CN107643281A - Industrial silicon dirt content test method - Google Patents
Industrial silicon dirt content test method Download PDFInfo
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- CN107643281A CN107643281A CN201710910602.4A CN201710910602A CN107643281A CN 107643281 A CN107643281 A CN 107643281A CN 201710910602 A CN201710910602 A CN 201710910602A CN 107643281 A CN107643281 A CN 107643281A
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Abstract
The invention discloses a kind of industrial silicon dirt content test method, including：Step 1: industrial silicon sample is ground into 30~70 μm of industrial silicon powder using vibrating mill；Step 2: weighing 1g industrial silicon powders, 3~5mL hydrofluoric acid is added；Continue to add 8~10mL hydrofluoric acid into polytetrafluoroethylene beaker afterwards, while nitrogen is passed through into hydrofluoric acid, the flow of nitrogen is 0.02~0.04mL/min, is continually fed into 5~7min of nitrogen；Step 3: polytetrafluoroethylene beaker is placed in heating plate, heated, backward polytetrafluoroethylene beaker add 2~3mL nitric acid and 4~5mL hydrochloric acid, after vigorous reaction stopping, adding 1~1.2mL perchloric acid, heating continues 18~20min altogether；Step 4: solution to be measured is detected using inductively coupled plasma emission spectrography.Detection limit of the present invention is low, and accuracy of detection is high, and detection error is small.
Description
Technical field
The present invention relates to chemical detection method, more particularly to a kind of industrial silicon dirt content test method.
Background technology
Industrial silicon has a wide range of applications in steel, coloured, electronics, chemical industry, medicine and other fields, annual a large amount of outlets.Work
Silica quality fraction is generally more than 98% in industry silicon, and impurity content directly affects product quality, therefore, accurate
True analysing impurity constituent content is to determine that the grade of industrial silicon is extremely important.But at present in the detection method of industrial silicon still
Existing defects, it is unsatisfactory in terms of detection limit, accuracy of detection and detection error.
The content of the invention
For above-mentioned technical problem, the present invention has designed and developed that a kind of detection limit is lower, accuracy of detection is higher, detection error
Smaller industrial silicon dirt content test method.
Technical scheme provided by the invention is：
A kind of industrial silicon dirt content test method, including：
Step 1: industrial silicon sample is ground into 30~70 μm of industrial silicon powder using vibrating mill；
Step 2: weighing industrial silicon powder described in 1g, it is placed in polytetrafluoroethylene beaker, adds 3~5mL hydrofluoric acid, will
Industrial silicon powder on polytetrafluoroethylene beaker wall is flushed to polytetrafluoroethylene beaker bottom, gently shakes polytetrafluoroethylene (PTFE) burning
Cup, shake 3~5min；Continue to add 8~10mL hydrofluoric acid into the polytetrafluoroethylene beaker afterwards, while into hydrofluoric acid
Nitrogen is passed through, the flow of the nitrogen is 0.02~0.04mL/min, is continually fed into 5~7min of nitrogen；
Step 3: the polytetrafluoroethylene beaker is placed in heating plate, being heated, heating-up temperature is 88~90 DEG C,
Backward polytetrafluoroethylene beaker add 2~3mL nitric acid and 4~5mL hydrochloric acid, after vigorous reaction stopping, adding 1~1.2mL
Perchloric acid, heating continue 18~20min altogether, the solution in the polytetrafluoroethylene beaker is completely dissolved to limpid, are cooled to
Room temperature；It will be configured to solution and move to 100mL volumetric flasks, constant volume is diluted with water, solution to be measured is made；
Step 4: detected using inductively coupled plasma emission spectrography to the solution to be measured, and from described
The content of following element to be measured is analyzed in testing result, the element to be measured includes aluminium, iron, calcium, magnesium, potassium, sodium, phosphorus, barium.
Preferably, vibrating mill is used in described industrial silicon dirt content test method, in the step 1 by work
Industry silicon sample is ground into 30~50 μm of industrial silicon powder.
Preferably, in described industrial silicon dirt content test method, in the step 2, industrial silicon described in 1g is weighed
Powder, it is placed in polytetrafluoroethylene beaker, adds 3mL hydrofluoric acid, the industrial silicon powder on polytetrafluoroethylene beaker wall is rinsed
To polytetrafluoroethylene beaker bottom, polytetrafluoroethylene beaker is gently shaken, shakes 3min.
