CN115718093A - High-purity quartz SiO matched with pretreatment device 2 Purity and impurity content detection method - Google Patents
High-purity quartz SiO matched with pretreatment device 2 Purity 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 81
- 239000010453 quartz Substances 0.000 title claims abstract description 79
- 239000012535 impurity Substances 0.000 title claims abstract description 50
- 238000001514 detection method Methods 0.000 title claims abstract description 33
- 238000012360 testing method Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 29
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000000523 sample Substances 0.000 claims description 68
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 60
- 230000029087 digestion Effects 0.000 claims description 30
- 229910052697 platinum Inorganic materials 0.000 claims description 30
- -1 polytetrafluoroethylene Polymers 0.000 claims description 29
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 29
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 29
- 238000002474 experimental method Methods 0.000 claims description 26
- 239000002253 acid Substances 0.000 claims description 24
- 238000005303 weighing Methods 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 12
- 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
- 239000012488 sample solution Substances 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 6
- 238000000120 microwave digestion Methods 0.000 claims description 6
- 238000005485 electric heating Methods 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 5
- 238000009616 inductively coupled plasma Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910004283 SiO 4 Inorganic materials 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
- 238000004020 luminiscence type Methods 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
- 239000000243 solution Substances 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
- 150000007513 acids Chemical class 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
- 229910003990 H4(SiMo12O40) Inorganic materials 0.000 claims description 2
- 238000000184 acid digestion Methods 0.000 claims description 2
- 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
- 238000012790 confirmation Methods 0.000 claims description 2
- 239000000112 cooling gas Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 229910052748 manganese Inorganic materials 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 238000001556 precipitation Methods 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 48
- 230000000694 effects Effects 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 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
- 239000000047 product Substances 0.000 description 2
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 2
- 238000012422 test repetition Methods 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229910004014 SiF4 Inorganic materials 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
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 230000031877 prophase Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide 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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Abstract
The invention discloses a high-purity quartz SiO matched with a pretreatment device 2 Purity and impurity content detection method. Comprises two sets of detection processes, wherein the first set of detection process is used for detecting high-purity quartz SiO 2 Content (c); the second set of detection process is used for detecting the content of high-purity quartz impurities. The detachable SiF in the matched pretreatment device of the invention 4 The trapping device can determine SiO by precipitation reaction and color reaction 2 The reaction is thoroughly carried out, so that the high-purity quartz sample is completely dissolved, and the test accuracy of the detection method is improved; the detection method has high test accuracy.
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 matched with a pretreatment device.
Background
At present, the high content of SiO 2 The raw material of the high-purity quartz is collectively called high-purity quartz, and the high-purity quartz is defined as SiO 2 The product grade of the quartz series product with the purity of more than 99 percent can be SiO 2 Purity is divided, i.e. low-end: w (SiO) 2 ) Not less than 99.9% (3N), middle-end: w (SiO) 2 )≥99.99％(4N), high-end: w (SiO) 2 ) Not less than 99.998% (4N 8), or divided according to the total amount of impurity elements such as Al, B, li, K, na, ca, mg, ti, fe, mn, cu, cr, ni, etc., i.e. the low end w is not more than 1000 × 10 -6 The middle end w is less than or equal to 100 multiplied by 10 -6 High end w is less than or equal to 20 multiplied by 10 -6 The high-purity quartz of each grade can be divided into varieties of 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 similar to the same images, besides, non-heavy metal impurities exist in the form of gas-liquid inclusions (mainly composed of C, H elements), and the impurities need a lithofacies 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. At present, the international market of high-end products of 4N8 and above is almost monopolized by the Union of America, but the industries of China, such as photovoltaic, electronic information, high-end electric light sources and the like, have great demand on high-purity quartz. For such high purity substances, detection and identification techniques are particularly critical.
