temperature≤35 DEG C;
Light room temperature 38 ± 0.1 DEG C;
RF power: 1150W;
Pump speed: 50r/min;
Above operating condition parameters is only for reference, and actual result is determined according to instrument degree of optimization;
(4) according to the atomic ratio of test result calculations tellurium, cadmium element.
As preferably: in step (1), when sampling, each sample repeats preparation four parts.
As preferably: in step (2), the dissolution time of sample dissolution is 5 minutes to 1 hour.
As preferably: in step (2), during sample dissolution, the reacting gas supervened will be overflowed.
As preferably: in step (3), adopt sour blank solution to add the method production standard curve of reference material, to check the element to be measured in sour blank solution, control constituent content to be measured in sour blank solution lower than 0.05 μ g/L.
This method adopts internal standard method, by the standard specimen signal intensity of comparative sample signal intensity and preparation, and expands sampling number of times and sampling amount, corrects the error because instrument signal drift, random signal Strength Changes and sampling unevenness cause.
Inductively coupled plasma optical emission spectrometer (ICP-OES) measures tellurium in cadmium telluride, cadmium element atomic ratio: the method is passed through by cadmium telluride sample dissolution in media as well, tellurium after constant volume is quantitative on ICP-OES instrument in Accurate Measurement sample, the amount of cadmium, then by drawing tellurium in cadmium telluride, cadmium element atomic ratio after computing.Its relative standard deviation of measurement result can control within 2%, and be typical accurate quantitative analyses assay method, its accuracy is high.
Certainly, this detection method also may be used for the atomic ratio mensuration of other binary semiconductor compounds.
In sum, owing to have employed technique scheme, the invention has the beneficial effects as follows: the degree of accuracy that the present invention substantially increases tellurium in cadmium telluride, cadmium element atomic ratio measures, relative standard deviation can control within 2%.Aforementioned two semiquantitative determination methods (XRF method and SEM-EDS method) of measurement result accuracy employing usually in current industry of this method for quantitatively determining; Thus accurately can detect and control the rich tellurium concentration of cadmium telluride, ensure the quality of solar film battery.
Embodiment
The present invention is described in detail below.
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment
Measure a method for tellurium in cadmium telluride, cadmium element atomic ratio, comprise the following steps:
1 reagent:
1.1 nitric acid: top grade is pure
1.2 deionized water
Standard specimen solution and element standard specimen solution to be measured in 1.3 Sc
1.3.1Sc inner mark solution (100ppm Sc): acidity is 5%HNO
3, this solution is stored in a FEP bottle,
1.3.2 Cd and Te is with reference to standard specimen solution (Calibrant:Cd/Te=1/1, at/at);
1.3.2.1 112mg(is claimed to be accurate to 0.1mg) high purity cadmium and 128mg(be accurate to 0.1mg) high purity tellurium; Transfer in 100 mL PP bottles;
1.3.2.2 with the nitric acid dissolve of 10mL 50%;
1.3.2.3 5g scandium inner mark solution (100ppm Sc, is obtained by step 1.3.1) is added
1.3.2.4 add deionized water to 100 g;
1.3.2.5 get the above-mentioned solution of 5g, use 5%HNO
3be diluted to 50g;
1.3.2.6 preparation 4 parts of Cd and Te are repeated with reference to standard specimen solution (i.e. SR1, SR2, SR3, SR4);
2, instrument and equipment
2.1 ICP-OES (U.S.'s thermoelectricity)
2.2 analytical balance
2.3 laboratory plastic articles
2.4 liquid-transfering gun
3, analytical procedure
3.1 sample: use clean plastic spoon, claim 240mg CdTe sample (being accurate to 0.1mg), transfer in 100mL PP bottle.Each sample repeats preparation four parts.
3.2 molten sample and constant volume:
3.2.1 10mL 50%HNO is measured with 10mL graduated cylinder
3in solution to each sample bottle, course of dissolution needed 5 minutes to 1 hour, between breaking-in period, unclamped bottle cap gently, and to determine that the gas produced can be overflowed, but solution can not be polluted by environment again;
3.2.2 5g scandium inner mark solution (100ppm Sc, is obtained by step 1.3.1) is added;
3.2.3 add deionized water to 100 g, shake up;
3.2.4 get the above-mentioned solution of 5g, use 5%HNO
3be diluted to 50g;
3.2.5 preparation 4 parts of testing samples (i.e. A, B, C, D) are repeated
3.3 tests:
3.3.1 ICP-OES condition of work:
Carrier gas flux: 0.6-0.7MPa; Camera temperature≤-45 DEG C; Generator temperature≤35 DEG C; Light room temperature 38 ± 0.1 DEG C; RF power: 1150W; Pump speed: 50r/min;
Above data are determined according to instrument degree of optimization;
3.3.2 signal detection mode:
The sample wash time: 25s;
Scanning times: 3 times.