Preferably, in described industrial silicon dirt content test method, in the step 2, continue to the polytetrafluoro
10mL hydrofluoric acid is added in ethene beaker, while nitrogen is passed through into hydrofluoric acid, the flow of the nitrogen is 0.04mL/min, is held
It is continuous to be passed through nitrogen 5min.
Preferably, in described industrial silicon dirt content test method, in the step 3, by the polytetrafluoroethylene (PTFE)
Beaker is placed in heating plate, is heated, and heating-up temperature is 90 DEG C, backward polytetrafluoroethylene beaker addition 3mL nitric acid and 5mL
Hydrochloric acid, after vigorous reaction stopping, 1.2mL perchloric acid is added, heating continues 20min, made in the polytetrafluoroethylene beaker altogether
Solution be completely dissolved to limpid, be cooled to room temperature.
Preferably, in described industrial silicon dirt content test method, in the step 4, the element to be measured is prepared
The singly mark solution of middle each element, and the mixed mark solution of element to be measured, using inductively coupled plasma emission spectrography to each
The singly mark solution of element and the mixed mark solution are analyzed, and by the analysis of spectra pair of the testing result and each element
Than analyzing the content of each element in the testing result.
The industrial silicon dirt content test method careful design of the present invention pre-treatment link of industrial silicon, is first added
A small amount of hydrofluoric acid is dissolved, and adds a large amount of hydrofluoric acid afterwards, and is passed through nitrogen to hydrofluoric acid, so as to promote silica to fill
Divide dissolving, and make to wave silicon progress thoroughly, be further continued for adding nitric acid, hydrochloric acid and perchloric acid afterwards, and heated, make member to be measured
Element dissolving, is finally detected using inductively coupled plasma emission spectrography.Detection limit of the present invention is low, and accuracy of detection is high,
Detection error is small.
Embodiment
The present invention is described in further detail below, to make those skilled in the art being capable of evidence with reference to specification word
To implement.
The present invention provides a kind of industrial silicon dirt content test method, including：
Step 1: industrial silicon sample is ground into 30~70 μm of industrial silicon powder using vibrating mill；
Step 2: weighing industrial silicon powder described in 1g, it is placed in polytetrafluoroethylene beaker, adds 3~5mL hydrofluoric acid, will
Industrial silicon powder on polytetrafluoroethylene beaker wall is flushed to polytetrafluoroethylene beaker bottom, gently shakes polytetrafluoroethylene (PTFE) burning
Cup, shake 3~5min；Continue to add 8~10mL hydrofluoric acid into the polytetrafluoroethylene beaker afterwards, while into hydrofluoric acid
Nitrogen is passed through, the flow of the nitrogen is 0.02~0.04mL/min, is continually fed into 5~7min of nitrogen；
Step 3: the polytetrafluoroethylene beaker is placed in heating plate, being heated, heating-up temperature is 88~90 DEG C,
Backward polytetrafluoroethylene beaker add 2~3mL nitric acid and 4~5mL hydrochloric acid, after vigorous reaction stopping, adding 1~1.2mL
Perchloric acid, heating continue 18~20min altogether, the solution in the polytetrafluoroethylene beaker is completely dissolved to limpid, are cooled to
Room temperature；It will be configured to solution and move to 100mL volumetric flasks, constant volume is diluted with water, solution to be measured is made；
Step 4: detected using inductively coupled plasma emission spectrography to the solution to be measured, and from described
The content of following element to be measured is analyzed in testing result, the element to be measured includes aluminium, iron, calcium, magnesium, potassium, sodium, phosphorus, barium.
The described industrial silicon dirt content test method careful design pre-treatment link of industrial silicon is invented, is first added few
Amount hydrofluoric acid is dissolved, and adds a large amount of hydrofluoric acid afterwards, and is passed through nitrogen to hydrofluoric acid, so as to promote silica abundant
Dissolving, and make to wave silicon progress thoroughly, to reduce interference of the element silicon to detection.In step 3, continuously add nitric acid, hydrochloric acid with
And perchloric acid, and heated, element to be measured can be promoted to dissolve.Detection limit of the present invention is low, and accuracy of detection is high, detection error
It is small.