In the common quartz industry, common detection technologies comprise an animal glue coagulation gravimetric method, a polyethylene oxide coagulation gravimetric method, a perchloric acid dehydration gravimetric method, a silicon tetrafluoride direct volatilization gravimetric method, a potassium silicofluoride titration method, a silicomolybdenum blue photometry, a potassium fluosilicate volumetric method and the like, but the detection methods can accurately measure SiO 2 The content range is only 20-98%, and the method is obviously not suitable for detecting high-purity quartz samples. In addition, a uniform detection standard does not exist in the high-purity quartz detection industry, and the technical standards of different industries are different.
The detection methods have the advantages that on one hand, the detection efficiency is low, the detection speed mainly depends on the number of containers for holding samples, the content of high-purity quartz impurities cannot be quantified, and on the other hand, the weight or absorbance change and SiO in the detection process are reduced 2 Content related, but SiO 2 Whether the chemical reaction is complete or not can not be accurately judged, which causes deviation of the accuracy of the test result
Disclosure of Invention
The invention aims to provide high-purity quartz SiO 2 Purity and impurity contentThe detection method aims to solve the problems of low detection efficiency and low test accuracy in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides high-purity quartz SiO matched with a pretreatment device 2 The method for detecting the purity and the impurity content is characterized by comprising the following steps of: s1, high-purity quartz SiO 2 Detecting the purity; s2, detecting the content of high-purity quartz impurities; the high-purity quartz SiO 2 The purity detection comprises the following substeps:
s11, weighing a high-purity quartz sample in a thousand-level clean laboratory, wherein the mass is recorded as m, and weighing a platinum crucible filled with the high-purity quartz sample, and the mass is recorded as m 1 (ii) a Weighing the un-burned platinum crucible for blank experiment, and recording the mass as m 3 The blank experiment is that the other analysis steps except the high-purity quartz sample and the high-purity quartz SiO 2 The purity detection steps are the same; placing the platinum crucible filled with the high-purity quartz sample and the platinum crucible of the blank experiment in a muffle furnace for burning, taking out the crucible, placing the crucible in a dryer, and cooling to room temperature;
s12, transferring the high-purity quartz sample to each polytetrafluoroethylene digestion tank, adding HF acid, placing the high-purity quartz sample in a microwave digestion instrument for digestion at a certain temperature and dispelling the acid until the high-purity quartz sample is nearly dry, and then removing the detachable SiF 4 The collecting device is arranged above the self-made polytetrafluoroethylene container;
s13, siO confirmation by color reaction 2 Has been completely converted into SiF 4 Then transferring the residual liquid in the tank to a platinum crucible, washing the inner wall of the polytetrafluoroethylene digestion tank by using 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 on an electric heating plate until the liquid is nearly dry, adding 10ml of distilled water again, evaporating to dryness, and simultaneously performing a blank experiment;
s14, wiping the outer wall of the crucible with wet filter paper after cooling, placing the platinum crucible in a muffle furnace for burning, weighing when cooling to room temperature, and recording the mass as m 2 And the mass of the platinum crucible for the blank experiment after firing is recorded as m 4 ；
S15、Calculating SiO according to the formula 2 And (4) purity.
Further, in the step S11, the muffle furnace temperature is 960 ± 5 ℃, the burning time is 3 hours, in the step S13, the electric heating plate temperature is 200 ± 5 ℃, and in the step S14, the muffle furnace temperature 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 SiO in high-purity quartz 2 Mass fraction, m 1 Mass of platinum crucible and high purity quartz sample, m 2 M is the mass of platinum crucible and residue after HF acid digestion and ignition 3 Mass m of the platinum crucible for the unfired blank experiment 4 The mass of the platinum crucible for the blank experiment after firing is shown, and m is the mass of the high-purity quartz sample.
