CN102608147A - Method for judging purity of silicon for crystalline silicon solar battery - Google Patents
Method for judging purity of silicon for crystalline silicon solar battery Download PDFInfo
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- CN102608147A CN102608147A CN201210041848XA CN201210041848A CN102608147A CN 102608147 A CN102608147 A CN 102608147A CN 201210041848X A CN201210041848X A CN 201210041848XA CN 201210041848 A CN201210041848 A CN 201210041848A CN 102608147 A CN102608147 A CN 102608147A
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Abstract
The invention relates to a method for judging purity of silicon for a crystalline silicon solar battery, which comprises the steps of: a, weighing silicon samples with given weight, b, adopting gas shield at a certain flow (80-120mL/min) and allowing the silicon samples to be fused at a certain heating rate (3-100 DEG C/min) and in a certain temperature range (0-1500 DEG C) in a simultaneous differential scanning calorimeter-thermo gravimetric analyzer (SDT), c, regressing a linear relationship between purities and melting points according to at least three samples with known purities and correct melting point testing results of the samples based on testing conditions set in Steps a and b, and d, calculating the purity of unknown samples according to the linear relationship between the purities and the melting points for other samples with unknown purities as long as the melting points of the samples with unknown purities are measured. The method has the beneficial effects that: 1, the operation is automatic, the total cost is lower, and the quality control is facilitated, 2, the method is a physical method for directly measuring the changes in the melting points, and is scientific and reasonable, and 3, the measuring precision is high, and the stability is higher.
Description
Technical field
The present invention relates to a kind of method of passing judgment on crystal silicon solar energy battery with silicon material purity.
Background technology
Silicon is one of the widest element of distributed in nature, is a kind of good semiconductor material, is the requisite starting material of integrated circuit, electronic component of national encourage growth.The purity that improves the silicon material has become one of current important problem both at home and abroad.And be used to make material such as solar cell, require the purity of silicon high, greater than more than 99.99%.
Along with the development day by day of photovoltaic industry, silicon raw material supplied materials control is required increasingly high, for fast, accurately, reasonably knowing silicon material supplied materials situation, need new method of testing.Present most of method of testing is the concentration of each impurity in the quantitative measurement silicon raw material, such as glow discharge mass spectrometry (GDMS), SIMS (SIMS), infra-red sepectrometry (FTIR), inductivity coupled plasma mass spectrometry (ICP-MS) or the like.Because the above means of testing and the limitation of equipment cause test result more single, therefore choose a kind of quick, easy, to measure the method for silicon purity accurately most important, improves the crystal pulling quality, reach synergy and fall this purpose.
Summary of the invention
Technical matters to be solved by this invention is: a kind of method of passing judgment on crystal silicon solar energy battery with silicon material purity is provided, can measures silicon purity quick, easy, accurately.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method of passing judgment on crystal silicon solar energy battery with silicon material purity, and its step comprises:
A. take by weighing the silicon material sample of constant weight, the weight of silicon material sample is between 1-7mg;
B. in differential thermal-thermogravimetric simultaneous thermal analysis appearance, with the gas shield of certain flow, flow is at 80-120mL/min; In certain heating rate and temperature range; Silicon material sample generation fusion, heating rate is at 3-100 ℃/min, and temperature range is in 0-1500 ℃;
C. on the test condition basis of step a and b setting,, return out the linear relationship of purity and fusing point according to sample and its correct fusing point test result of at least three kinds of known purity;
As long as d. the sample of other unknown purity is measured the fusing point of this sample,, just can calculate the purity of unknown sample according to the linear relationship of purity and fusing point.
Further, obtain relation equation, be expressed as according to the linear relationship of purity that returns out among the step c and fusing point:
y＝ax+b，
In the formula: y is the purity of sample, and x is sample fusing point ratio (T0-Ts)/T0^2, T0: be the fusing point (1420 ℃) of pure sample article, Ts is the fusing point of sample, and a, b are the constant parameter relevant with sample;
With the fusing point substitution relation equation y=ax+b of the sample that records unknown purity in the steps d, obtain the purity of sample.
Further, wherein a, b value are respectively-0.0443 and 1.
The invention has the beneficial effects as follows: 1. automation mechanized operation, overall cost is lower, is beneficial to quality control; 2. belong to the physics method, directly measure the variation of fusing point, methodological science is reasonable; 3. measuring accuracy is high, and stability is better, and data are more accurate, and systematic error is little.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Fig. 1 is the melting curve map of sample fusing of the present invention;
Fig. 2 is the melting curve of the sample of three kinds of known purity of the present invention;
Fig. 3 is fusing point and the linear relationship of purity of the sample of three kinds of known purity of the present invention;
Fig. 4 is the melting curve of the sample of unknown purity of the present invention;
Embodiment
When material purity reduced, its fusing point also can reduce, even and its melting region can broaden. the impurity of minute quantity also can greatly change the width of melting region.Purity is high more, and fusing point is high more. and melting peak is sharper steep.Utilization of the present invention causes this principle of fusing point decline to measure material purity because of material section is impure.