Time and the precise control of flew of nitrogen are passed through, nitrogen overlong time is passed through or flow is excessive, then may cause
Other impurities are carried over；It is passed through that the nitrogen time is too short or flow is too small, then causes silicon to volatilize completely, testing result is produced
Raw interference.
Solution to be measured can be detected using condition of the prior art in step 4 of the present invention.Using full spectrum direct-reading
Plasma spectrometer and two-dimensional array detector.Device parameter is：Power 1150W, carrier gas flux 0.08L/min, aid in gas
Flow 1.0L/min, pump speed 140r/min, nebulizer pressure 205kPa.
Preferably, vibrating mill is used in described industrial silicon dirt content test method, in the step 1 by work
Industry silicon sample is ground into 30~50 μm of industrial silicon powder.
Preferably, in described industrial silicon dirt content test method, in the step 2, industrial silicon described in 1g is weighed
Powder, it is placed in polytetrafluoroethylene beaker, adds 3mL hydrofluoric acid, the industrial silicon powder on polytetrafluoroethylene beaker wall is rinsed
To polytetrafluoroethylene beaker bottom, polytetrafluoroethylene beaker is gently shaken, shakes 3min.
Preferably, in described industrial silicon dirt content test method, in the step 2, continue to the polytetrafluoro
10mL hydrofluoric acid is added in ethene beaker, while nitrogen is passed through into hydrofluoric acid, the flow of the nitrogen is 0.04mL/min, is held
It is continuous to be passed through nitrogen 5min.
Preferably, in described industrial silicon dirt content test method, in the step 3, by the polytetrafluoroethylene (PTFE)
Beaker is placed in heating plate, is heated, and heating-up temperature is 90 DEG C, backward polytetrafluoroethylene beaker addition 3mL nitric acid and 5mL
Hydrochloric acid, after vigorous reaction stopping, 1.2mL perchloric acid is added, heating continues 20min, made in the polytetrafluoroethylene beaker altogether
Solution be completely dissolved to limpid, be cooled to room temperature.
Preferably, in described industrial silicon dirt content test method, in the step 4, the element to be measured is prepared
The singly mark solution of middle each element, and the mixed mark solution of element to be measured, using inductively coupled plasma emission spectrography to each
The singly mark solution of element and the mixed mark solution are analyzed, and by the analysis of spectra pair of the testing result and each element
Than analyzing the content of each element in the testing result.
Embodiment one
Step 1: industrial silicon sample is ground into 30~50 μm of industrial silicon powder using vibrating mill；
Step 2: weighing industrial silicon powder described in 1g, it is placed in polytetrafluoroethylene beaker, 5mL hydrofluoric acid is added, by poly- four
Industrial silicon powder in PVF walls of beaker is flushed to polytetrafluoroethylene beaker bottom, gently shakes polytetrafluoroethylene beaker, shakes
Dynamic 5min；Continue to add 10mL hydrofluoric acid into the polytetrafluoroethylene beaker afterwards, while nitrogen is passed through into hydrofluoric acid, institute
The flow for stating nitrogen is 0.04mL/min, is continually fed into nitrogen 7min；
Step 3: the polytetrafluoroethylene beaker is placed in heating plate, heated, heating-up temperature is 90 DEG C, afterwards
3mL nitric acid and 5mL hydrochloric acid are added to polytetrafluoroethylene beaker, after vigorous reaction stopping, adding 1.2mL perchloric acid, heating is altogether
Continue 20min, the solution in the polytetrafluoroethylene beaker is completely dissolved to limpid, be cooled to room temperature；It will be configured to solution
100mL volumetric flasks are moved to, constant volume is diluted with water, solution to be measured is made；
Step 4: the singly mark solution of each element in the element to be measured is prepared, and the mixed mark solution of element to be measured, use
Inductively coupled plasma emission spectrography is analyzed the singly mark solution of each element and the mixed mark solution, and by described in
The analysis of spectra of testing result and each element contrasts, and analyzes the content of each element in the testing result.
Precision test (n=10) is carried out using the method described in the present embodiment, the relative standard deviation of 8 kinds of elements is shown in Table
1, the precision of method is used as using relative standard deviation.In addition, carrying out mark-on reclaims experiment to industrial silicon sample, each element is returned
Yield is shown in Table 1.