Further, the detection of the impurity content of the high-purity quartz comprises the following substeps:
s21, weighing the sample in a thousand-level clean laboratory, and recording 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 a blank experiment is that other analysis steps are the same as the detection steps of the content of the high-purity quartz impurities except that the high-purity quartz sample is not added;
s22, after digestion, taking out the container, placing the container in an acid dispelling instrument, and taking out the detachable SiF 4 The trapping device is arranged above the self-made polytetrafluoroethylene container and confirms SiO according to color reaction 2 Has been completely converted into SiF 4 Slowly heating to evaporate to dryness at 100 ℃ to remove HF acid completely, cooling, and taking down a SiF4 trapping device;
s23, adding a plurality of diluted HNO (HNO) with the volume of 5% into a self-made polytetrafluoroethylene container by using a liquid transfer device 3 The volume of the sample solution is recorded as v, after shaking up, inductively coupled plasma is used for generating in a hundred-grade clean laboratoryThe optical spectrometer detects the content of elements in sample liquid in the self-made polytetrafluoroethylene container, and at the moment, the concentration of the detected elements in the sample solution is recorded as c 1 The blank experiment operation is also operated according to the flow, and the concentration of the element to be measured in the blank experiment solution is recorded as c 2 Elements in the sample liquid comprise Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni and Ti;
and S24, calculating the mass fraction of the content of the detected impurity elements 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 detected 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, m 5 Is the mass of the sample.
Further, the operating conditions of the inductively coupled plasma luminescence spectrometer are as follows: the power was set to 1.1kW, the cooling gas flow was set to 12L/min, the auxiliary gas flow was set to 0.2L/min, the atomizer flow was set to 0.6L/min, the sample size was 1.5ml/min, and the sample lifting time was 15s.
Further, the principle is as follows: siO2 2 Reaction with HF to SiF 4 ，SiF 4 Reacting with sodium carbonate solution to generate H 4 SiO 4 Under acidic conditions, H 4 SiO 4 With ammonium molybdate to form yellow silicomolybdic acid complex [ H 4 (SiMo 12 O 40 )]Determination of SiO according to shade of color 2 The reaction is completely carried out, and the high-purity quartz sample is ensured to be completely dissolved, thereby avoiding SiO 2 Incomplete conversion to SiF 4 Residual SiO 2 Impurities in the crystal lattice cannot be dissolved out, so that the test result is deviated.
Furthermore, a hundred thousand grade electronic balance is required to be used for weighing the sample during weighing, electronic grade hydrofluoric acid is required for digesting the sample, and electronic grade nitric acid and ultrapure water are required for digesting the sample.
Furthermore, the mass fraction of the electronic-grade hydrofluoric acid is 40%, the content of single metal impurities is less than or equal to 1ppb, the mass fraction of the electronic-grade nitric acid is 69%, the content of single metal impurities is less than or equal to 10ppb, and the resistivity of the ultrapure water is 18.25M omega cm.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
(1) Detachable SiF matched with self-made polytetrafluoroethylene digestion tank 4 The trapping device can determine SiO by precipitation reaction and color reaction 2 The reaction is completely carried out, the high-purity quartz sample is ensured to be completely dissolved, and the test accuracy of the detection method is improved.
(2) The detection method has high test accuracy, the accuracy of the test result of impurities such as Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni and Ti in the high-purity quartz is 0.1ppm, the relative standard deviation is less than or equal to 15 percent (the test repetition times is 10 times), and the SiO detection method of the high-purity quartz has high SiO detection accuracy 2 The accuracy of the content test result is 99.9%, and the relative standard deviation is less than or equal to 5% (the test repetition times are 10 times).
Drawings
FIG. 1 is a graph of SiO vs. test parameters for example 1 of the present invention 2 The effect of the content test;
FIG. 2 shows experimental design test values of 29 sets of response surfaces in example 2 of the present invention;
FIG. 3 is a graph of the effect of the test parameters of example 2 of the present invention on the total impurity level test;
FIG. 4 is a schematic view of the external form of the self-made polytetrafluoroethylene digestion tank of the invention;
FIG. 5 isbase:Sub>A schematic sectional view of the self-made polytetrafluoroethylene digestion tank A-A of the invention.
Detailed Description
The invention provides a high-purity quartz SiO matched with a pretreatment device 2 The method for detecting the purity and the impurity content optimizes parameters before experiments.
