CN115718093B - High-purity quartz SiO matched with pretreatment device2Purity and impurity content detection method - Google Patents
High-purity quartz SiO matched with pretreatment device2Purity and impurity content detection method Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000010453 quartz Substances 0.000 title claims abstract description 77
- 239000012535 impurity Substances 0.000 title claims abstract description 47
- 238000001514 detection method Methods 0.000 title claims abstract description 26
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 56
- 238000012360 testing method Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 64
- 239000000523 sample Substances 0.000 claims description 64
- 230000029087 digestion Effects 0.000 claims description 32
- 229910052697 platinum Inorganic materials 0.000 claims description 32
- -1 polytetrafluoroethylene Polymers 0.000 claims description 30
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 30
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 30
- 238000002474 experimental method Methods 0.000 claims description 27
- 239000002253 acid Substances 0.000 claims description 23
- 238000005303 weighing Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 14
- 239000012488 sample solution Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 9
- 229910052700 potassium Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 8
- 238000000120 microwave digestion Methods 0.000 claims description 6
- 238000009616 inductively coupled plasma Methods 0.000 claims description 5
- 238000004020 luminiscence type Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 4
- 229910052909 inorganic silicate Inorganic materials 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 229910004014 SiF4 Inorganic materials 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 239000012490 blank solution Substances 0.000 claims description 2
- 238000005485 electric heating Methods 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 description 49
- 230000000694 effects Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000012422 test repetition Methods 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 210000003000 inclusion body Anatomy 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for detecting the purity and impurity content of high-purity quartz SiO 2 matched with a pretreatment device. The method comprises two sets of detection processes, wherein the first set of detection process is used for detecting the SiO 2 content of the high-purity quartz; the second set of detection flow is used for detecting the impurity content of the high-purity quartz. The detachable SiF 4 trapping device in the matched pretreatment device can thoroughly react through precipitation reaction and color reaction so as to ensure that SiO 2 completely reacts, ensure that a high-purity quartz sample is completely dissolved, and be beneficial to improving the test accuracy of a detection method; the test accuracy of the detection method is high.
Description
Technical Field
The invention relates to the field of analysis and detection, in particular to a method for detecting the purity and impurity content of high-purity quartz SiO2 by a matched pretreatment device.
Background
Currently, quartz raw materials with high content of SiO 2 purity are collectively called high-purity quartz, the high-purity quartz is defined as quartz series products with SiO 2 purity more than 99%, the product grades can be divided according to the purity of SiO 2, namely, the low end is more than or equal to 99.9% (3N) of w (SiO 2), and the middle end is: w (SiO 2) is more than or equal to 99.99 percent (4N), high end: the w (SiO 2) is more than or equal to 99.998 percent (4N 8), and the total amount of impurity elements such as Al, B, li, K, na, ca, mg, ti, fe, mn, cu, cr, ni in the product can be divided, namely, the low end w is less than or equal to 1000 multiplied by 10 -6, the middle end w is less than or equal to 100 multiplied by 10 -6, the high end w is less than or equal to 20 multiplied by 10 -6, and the high-purity quartz of each grade can be divided into varieties such as 40-80 meshes, 80-140 meshes, 80-200 meshes, 80-300 meshes and the like according to the granularity. Heavy metal impurity elements exist in crystal lattices of quartz minerals in the form of impurity minerals and similar substances, and besides, non-heavy metal impurities exist in the form of gas-liquid inclusion bodies (mainly comprising C, H elements), and the impurities need rock phase analysis means for identification, such as a Scanning Electron Microscope (SEM), an X-ray diffractometer (XRD), a differential thermal analyzer, a thermogravimetric analyzer, an infrared spectrometer and the like. The international market of high-end products of 4N8 and above is almost monopolized by the U.S. Unimin company, but the industries of photovoltaic, electronic information, high-end electric light sources and the like in China have great demands on high-purity quartz. For such high purity materials, detection and identification techniques are particularly critical.
In the common quartz industry, common detection technologies include an animal gel weight method, a polyethylene oxide condensation weight method, a perchloric acid dehydration weight method, a silicon tetrafluoride direct volatilization weight method, a potassium silicofluoride titration method, a molybdenum silicon blue photometry method, a potassium fluosilicate capacity method and the like, but the detection methods can accurately measure the content of SiO 2 within the range of only 20-98%, and are obviously not suitable for detecting high-purity quartz samples. In addition, there is no unified detection standard in the high-purity quartz detection industry, and the technical standards of different industries are different.