Detection limit, relative standard deviation and the rate of recovery of each element of table 1
The test limit of method described in the present embodiment is low, and relative standard deviation has good precision below 1%.
The rate of recovery is 92%~106%, has the higher degree of accuracy.
Embodiment two
Step 1: industrial silicon sample is ground into 30~50 μm of industrial silicon powder using vibrating mill.
Step 2: weighing industrial silicon powder described in 1g, it is placed in polytetrafluoroethylene beaker, 3mL hydrofluoric acid is added, by poly- four
Industrial silicon powder in PVF walls of beaker is flushed to polytetrafluoroethylene beaker bottom, gently shakes polytetrafluoroethylene beaker, shakes
Dynamic 3min；Continue to add 10mL hydrofluoric acid into the polytetrafluoroethylene beaker, while nitrogen is passed through into hydrofluoric acid, the nitrogen
The flow of gas is 0.04mL/min, is continually fed into nitrogen 5min.
Step 3: the polytetrafluoroethylene beaker is placed in heating plate, heated, heating-up temperature is 90 DEG C, afterwards
3mL nitric acid and 5mL hydrochloric acid are added to polytetrafluoroethylene beaker, after vigorous reaction stopping, adding 1.2mL perchloric acid, heating is altogether
Continue 20min, the solution in the polytetrafluoroethylene beaker is completely dissolved to limpid, be cooled to room temperature；It will be configured to solution
100mL volumetric flasks are moved to, constant volume is diluted with water, solution to be measured is made.
Step 4: the singly mark solution of each element in the element to be measured is prepared, and the mixed mark solution of element to be measured, use
Inductively coupled plasma emission spectrography is analyzed the singly mark solution of each element and the mixed mark solution, and by described in
The analysis of spectra of testing result and each element contrasts, and analyzes the content of each element in the testing result.
Precision test (n=10) is carried out using the method described in the present embodiment, the relative standard deviation of 8 kinds of elements is shown in Table
2, the precision of method is used as using relative standard deviation.In addition, carrying out mark-on reclaims experiment to industrial silicon sample, each element is returned
Yield is shown in Table 2.
Detection limit, relative standard deviation and the rate of recovery of each element of table 2
The test limit of method described in the present embodiment is low, and relative standard deviation has good precision below 1%.
The rate of recovery is 92%~106%, has the higher degree of accuracy.
Embodiment three
Step 1: industrial silicon sample is ground into 40~70 μm of industrial silicon powder using vibrating mill；
Step 2: weighing industrial silicon powder described in 1g, it is placed in polytetrafluoroethylene beaker, 3mL hydrofluoric acid is added, by poly- four
Industrial silicon powder in PVF walls of beaker is flushed to polytetrafluoroethylene beaker bottom, gently shakes polytetrafluoroethylene beaker, shakes
Dynamic 3min；Continue to add 8mL hydrofluoric acid into the polytetrafluoroethylene beaker afterwards, while nitrogen is passed through into hydrofluoric acid, institute
The flow for stating nitrogen is 0.02mL/min, is continually fed into nitrogen 5min；
Step 3: the polytetrafluoroethylene beaker is placed in heating plate, heated, heating-up temperature is 88 DEG C, afterwards
2mL nitric acid and 4mL hydrochloric acid are added to polytetrafluoroethylene beaker, after vigorous reaction stopping, adding 1mL perchloric acid, heating is held altogether
Continuous 18min, the solution in the polytetrafluoroethylene beaker is completely dissolved to limpid, be cooled to room temperature；It will be configured to solution shifting
To 100mL volumetric flasks, constant volume is diluted with water, solution to be measured is made；
Step 4: the singly mark solution of each element in the element to be measured is prepared, and the mixed mark solution of element to be measured, use
Inductively coupled plasma emission spectrography is analyzed the singly mark solution of each element and the mixed mark solution, and by described in
The analysis of spectra of testing result and each element contrasts, and analyzes the content of each element in the testing result.
Precision test (n=10) is carried out using the method described in the present embodiment, the relative standard deviation of 8 kinds of elements is shown in Table
3, the precision of method is used as using relative standard deviation.In addition, carrying out mark-on reclaims experiment to industrial silicon sample, each element is returned
Yield is shown in Table 3.