The test result of the chemical analysis method, the amount of HF acid agent, the quality of the sample and the digestion time are found through the prophase exploratory experimentRelating to digestion temperature, in order to obtain optimized parameters, a response surface method is used for researching the influence of HF acid dosage, sample quality, digestion time and digestion temperature on a test result, and the influence of the sample quality, the HF dosage, the digestion temperature and the digestion time on SiO 2 The influence relationship of the content test is shown in FIG. 1, and the sample quality and HF dose significantly influence SiO 2 Results of content testing, siO with increasing sample mass and HF dose 2 The content test results are increased first and then decreased. And digestion temperature and 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 method comprises the steps of testing the impurity content of a high-purity quartz sample by an ICP-OES (inductively coupled plasma-optical emission spectroscopy) instrument analysis method, testing impurity elements including Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni and Ti, and similarly, taking the test value of the total impurity content as a response value, and adopting a response surface method to process SiO 2 The test parameters of the instrumental analysis method are optimized, and 29 groups of experiments are developed to research the influence of HF acid dosage, sample quality, digestion time and digestion temperature on the precision of the test result. The experimental control parameters were as follows: the dosage of HF acid is 4-20ml, the sample mass is 0.2-2.0g, the digestion time is 30-60min, the digestion temperature is 150-220 ℃, and figure 2 is the test value of the response surface. As can be seen from FIG. 2, when the test parameters are changed, the test result of the total content of impurities shows a large fluctuation, which indicates that the selected test parameters have a significant influence on the test result. The finally selected optimized test parameters are as follows: the sample mass is 2.0g, the HF dose 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 containing the high-purity quartz sample, putting the platinum crucible containing the high-purity quartz sample and the platinum crucible of a blank experiment in a muffle furnace at 960 +/-5 ℃ for burning for 3h, taking out the crucibles, putting the crucibles in a dryer, and cooling to room temperature;
s2, transferring the high-purity quartz sample to each polytetrafluoroethylene digestion tank, adding 20ml of HF acid, and placing the high-purity quartz sample in a microwave digestion instrument to digest 45m at the temperature of 150 DEG Cin and driving acid to near dryness, and adding detachable SiF 4 The collecting device is arranged above the self-made polytetrafluoroethylene container;
s3, confirming SiO according to the color reaction 2 Has been completely converted into SiF 4 Then transferring the residual liquid in the tank to a platinum crucible, washing the inner wall of the polytetrafluoroethylene digestion tank by using a small amount of water, adding a plurality of drops of water and a plurality of HF acids when the liquid in the platinum crucible is nearly dry, evaporating on an electric heating plate at 200 +/-5 ℃ until the liquid is nearly dry, adding 10ml of distilled water again, evaporating to dryness, and simultaneously carrying out a blank experiment;
s4, wiping the outer wall of the crucible with wet filter paper after cooling, placing the platinum crucible in a muffle furnace at 960 +/-5 ℃ for burning for 1h, and weighing after cooling to room temperature;
s5, calculating SiO according to a formula 2 And (4) purity.
10 replicates were performed and the results are shown in Table 1:
TABLE 1SiO 2 Content test
| Number of repetitions | SiO 2 Content average (%) | SiO 2 Content average (%) | Relative standard deviation (%) |
| 10 | 99.95 | 3.49 | 3.5 |
As can be seen from Table 1, the detection accuracy of the high-purity quartz can stably reach the level of 3N (99.9%), and the relative standard deviation of 10 repeated experiments is only 3.5%, which indicates that the accuracy of the method can meet the test requirements.