On one hand, the detection methods have low detection efficiency, the detection rate mainly depends on the number of containers for containing samples, the content of high-purity quartz impurities cannot be quantified, on the other hand, the weight or absorbance change in the detection process is related to the content of SiO 2, but whether SiO 2 participates in chemical reaction thoroughly but cannot be accurately judged, which leads to deviation of the accuracy of a test result
Disclosure of Invention
The invention aims to provide a method for detecting the purity and impurity content of high-purity quartz SiO 2 so as to solve the problems of low detection efficiency and low test accuracy in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
The invention provides a method for detecting the purity and impurity content of high-purity quartz SiO 2 matched with a pretreatment device, which is characterized by comprising the following steps: s1, detecting the purity of high-purity quartz SiO 2; s2, detecting the impurity content of the high-purity quartz; the high-purity quartz SiO 2 purity detection comprises the following substeps:
S11, weighing a high-purity quartz sample in a thousands-grade clean laboratory, wherein the mass is marked as m, and weighing a platinum crucible filled with the high-purity quartz sample, wherein the mass is marked as m 1; weighing a platinum crucible for a non-burnt blank experiment, wherein the mass of the platinum crucible is recorded as m 3, and the blank experiment is that other analysis steps are the same as the high-purity quartz SiO 2 purity detection step except for an un-heightened quartz sample; placing a platinum crucible filled with a high-purity quartz sample and a platinum crucible for blank experiments in a muffle furnace for burning, taking out the crucible, and placing the crucible in a dryer for cooling to room temperature;
s12, transferring a high-purity quartz sample to each polytetrafluoroethylene digestion tank, adding HF acid, then placing the high-purity quartz sample in a microwave digestion instrument to digest at a certain temperature and remove the acid until the high-purity quartz sample is nearly dry, and installing a detachable SiF 4 trapping device above a self-made polytetrafluoroethylene container;
S13, confirming that SiO 2 is completely converted into SiF 4 according to a color reaction, transferring residual liquid in a tank into a platinum crucible, washing the inner wall of a polytetrafluoroethylene digestion tank with a small amount of water, sequentially adding a plurality of drops of water and a plurality of HF acids when the liquid in the platinum crucible is nearly dry, evaporating to nearly dry on an electric plate, adding 10ml of distilled water again, evaporating to dry, and simultaneously performing a blank experiment;
S14, wiping the outer wall of the crucible by wet filter paper after cooling, burning the platinum crucible in a muffle furnace, weighing the crucible when cooling to room temperature, marking the mass as m 2, and marking the mass of the platinum crucible for a blank experiment after burning as m 4;
S15, calculating the purity of SiO 2 according to a formula.
Further, the temperature of the muffle furnace in the step S11 is 960+/-5 ℃ and the burning time is 3 hours, the temperature of the electric heating plate in the step S13 is 200+/-5 ℃, and the temperature of the muffle furnace in the step S14 is 960+/-5 ℃ and the burning time is 1 hour.
Further, the calculation formula in step S15 is as follows:
Wherein w (SiO 2) is the mass fraction of SiO 2 in the high-purity quartz, m 1 is the mass of a platinum crucible and a high-purity quartz sample, m 2 is the mass of the platinum crucible and residues after digestion by HF acid and firing, m 3 is the mass of the platinum crucible for a blank experiment without firing, m 4 is the mass of the platinum crucible for a blank experiment after firing, and m is the mass of the high-purity quartz sample.
Further, the high purity quartz impurity content detection comprises the following substeps:
S21, weighing a sample in a thousand-level clean laboratory, marking the mass as m 5, placing the sample in a self-made polytetrafluoroethylene container, adding HF acid into the polytetrafluoroethylene container, placing the polytetrafluoroethylene container in a microwave digestion instrument, and decomposing the sample at a certain temperature, wherein the blank experiment is that other analysis steps are the same as the step of detecting the impurity content of the high-purity quartz except that the high-purity quartz sample is not added;
S22, after digestion is finished, taking out the container, placing the container in an acid-removing instrument, installing a detachable SiF 4 trapping device above a self-made polytetrafluoroethylene container, confirming that SiO 2 is completely converted into SiF 4 according to a color reaction, then slowly heating and evaporating to dryness at 100 ℃ to remove HF acid, and taking down the SiF4 trapping device after cooling;
S23, adding a plurality of 5% diluted HNO 3 in volume into a self-made polytetrafluoroethylene container by using a liquid transfer device, marking the volume of a sample solution as v, shaking uniformly, detecting the content of elements in the sample solution in the self-made polytetrafluoroethylene container by using an inductively coupled plasma luminescence spectrometer in a hundred-grade clean laboratory, marking the concentration of the detected elements in the sample solution as c 1, performing blank experiment operation according to the flow, marking the concentration of the detected elements in the blank experiment solution as c 2, and marking the elements in the sample solution as Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni, ti;
S24, calculating the mass fraction of the content of the impurity element to be detected according to a formula.