3.3.3 analytical element parameter:
Cd–228.8 nm；Te –214.2 nm；Sc–361.3nm。
3.3.4 sour blank level is checked:
The typical curve using sour blank to add standard making checks that acid is blank, and the constituent content to be measured generally controlled in sour blank should lower than 0.05ug/L.
If 3.3.5 calibration cannot accept:
Check that acid is blank in the same way, if sour blank cannot accept, then should prepare a set of new acidity scale accurate.This checks the blank contaminated chance of acid, and the process preparing acidity scale standard also may cause acidity scale standard contaminated.
3.3.6, during working sample, following order is adopted to detect successively: A, SR1, B, SR2, C, SR3, D, SR4;
3.3.7 the content of Te and Cd in cadmium telluride sample is gone out according to following formulae discovery; Calculate tellurium in cadmium telluride sample, cadmium element atomic ratio again.
Equation (1) and (2) describe the method (unit: mg/g) measuring Te and Cd content in high-purity cadmium telluride with ICP-OES.
（1）
（2）
In formula:
I
te, I
cd, I
scthe intensity of-apparatus measures Te, Cd and Sc out;
Mg
te, mg
cdthe weight (unit: mg) of Te and Cd in-standard reference solution;
G
cdTe---CdTe example weight (unit: g);
G
sc---target weight (unit: g) in Sc;
Sample---CdTe sample;
Standard---standard reference solution;
Measured data and result of calculation following table:
In table: SD is standard deviation, RSD is relative standard deviation.
As can be seen from the table, add up to and carried out 4 times (4 × 2) experiment, totally 32 groups of data, tellurium/cadmium atomic ratio relative standard deviation, all within 2%, illustrates that this analysis measurement result accuracy is high.
Claims (5)
1. measure a method for tellurium in cadmium telluride, cadmium element atomic ratio, it is characterized in that comprising the following steps:
(1) sample: accurately take testing sample, be accurate to 0.01mg;
(2) sample dissolution constant volume: by taken sample dissolution in percent by volume be the HNO of 50%
3solution dissolves, then adds Sc as internal standard compound and add deionized water, shakes up, gets part previous solu, add the HNO that percent by volume is 5%
3carry out dilution constant volume, obtain testing sample;
(3) test: adopt ICP-OES to test, analytical element parameter: Cd – 228.8nm, Te – 214.2 nm, Sc – 361.3nm;
(4) go out the content of Te and Cd in cadmium telluride sample according to test result according to following formulae discovery, then calculate the atomic ratio of tellurium, cadmium element;
（1）
（2）
(3)
In formula:
I
te, I
cd, I
scthe intensity of-apparatus measures Te, Cd and Sc out;
Mg
te, mg
cdthe weight (unit: mg) of Te and Cd in-standard reference solution;
G
cdTe---CdTe example weight (unit: g);
G
sc---target weight (unit: g) in Sc;
D---Te/Cd atomic ratio;
Sample---CdTe sample;
Standard---standard reference solution.
2. a kind of method measuring tellurium in cadmium telluride, cadmium element atomic ratio according to claim 1, it is characterized in that: in step (1), when sampling, each sample repeats preparation four parts.
3. a kind of method measuring tellurium in cadmium telluride, cadmium element atomic ratio according to claim 1, is characterized in that: in step (2), and the dissolution time of sample dissolution is 5 minutes to 1 hour.
4. a kind of method measuring tellurium in cadmium telluride, cadmium element atomic ratio according to claim 1, is characterized in that: in step (2), during sample dissolution, the reacting gas supervened will be overflowed.
5. a kind of method measuring tellurium in cadmium telluride, cadmium element atomic ratio according to claim 1, it is characterized in that: in step (3), the nitric acid blank solution of 5% is adopted to add the method production standard curve of reference material, to check the element to be measured in the nitric acid blank solution of 5%, the constituent content to be measured in the nitric acid blank solution of control 5% is lower than 0.05 μ g/L.
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| CN109019531B (en) * | 2018-08-07 | 2021-12-17 | 中船重工黄冈贵金属有限公司 | Method for preparing high-purity tellurium dioxide by taking crude tellurium as raw material |
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| CN101551357A (en) * | 2009-02-26 | 2009-10-07 | 中国兵器工业集团第五三研究所 | ICP-MS measuring method of trace metal impurities in high purity lead |
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| CN101551357A (en) * | 2009-02-26 | 2009-10-07 | 中国兵器工业集团第五三研究所 | ICP-MS measuring method of trace metal impurities in high purity lead |
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| 中华人民共和国工业和信息化部.高纯二氧化碲.《中华人民共和国有色金属行业标准》.2012,4-8. * |
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