A kind of method of passing judgment on crystal silicon solar energy battery with silicon material purity, its step comprises:
A. take by weighing the silicon material sample of constant weight, the weight of silicon material sample is between 1-7mg;
B. in differential thermal-thermogravimetric simultaneous thermal analysis appearance (SDT), with the gas shield of certain flow, flow is at 80-120mL/min; In certain heating rate and temperature range; Silicon material sample generation fusion, heating rate is at 3-100 ℃/min, and temperature range is in 0-1500 ℃;
C. on the test condition basis of step a and b setting, as sample test result accurately, draw its fusing point with sharp-pointed melting peak.As shown in Figure 1, curve 1 is the correct test result of this sample.According to the sample and its correct fusing point test result of at least three kinds of known purity, return out the linear relationship of purity and fusing point, as shown in Figure 3, can obtain relation equation by this linear relationship, be expressed as:
y＝ax+b，
In the formula: y is the purity of sample, and x is sample fusing point ratio (T0-Ts)/T0^2, T0: be the fusing point (1420 ℃) of pure sample article, Ts is the fusing point of sample, and a, b are the constant parameter relevant with sample;
As long as d. the sample of other unknown purity is measured the fusing point of this sample, substitution relation equation y=ax+b can obtain the purity of sample.
For example: the value of known 1#, 2#, three kinds of silicon material of 3# sample purity is: 0.99999995107000,0.99999990373000,0.99999992620000.Take by weighing the silicon material sample of constant weight, in certain gas shield and heating rate, the result is as shown in Figure 2, and the melting point values of three kinds of samples is respectively: 1418.25 ℃, 1416.12 ℃, 1416.95 ℃.Relation equation between fusing point and the sample purity is expressed as:
Y=ax+b, its a, b value are respectively-0.0443,1
In the formula: y is the purity of sample, and x is sample fusing point ratio (T0-Ts)/T0^2, T0: be the fusing point (1420 ℃) of pure sample article, Ts is the fusing point of sample, and a, b are the parameters relevant with sample.
The assumed condition of this equation: 1, impurity is not fused to melt substance; 2, purity is higher than more than 98%
The silicon material sample melted process of unknown purity is as shown in Figure 4, finds out that by the fusion peak value fusing point of this sample is 1416.14 ℃, and according to formula y=-0.0443x+1, the purity that draws this sample is 0.999999915196.
Claims (3)
1. method of passing judgment on crystal silicon solar energy battery with silicon material purity, it is characterized in that: its step comprises:
A. take by weighing the silicon material sample of constant weight, the weight of silicon material sample is between 1-7mg;
B. in differential thermal-thermogravimetric simultaneous thermal analysis appearance, with the gas shield of certain flow, flow is at 80-120mL/min; In certain heating rate and temperature range; Silicon material sample generation fusion, heating rate is at 3-100 ℃/min, and temperature range is in 0-1500 ℃;
C. on the test condition basis of step a and b setting,, return out the linear relationship of purity and fusing point according to sample and its correct fusing point test result of at least three kinds of known purity;
As long as d. the sample of other unknown purity is measured the fusing point of this sample,, just can calculate the purity of unknown sample according to the linear relationship of purity and fusing point.
2. judge crystal silicon solar energy battery according to claim 1 is characterized in that with the method for silicon material purity: the linear relationship according to purity that returns out among the step c and fusing point obtains relation equation, is expressed as:
y＝ax+b，
In the formula: y is the purity of sample, and x is sample fusing point ratio (T0-Ts)/T0^2, T0: be the fusing point (1420 ℃) of pure sample article, Ts is the fusing point of sample, and a, b are the constant parameter relevant with sample;
With the fusing point substitution relation equation y=ax+b of the sample that records unknown purity in the steps d, obtain the purity of sample.
3. judge crystal silicon solar energy battery according to claim 2 is characterized in that with the method for silicon material purity: wherein a, b value are respectively-0.0443 and 1.
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| CN201210041848XA CN102608147A (en) | 2012-02-23 | 2012-02-23 | Method for judging purity of silicon for crystalline silicon solar battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103399034A (en) * | 2013-08-09 | 2013-11-20 | 北京市农林科学院 | Method for detecting purity of stearic acid |
| CN105424743A (en) * | 2015-12-02 | 2016-03-23 | 常州大学 | Method for rapidly determining purity of raw materials in process of producing polyglycolic acid |
-
2012
- 2012-02-23 CN CN201210041848XA patent/CN102608147A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103399034A (en) * | 2013-08-09 | 2013-11-20 | 北京市农林科学院 | Method for detecting purity of stearic acid |
| CN103399034B (en) * | 2013-08-09 | 2016-03-16 | 北京市农林科学院 | Detect the method for purity of stearic acid |
| CN105424743A (en) * | 2015-12-02 | 2016-03-23 | 常州大学 | Method for rapidly determining purity of raw materials in process of producing polyglycolic acid |
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Application publication date: 20120725 |