Detection limit, relative standard deviation and the rate of recovery of each element of table 3
The test limit of method described in the present embodiment is low, and relative standard deviation has good precision below 1%.
The rate of recovery is 91%~106%, has the higher degree of accuracy.
Example IV
Step 1: industrial silicon sample is ground into 30~60 μm of industrial silicon powder using vibrating mill；
Step 2: weighing industrial silicon powder described in 1g, it is placed in polytetrafluoroethylene beaker, 3mL hydrofluoric acid is added, by poly- four
Industrial silicon powder in PVF walls of beaker is flushed to polytetrafluoroethylene beaker bottom, gently shakes polytetrafluoroethylene beaker, shakes
Dynamic 3~5min；Continue to add 9mL hydrofluoric acid into the polytetrafluoroethylene beaker afterwards, while nitrogen be passed through into hydrofluoric acid,
The flow of the nitrogen is 0.02mL/min, is continually fed into nitrogen 6min；
Step 3: the polytetrafluoroethylene beaker is placed in heating plate, heated, heating-up temperature is 88 DEG C, afterwards
2mL nitric acid and 4mL hydrochloric acid are added to polytetrafluoroethylene beaker, after vigorous reaction stopping, adding 1mL perchloric acid, heating is held altogether
Continuous 18min, the solution in the polytetrafluoroethylene beaker is completely dissolved to limpid, be cooled to room temperature；It will be configured to solution shifting
To 100mL volumetric flasks, constant volume is diluted with water, solution to be measured is made；
Step 4: the singly mark solution of each element in the element to be measured is prepared, and the mixed mark solution of element to be measured, use
Inductively coupled plasma emission spectrography is analyzed the singly mark solution of each element and the mixed mark solution, and by described in
The analysis of spectra of testing result and each element contrasts, and analyzes the content of each element in the testing result.
Precision test (n=10) is carried out using the method described in the present embodiment, the relative standard deviation of 8 kinds of elements is shown in Table
4, the precision of method is used as using relative standard deviation.In addition, carrying out mark-on reclaims experiment to industrial silicon sample, each element is returned
Yield is shown in Table 4.
Detection limit, relative standard deviation and the rate of recovery of each element of table 4
The test limit of method described in the present embodiment is low, and relative standard deviation has good precision below 1%.
The rate of recovery is 92%~106%, has the higher degree of accuracy.
Embodiment five
Step 1: industrial silicon sample is ground into 50~70 μm of industrial silicon powder using vibrating mill；
Step 2: weighing industrial silicon powder described in 1g, it is placed in polytetrafluoroethylene beaker, 5mL hydrofluoric acid is added, by poly- four
Industrial silicon powder in PVF walls of beaker is flushed to polytetrafluoroethylene beaker bottom, gently shakes polytetrafluoroethylene beaker, shakes
Dynamic 3min；Continue to add 10mL hydrofluoric acid into the polytetrafluoroethylene beaker afterwards, while nitrogen is passed through into hydrofluoric acid, institute
The flow for stating nitrogen is 0.03mL/min, is continually fed into nitrogen 5min；
Step 3: the polytetrafluoroethylene beaker is placed in heating plate, heated, heating-up temperature is 90 DEG C, afterwards
3mL nitric acid and 5mL hydrochloric acid are added to polytetrafluoroethylene beaker, after vigorous reaction stopping, adding 1.2mL perchloric acid, heating is altogether
Continue 20min, the solution in the polytetrafluoroethylene beaker is completely dissolved to limpid, be cooled to room temperature；It will be configured to solution
100mL volumetric flasks are moved to, constant volume is diluted with water, solution to be measured is made；
Step 4: the singly mark solution of each element in the element to be measured is prepared, and the mixed mark solution of element to be measured, use
Inductively coupled plasma emission spectrography is analyzed the singly mark solution of each element and the mixed mark solution, and by described in
The analysis of spectra of testing result and each element contrasts, and analyzes the content of each element in the testing result.
Precision test (n=10) is carried out using the method described in the present embodiment, the relative standard deviation of 8 kinds of elements is shown in Table
5, the precision of method is used as using relative standard deviation.In addition, carrying out mark-on reclaims experiment to industrial silicon sample, each element is returned
Yield is shown in Table 5.