Further, the calculation formula in step S24 is as follows:
w (impurity) is the mass fraction of the content of the element to be measured in the sample, c 1 is the concentration of the element to be measured in the sample solution, c 2 is the concentration of the element to be measured in the blank solution, v is the volume of the sample solution, and m 5 is the mass of the sample.
Further, the working conditions of the inductively coupled plasma luminescence spectrometer are as follows: the power is set to be 1.1kW, the cooling air flow is set to be 12L/min, the auxiliary air flow is set to be 0.2L/min, the atomizer flow is set to be 0.6L/min, the sample injection amount is 1.5ml/min, and the sample lifting time is 15s.
Further, the principle is as follows: siO 2 reacts with HF to generate SiF 4,SiF4, and reacts with sodium carbonate solution to generate H 4SiO4, under an acidic condition, H 4SiO4 reacts with ammonium molybdate to generate yellow silicomolybdic acid complex [ H 4(SiMo12O40 ], the SiO 2 is determined to react thoroughly according to the color shade, and the high-purity quartz sample is ensured to be completely dissolved, so that the phenomenon that the SiO 2 is not converted into SiF 4, impurities in residual SiO 2 crystal lattices cannot be dissolved out, and a test result is deviated is avoided.
Furthermore, a hundred thousand-level electronic balance is needed for weighing the sample, electronic-level hydrofluoric acid is needed for digestion of the sample, and electronic-level nitric acid and ultrapure water are needed.
Further, the electron-level hydrofluoric acid has a mass fraction of 40% and a single metal impurity content of not more than 1ppb, the electron-level nitric acid has a mass fraction of 69% and a single metal impurity content of not more than 10ppb, and the ultrapure water has a resistivity of 18.25mΩ·cm.
Based on the technical scheme, the embodiment of the invention at least has the following technical effects:
(1) The self-made polytetrafluoroethylene digestion tank is matched with the detachable SiF 4 trapping device, and the precipitation reaction and the color reaction can be performed, so that the SiO 2 is determined to completely react, the high-purity quartz sample is ensured to be completely dissolved, and the testing accuracy of the detection method is improved.
(2) The test accuracy of the detection method is high, the accuracy of a test result of impurities such as Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni, ti in high-purity quartz is 0.1ppm, the relative standard deviation is less than or equal to 15 percent (the test repetition number is 10), the accuracy of a test result of the SiO 2 content in high-purity quartz is 99.9 percent, and the relative standard deviation is less than or equal to 5 percent (the test repetition number is 10).
Drawings
FIG. 1 is the effect of the test parameters of example 1 of the present invention on the SiO 2 content test;
FIG. 2 is a graph of experimental design test values for 29 sets of response curves according to example 2 of the present invention;
FIG. 3 is the effect of the test parameters of example 2 of the present invention on the total impurity level test;
FIG. 4 is a schematic diagram of the appearance of a self-made polytetrafluoroethylene digestion tank according to the invention;
FIG. 5 is a schematic cross-sectional view of a self-made polytetrafluoroethylene digestion tank A-A of the invention.
Detailed Description
The invention provides a method for detecting the purity and impurity content of high-purity quartz SiO 2 matched with a pretreatment device, and parameter optimization is carried out before an experiment.
The test result of the chemical analysis method is related to the HF acid dosage, the sample quality, the digestion time and the digestion temperature through the early exploratory experiment, in order to obtain the optimized parameters, the influence of the HF acid dosage, the sample quality, the digestion time and the digestion temperature on the test result is explored by using a response surface method, the influence relationship of the sample quality and the HF dosage, the digestion temperature and the digestion time on the SiO 2 content test is shown in figure 1, the sample quality and the HF dosage obviously influence the SiO 2 content test result, and the SiO 2 content test result is increased and then reduced as the sample quality and the HF dosage are increased. And the digestion temperature and the digestion time have little influence on the test result. The finally selected optimized test parameters are as follows: the sample mass is 2.0g, the HF dosage is 20ml, the digestion temperature is 150 ℃, and the digestion time is 45min.