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 container in a microwave digestion instrument, and decomposing the sample at 165 ℃ for 45 min;
s2, after digestion, taking out the container, placing the container in an acid dispelling instrument, and taking out the detachable SiF 4 The trapping device is arranged above the self-made polytetrafluoroethylene container and confirms SiO according to color reaction 2 Has been completely converted into SiF 4 Then slowly heating at 100 deg.C to evaporate to remove HF acid, cooling, and removing SiF 4 A trapping device;
s3, adding a plurality of diluted HNO (HNO) with the volume of 5% into a self-made polytetrafluoroethylene container 3 After shaking up, the content of elements (including Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni and Ti) in sample liquid in a polytetrafluoroethylene container prepared by an inductively coupled plasma luminescence spectrometer in a hundred-grade clean laboratory, and blank experiment operation is also carried out according to the flow;
and S4, calculating the mass fraction of the content of the impurity elements according to a formula.
The impurity elements (Al, ca, K, cr, co, cu, zn, na, fe, mg, cd, mn, ni, ti) of the high-purity quartz sample were tested, and the results are shown in Table 2:
TABLE 2 content test of impurity elements
| 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 |
| |
0 | 0 |
| |
0 | 0 |
| Ca | 4.48 | 7.48 |
| Al | 2.28 | 16.44 |
As can be seen from Table 2, the total amount of impurities in the high-purity quartz sample is less than 100ppm, which indicates that the sample belongs to the category of 4N-grade high-purity quartz, and 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 (9)
1. High-purity quartz SiO matched with pretreatment device 2 The method for detecting the purity and the impurity content is characterized by comprising the following steps of: s1, high-purity quartz SiO 2 Detecting the purity; s2, detecting the content of high-purity quartz impurities; the high-purity quartz SiO 2 The purity detection comprises the following substeps:
s11, weighing a high-purity quartz sample in a thousand-level clean laboratory, wherein the mass is recorded as m, and weighing a platinum crucible filled with the high-purity quartz sample, and the mass is recorded as m 1 (ii) a Weighing the un-burned platinum crucible for blank experiment, and recording the mass as m 3 Blank experiment is that except for not heightening the pure quartz sample, other analysis stepsWith the high-purity quartz SiO 2 The purity detection steps are the same; placing the platinum crucible filled with the high-purity quartz sample and the platinum crucible of the blank experiment in a muffle furnace for burning, taking out the crucible, placing the crucible in a dryer, and cooling to room temperature;
s12, transferring the high-purity quartz sample to each polytetrafluoroethylene digestion tank, adding HF acid, placing the high-purity quartz sample in a microwave digestion instrument for digestion at a certain temperature and dispelling the acid until the high-purity quartz sample is nearly dry, and then removing the detachable SiF 4 The collecting device is arranged above the self-made polytetrafluoroethylene container;
s13, siO confirmation by color reaction 2 Has been completely converted into SiF 4 Then transferring the residual liquid in the tank to a platinum crucible, washing the inner wall of the polytetrafluoroethylene digestion tank by using 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 on an electric heating plate until the liquid is nearly dry, adding 10ml of distilled water again, evaporating to dryness, and simultaneously performing a blank experiment;
s14, after cooling, wiping the outer wall of the crucible with wet filter paper, placing the platinum crucible in a muffle furnace for firing, weighing when cooling to room temperature, and recording the mass as m 2 And the mass of the platinum crucible for the blank experiment after firing is recorded as m 4 ；
S15, calculating SiO according to a formula 2 And (4) purity.
2. The high-purity quartz SiO matched with pretreatment device according to claim 1 2 The method for detecting the purity and the impurity content is characterized in that the temperature of the muffle furnace in the step S11 is 960 +/-5 ℃, the ignition time is 3 hours, the temperature of the electric heating plate in the step S13 is 200 +/-5 ℃, the temperature of the muffle furnace in the step S14 is 960 +/-5 ℃, and the ignition time is 1 hour.
3. The high-purity quartz SiO matched with pretreatment device according to claim 1 2 The method for detecting the purity and the impurity content is characterized in that in the step S15, the calculation formula is as follows:
wherein w (SiO) 2 ) Is SiO in high-purity quartz 2 Mass fraction, m 1 Mass of platinum crucible and high purity quartz sample, m 2 M is the mass of platinum crucible and residue after HF acid digestion and ignition 3 Mass of platinum crucible for unfired blank experiment, m 4 The mass of the platinum crucible for the blank experiment after firing is shown, and m is the mass of the high-purity quartz sample.