Detection limit, relative standard deviation and the rate of recovery of each element of table 5
The test limit of method described in the present embodiment is low, and relative standard deviation has good precision below 1%.
The rate of recovery is 91%~106%, has the higher degree of accuracy.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited
In specific details.
Claims (6)
- A kind of 1. industrial silicon dirt content test method, it is characterised in that including：Step 1: industrial silicon sample is ground into 30~70 μm of industrial silicon powder using vibrating mill；Step 2: weighing industrial silicon powder described in 1g, it is placed in polytetrafluoroethylene beaker, 3~5mL hydrofluoric acid is added, by poly- four Industrial silicon powder in PVF walls of beaker is flushed to polytetrafluoroethylene beaker bottom, gently shakes polytetrafluoroethylene beaker, shakes Dynamic 3~5min；Continue to add 8~10mL hydrofluoric acid into the polytetrafluoroethylene beaker afterwards, while be passed through into hydrofluoric acid Nitrogen, the flow of the nitrogen is 0.02~0.04mL/min, is continually fed into 5~7min of nitrogen；Step 3: the polytetrafluoroethylene beaker is placed in heating plate, heated, heating-up temperature is 88~90 DEG C, afterwards 2~3mL nitric acid and 4~5mL hydrochloric acid are added to polytetrafluoroethylene beaker, after vigorous reaction stopping, adding the high chlorine of 1~1.2mL Acid, heating continue 18~20min altogether, the solution in the polytetrafluoroethylene beaker is completely dissolved to limpid, are cooled to room temperature； It will be configured to solution and move to 100mL volumetric flasks, constant volume is diluted with water, solution to be measured is made；Step 4: detected using inductively coupled plasma emission spectrography to the solution to be measured, and from the detection As a result the content of element to be measured below middle analysis, the element to be measured include aluminium, iron, calcium, magnesium, potassium, sodium, phosphorus, barium.
- 2. industrial silicon dirt content test method as claimed in claim 1, it is characterised in that using vibration in the step 1 Industrial silicon sample is ground into 30~50 μm of industrial silicon powder by grinding machine.
- 3. industrial silicon dirt content test method as claimed in claim 1, it is characterised in that in the step 2, weigh 1g The industrial silicon powder, is placed in polytetrafluoroethylene beaker, 3mL hydrofluoric acid is added, by the industry on polytetrafluoroethylene beaker wall Silicon powder is flushed to polytetrafluoroethylene beaker bottom, gently shakes polytetrafluoroethylene beaker, shakes 3min.
- 4. industrial silicon dirt content test method as claimed in claim 1, it is characterised in that in the step 2, continue to 10mL hydrofluoric acid is added in the polytetrafluoroethylene beaker, while nitrogen is passed through into hydrofluoric acid, the flow of the nitrogen is 0.04mL/min, it is continually fed into nitrogen 5min.
- 5. industrial silicon dirt content test method as claimed in claim 1, it is characterised in that in the step 3, by described in Polytetrafluoroethylene beaker is placed in heating plate, is heated, heating-up temperature be 90 DEG C, backward polytetrafluoroethylene beaker addition 3mL nitric acid and 5mL hydrochloric acid, after vigorous reaction stopping, 1.2mL perchloric acid is added, heating continues 20min, makes described poly- four altogether Solution in PVF beaker is completely dissolved to limpid, is cooled to room temperature.
- 6. industrial silicon dirt content test method as claimed in claim 1, it is characterised in that in the step 4, prepare institute The singly mark solution of each element in element to be measured, and the mixed mark solution of element to be measured are stated, is launched using inductively coupled plasma Spectroscopic methodology is analyzed the singly mark solution of each element and the mixed mark solution, and by point of the testing result and each element Spectrogram contrast is analysed, analyzes the content of each element in the testing result.
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| CN109709203A (en) * | 2019-01-31 | 2019-05-03 | 内蒙古通威高纯晶硅有限公司 | The detection method of phosphorus content in a kind of polysilicon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109709203A (en) * | 2019-01-31 | 2019-05-03 | 内蒙古通威高纯晶硅有限公司 | The detection method of phosphorus content in a kind of polysilicon |
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|---|---|
| CN107643281B (en) | 2020-04-07 |
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