The instrument analysis method tests the impurity content of the high-purity quartz sample through ICP-OES, the tested impurity elements comprise Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni, ti, similarly, the test value of the total impurity content is taken as a response value, the response surface method is adopted to optimize the test parameters of the SiO 2 instrument analysis method, and 29 groups of experiments are carried out to study the influence of the HF acid dosage, the sample quality, the digestion time and the digestion temperature on the accuracy of the test result. The experimental control parameters are as follows: the dosage of HF acid is 4-20ml, the mass of the sample is 0.2-2.0g, the digestion time is 30-60min, the digestion temperature is 150-220 ℃, and the test value of the response surface is shown in figure 2. As can be seen from fig. 2, when the test parameters are changed, the test results of the total impurity content show a larger fluctuation, which indicates that the selected test parameters have a significant influence on the test results. The finally selected optimized test parameters are as follows: the sample mass is 2.0g, the HF dosage is 20ml, the digestion temperature is 165 ℃, and the digestion time is 45min.
Example 1
S1, weighing 2.0g of high-purity quartz sample in a thousand-level clean laboratory, weighing a platinum crucible filled with the high-purity quartz sample, burning the platinum crucible filled with the high-purity quartz sample and a platinum crucible for blank experiments in a muffle furnace at 960+/-5 ℃ for 3 hours, taking out the crucible, and cooling to room temperature in a dryer;
S2, transferring a high-purity quartz sample to each polytetrafluoroethylene digestion tank, adding 20ml of HF acid, then placing the quartz sample in a microwave digestion instrument to digest for 45min at 150 ℃ and remove the acid until the quartz sample is nearly dry, and installing a detachable SiF 4 trapping device above a self-made polytetrafluoroethylene container;
S3, confirming that SiO 2 is completely converted into SiF 4 according to a color reaction, transferring residual liquid in a tank into a platinum crucible, washing the inner wall of the polytetrafluoroethylene digestion tank with a small amount of water, sequentially adding a plurality of drops of water and a plurality of HF acids when the liquid in the platinum crucible is nearly dry, evaporating to nearly dry on an electric plate at 200+/-5 ℃, adding 10ml of distilled water again, evaporating to dry, and simultaneously performing a blank experiment;
s4, wiping the outer wall of the crucible with wet filter paper after cooling, burning the platinum crucible in a muffle furnace at 960+/-5 ℃ for 1h, and weighing when cooling to room temperature;
S5, calculating the purity of SiO 2 according to a formula.
10 Replicates were run and the results are shown in table 1:
TABLE 1SiO 2 content test
| Number of repetitions | Average SiO 2 content (%) | Average SiO 2 content (%) | Relative standard deviation (%) |
| 10 | 99.95 | 3.49 | 3.5 |
As shown in table 1, the detection accuracy of the high-purity quartz can reach 3N (99.9%) stably, and the relative standard deviation of 10 repeatability experiments is only 3.5%, which indicates that the accuracy of the method can meet the test requirement.
Example 2
S1, weighing 2.0g of a sample in a thousand-level clean laboratory, placing the sample in a self-made polytetrafluoroethylene container, adding 20ml of HF acid into the polytetrafluoroethylene container, placing the polytetrafluoroethylene container in a microwave digestion instrument, and decomposing the sample at 165 ℃ for 45 min;
S2, after digestion is finished, taking out the container, placing the container in an acid-removing instrument, installing a detachable SiF 4 trapping device above a self-made polytetrafluoroethylene container, confirming that SiO 2 is completely converted into SiF 4 according to a color reaction, then slowly heating and evaporating to dryness at 100 ℃ to remove HF acid, and taking down the SiF 4 trapping device after cooling;
S3, adding a plurality of 5% diluted HNO 3 in volume percent into a self-made polytetrafluoroethylene container, shaking uniformly, and then performing blank experiment operation according to the flow by using an inductively coupled plasma luminescence spectrometer to self-make the content of elements (including Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni, ti) in sample liquid in the polytetrafluoroethylene container in a hundred-grade clean laboratory;
S4, calculating the mass fraction of the impurity element content according to a formula.