4. The high-purity quartz SiO matched with pretreatment device according to claim 1 2 The method for detecting the purity and the impurity content is characterized in that the method for detecting the impurity content of the high-purity quartz comprises the following substeps:
s21, weighing the sample in a thousand-level clean laboratory, and recording 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 a blank experiment is that other analysis steps are the same as the detection steps of the content of the high-purity quartz impurities except that the high-purity quartz sample is not added;
s22, after digestion, taking out the container, placing the container in an acid dispelling instrument, and taking out the detachable SiF 4 The trapping device is arranged above the self-made polytetrafluoroethylene container and confirms SiO according to color reaction 2 Has been completely converted into SiF 4 Then slowly heating at 100 deg.C to evaporate to remove HF acid, cooling, and removing SiF 4 A trapping device;
s23, adding a plurality of diluted HNO (HNO) with the volume of 5% into a self-made polytetrafluoroethylene container by using a liquid transfer device 3 The volume of the sample solution is recorded as v, after shaking up, the content of the element in the sample liquid in the self-made polytetrafluoroethylene container is detected by using an inductively coupled plasma luminescence spectrometer in a hundred-grade clean laboratory, and at the moment, the concentration of the detected element in the sample solution is recorded as c 1 The blank experiment operation is also operated according to the flow, and the concentration of the element to be measured in the blank experiment solution is recorded as c 2 The elements in the sample liquid comprise Al, ca, K, cr, co, cu, zn and Na、Fe、Mg、Cd、Mn、Ni、Ti；
And S24, calculating the mass fraction of the content of the detected impurity elements according to a formula.
5. The high-purity quartz SiO matched with pretreatment device according to claim 3 2 The method for detecting purity and impurity content is characterized in that the calculation formula in the step S24 is as follows:
w (impurity) is the mass fraction of the content of the element to be detected 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, m 5 Is the mass of the sample.
6. The high-purity quartz SiO matched with pretreatment device according to claim 4 2 The method for detecting the purity and the impurity content is characterized in that the working conditions of the inductively coupled plasma luminescence spectrometer are as follows: the power was set to 1.1kW, the cooling gas flow was set to 12L/min, the auxiliary gas flow was set to 0.2L/min, the atomizer flow was set to 0.6L/min, the sample size was 1.5ml/min, and the sample lifting time was 15s.
7. The high-purity quartz SiO matched with pretreatment device according to any one of claims 1 to 6 2 The method for detecting the purity and the impurity content is characterized by comprising the following steps of: siO2 2 Reaction with HF to form SiF 4 ，SiF 4 Reacting with sodium carbonate solution to generate H 4 SiO 4 Under acidic conditions, H 4 SiO 4 With ammonium molybdate to form yellow silicomolybdic acid complex [ H 4 (SiMo 12 O 40 )]Determination of SiO from shade of color 2 The reaction is completely carried out, and the high-purity quartz sample is ensured to be completely dissolved, thereby avoiding SiO 2 Incomplete conversion to SiF 4 Residual SiO 2 Lattice of the crystalThe impurities in (1) cannot be dissolved out, so that the test result is deviated.
8. The high-purity quartz SiO matched with pretreatment device according to claim 1 or 4 2 The method for detecting the purity and the impurity content is characterized in that a hundred thousand-level electronic balance is used for weighing a sample during weighing, electronic-level hydrofluoric acid is used for digesting the sample, and electronic-level nitric acid and ultrapure water are used.
9. The high-purity quartz SiO matched with pretreatment device of claim 8 2 The method for detecting the purity and the impurity content is characterized in that the mass fraction of the electronic-grade hydrofluoric acid is 40%, the content of a single metal impurity is less than or equal to 1ppb, the mass fraction of the electronic-grade nitric acid is 69%, the content of the single metal impurity is less than or equal to 10ppb, and the resistivity of the ultrapure water is 18.25M omega cm.
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