The impurity element (Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni, ti) of the high-purity quartz sample was tested, and the results are shown in table 2:
TABLE 2 impurity element content test
| Relative standard deviation (%) | Concentration (ppm) | |
| Zn | 10.11 | 0.02 |
| Ti | 2.42 | 1.23 |
| Ni | 2.78 | 0.07 |
| Na | 2.66 | 4.89 |
| Mn | 1.43 | 0.07 |
| Mg | 11.05 | 0.59 |
| K | 11.76 | 1.28 |
| Fe | 2.94 | 1.59 |
| Cu | 2.91 | 0.05 |
| Cr | 2.61 | 0.09 |
| Co | 0 | 0 |
| Cd | 0 | 0 |
| Ca | 4.48 | 7.48 |
| Al | 2.28 | 16.44 |
As shown in Table 2, the total impurity amount of the high-purity quartz sample is less than 100ppm, which indicates that the sample belongs to the category of 4N-grade high-purity quartz, the accuracy of the test result of each impurity is 0.1ppm, and the relative standard deviation is less than or equal to 15%, which indicates that the detection method has higher test accuracy.
Claims (6)
1. The method for detecting the purity and impurity content of the high-purity quartz SiO 2 matched with the pretreatment device is characterized by comprising the following steps of: s1, detecting the purity of high-purity quartz SiO 2; s2, detecting the impurity content of the high-purity quartz; the high-purity quartz SiO 2 purity detection comprises the following substeps:
S11, weighing a high-purity quartz sample in a thousands-grade clean laboratory, wherein the mass is marked as m, and weighing a platinum crucible filled with the high-purity quartz sample, wherein the mass is marked as m 1; weighing a platinum crucible for a non-burnt blank experiment, wherein the mass of the platinum crucible is recorded as m 3, and the blank experiment is that other analysis steps are the same as the high-purity quartz SiO 2 purity detection step except for an un-heightened quartz sample; placing a platinum crucible filled with a high-purity quartz sample and a platinum crucible for blank experiments in a muffle furnace for burning, taking out the crucible, and placing the crucible in a dryer for cooling to room temperature;
s12, transferring a high-purity quartz sample to each polytetrafluoroethylene digestion tank, adding HF acid, then placing the high-purity quartz sample in a microwave digestion instrument to digest at a certain temperature and remove the acid until the high-purity quartz sample is nearly dry, and installing a detachable SiF 4 trapping device above a self-made polytetrafluoroethylene container;
S13, confirming that SiO 2 is completely converted into SiF 4 according to a color reaction, transferring residual liquid in a tank into a platinum crucible, washing the inner wall of a polytetrafluoroethylene digestion tank with a small amount of water, sequentially adding a plurality of drops of water and a plurality of HF acids when the liquid in the platinum crucible is nearly dry, evaporating to nearly dry on an electric plate, adding 10ml of distilled water again, evaporating to dry, and simultaneously performing a blank experiment;
S14, wiping the outer wall of the crucible by wet filter paper after cooling, burning the platinum crucible in a muffle furnace, weighing the crucible when cooling to room temperature, marking the mass as m 2, and marking the mass of the platinum crucible for a blank experiment after burning as m 4;
S15, calculating the purity of SiO 2 according to a formula, wherein the calculation formula in the step S15 is as follows:
Wherein w (SiO 2) is the mass fraction of SiO 2 in the high-purity quartz, m 1 is the mass of a platinum crucible and a high-purity quartz sample, m 2 is the mass of the platinum crucible and residues after digestion by HF acid and firing, m 3 is the mass of the platinum crucible for blank experiments without firing, m 4 is the mass of the platinum crucible for blank experiments after firing, and m is the mass of the high-purity quartz sample;
the method for detecting the impurity content of the high-purity quartz comprises the following substeps:
S21, weighing a sample in a thousand-level clean laboratory, marking the mass as m 5, placing the sample in a self-made polytetrafluoroethylene container, adding HF acid into the polytetrafluoroethylene container, placing the polytetrafluoroethylene container in a microwave digestion instrument, and decomposing the sample at a certain temperature, wherein the blank experiment is that other analysis steps are the same as the step of detecting the impurity content of the high-purity quartz except that the high-purity quartz sample is not added;
S22, after digestion is finished, taking out the container, placing the container in an acid-removing instrument, installing a detachable SiF 4 trapping device above a self-made polytetrafluoroethylene container, confirming that SiO 2 is completely converted into SiF 4 according to a color reaction, then slowly heating and evaporating to dryness at 100 ℃ to remove HF acid, and taking down the SiF 4 trapping device after cooling;
S23, adding a plurality of 5% diluted HNO 3 in volume into a self-made polytetrafluoroethylene container by using a liquid transfer device, marking the volume of a sample solution as v, shaking uniformly, detecting the content of elements in the sample solution in the self-made polytetrafluoroethylene container by using an inductively coupled plasma luminescence spectrometer in a hundred-grade clean laboratory, marking the concentration of the detected elements in the sample solution as c 1, performing blank experiment operation according to the flow, marking the concentration of the detected elements in the blank experiment solution as c 2, and marking the elements in the sample solution as Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni, ti;
S24, calculating mass fractions of the content of the impurity elements to be detected according to a formula, wherein the calculation formula in the step S24 is as follows:
w (impurity) is the mass fraction of the content of the element to be measured in the sample, c 1 is the concentration of the element to be measured in the sample solution, c 2 is the concentration of the element to be measured in the blank solution, v is the volume of the sample solution, and m 5 is the mass of the sample.
2. The method for detecting the purity and the impurity content of the high-purity quartz SiO 2 matched with the pretreatment device according to claim 1, wherein the muffle furnace temperature in the step S11 is 960+/-5 ℃ and the firing time is 3h, the electric heating plate temperature in the step S13 is 200+/-5 ℃, and the muffle furnace temperature in the step S14 is 960+/-5 ℃ and the firing time is 1h.
3. The method for detecting the purity and the impurity content of the high-purity quartz SiO 2 matched with the pretreatment device according to claim 1, wherein the working conditions of the inductively coupled plasma luminescence spectrometer are as follows: the power is set to be 1.1kW, the cooling air flow is set to be 12L/min, the auxiliary air flow is set to be 0.2L/min, the atomizer flow is set to be 0.6L/min, the sample injection amount is 1.5ml/min, and the sample lifting time is 15s.
4. A method for detecting the purity and impurity content of high-purity quartz SiO 2 matched with a pretreatment device according to any one of claims 1 to 3, characterized by comprising the following steps: siO 2 reacts with HF to generate SiF 4,SiF4, and reacts with sodium carbonate solution to generate H 4SiO4, under an acidic condition, H 4SiO4 reacts with ammonium molybdate to generate yellow silicomolybdic acid complex [ H 4(SiMo12O40 ], the SiO 2 is determined to react thoroughly according to the color shade, and the high-purity quartz sample is ensured to be completely dissolved, so that the phenomenon that the SiO 2 is not converted into SiF 4, impurities in residual SiO 2 crystal lattices cannot be dissolved out, and a test result is deviated is avoided.
5. The method for detecting the purity and the impurity content of the high-purity quartz SiO 2 matched with the pretreatment device according to claim 1, wherein a hundred thousand-level electronic balance is used for weighing the sample, and electronic-level hydrofluoric acid and electronic-level nitric acid and ultrapure water are used for digestion of the sample.
6. The method for detecting the purity and the impurity content of the high-purity quartz SiO 2 matched with the pretreatment device according to claim 5, wherein the electronic grade hydrofluoric acid is 40% by mass, the content of single metal impurities is less than or equal to 1ppb, the electronic grade nitric acid is 69% by mass, the content of single metal impurities is less than or equal to 10ppb, and the resistivity of the ultrapure water is 18.25MΩ & cm.
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| US5877027A (en) * | 1996-03-18 | 1999-03-02 | Shin-Etsu Quartz Products Co., Ltd. | Method for the analysis of impurity contents in silicon dioxide |
| CN109490059A (en) * | 2018-09-19 | 2019-03-19 | 中钢集团新型材料（浙江）有限公司 | It is a kind of to measure high purity graphite boron content pre-treating method using ICP |
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| CN102607984A (en) * | 2012-02-29 | 2012-07-25 | 成都中光电科技有限公司 | Test method for compositions of fine silica powder |
| JP6459903B2 (en) * | 2015-10-30 | 2019-01-30 | 信越半導体株式会社 | Impurity analysis method and silicon single crystal manufacturing method |
| CN113275121A (en) * | 2021-06-11 | 2021-08-20 | 四川敏田科技发展有限公司 | High-purity quartz sand manufacturing system and manufacturing method |
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| US5877027A (en) * | 1996-03-18 | 1999-03-02 | Shin-Etsu Quartz Products Co., Ltd. | Method for the analysis of impurity contents in silicon dioxide |
| CN109490059A (en) * | 2018-09-19 | 2019-03-19 | 中钢集团新型材料（浙江）有限公司 | It is a kind of to measure high purity graphite boron content pre-treating method using ICP |
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