CN111060581A - Method for measuring metal impurities of solar-grade polycrystalline silicon substrate - Google Patents
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Abstract
The invention discloses a method for measuring metal impurities of a solar-grade polycrystalline silicon substrate, which comprises the following steps: preparing a sample; sample treatment; taking out the digestion tank after digestion is finished, cooling, pouring the digestion solution into an acid dispelling tank, placing the acid dispelling tank into an acid dispelling device, adding ultrapure hydrofluoric acid after a sample is evaporated to dryness, continuing to evaporate to dryness, taking out and cooling, and adding 2g of nitric acid solution; preparing a blank of a sample; preparing a standard use solution; testing the standard use solution and drawing a working curve; measuring the content of metal elements in the sample to obtain a measured value of the sample; testing the content of each metal element in a blank of the sample; calculating an analysis result; according to the measuring method, the polycrystalline silicon sample is processed by the microwave digestion instrument, the content of the trace metal elements in the solar-grade polycrystalline silicon substrate is measured by the inductively coupled plasma mass spectrometer, the content of each metal impurity in the polycrystalline silicon sample can be accurately measured, and guidance is provided for production of solar-grade polycrystalline silicon.
Description
Technical Field
The invention relates to the technical field of chemical new energy equipment, in particular to a method for measuring metal impurities of a solar-grade polycrystalline silicon substrate.
Background
The solar grade polysilicon is an important semiconductor material, is widely used in photovoltaic and electronic industries, and is also a basic material of a solar cell, the content of metal impurities is low, and the content of the metal impurities has great influence on the conductivity, the product service life and the photoelectric conversion efficiency of the solar grade polysilicon, so that the accurate measurement of the content of the metal impurities has very important significance on the production of the solar grade polysilicon.
Disclosure of Invention
In view of the above, the present invention provides a method for measuring metal impurities in a solar-grade polysilicon matrix, so as to accurately measure the content of metal impurities in the solar-grade polysilicon.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for measuring metal impurities in a solar-grade polycrystalline silicon substrate comprises the following steps:
1) preparing a sample, namely crushing a polycrystalline silicon sample into particles, adding a mixed acid soaking solution, soaking for a first preset time, and then cleaning and drying;
2) sample treatment, namely weighing 0.4-0.5g of the sample prepared in the step 1), placing the sample in a microwave digestion tank, adding ultrapure water and mixed acid solution, wherein the volume ratio of the ultrapure water to the mixed acid solution is 1:4, and then placing the digestion tank in a microwave digestion instrument for digestion;
3) taking out the digestion tank after digestion, cooling, pouring the digestion solution into an acid dispelling tank, placing the acid dispelling tank in an acid dispelling device with constant temperature of 180 ℃ to dispel SiF4After the sample is evaporated to dryness, adding 2mL of ultrapure hydrofluoric acid, continuing to evaporate to dryness, taking out and cooling, and adding 2g of nitric acid solution;
4) preparing a sample blank according to the steps 2) to 3) without adding a sample;
5) preparing standard use solution, respectively adding 0, 25, 75, 125 and 250 mu l of mixed standard solution into five volumetric flasks, quantifying to 25g, shaking up, wherein the concentrations of iron, chromium, nickel, copper and zinc in the series of mixed standard solution are respectively 1, 3, 5 and 10 mu g/ml;
6) testing the standard use solution prepared in the step 5) by using an inductively coupled plasma mass spectrometer and drawing a working curve;
7) measuring the content of metal elements in the sample obtained in the step 3) to obtain a sample measurement value;
8) adding 2.0g of nitric acid solution into the blank of the sample prepared in the step 4), standing for a second preset time, and testing the content of each metal element in the blank of the sample;
9) and (3) calculating an analysis result, wherein the content of the metal elements in the polycrystalline silicon is calculated according to the formula (1):
in the formula:
omega-metal impurity content in the polysilicon, unit nanogram per gram (ng/g); c1-value determined for metal impurities in the sample in nanograms per gram (ng/g); c2-measured value of metallic impurities in the blank sample, in nanograms per gram (ng/g); 2-quantitative value of sample and sample blank solution, unit g; m 1-sample weight, unit g.
Preferably, in the step 1), the polysilicon sample is crushed into silicon grains with the diameter of 2mm-4 mm.
Preferably, the mixed acid soaking liquid is prepared from ultrapure nitric acid, ultrapure hydrofluoric acid and ultrapure water according to a mass ratio MHNO3：MHF：MH206: 18; 76 are mixed and configured.
Preferably, the mixed acid solution is prepared by mixing ultrapure nitric acid and ultrapure hydrofluoric acid according to a mass ratio MHNO3：MHF1: 3 are mixed and prepared.
Preferably, the drying in step 1) is performed under the protection of argon.
Preferably, in said step 7), at least three measurements are performed on the sample, and then the arithmetic mean is taken as the final sample measurement value.
Preferably, the acid removing process in the step 3) is carried out in a hundred-grade fume hood.
Preferably, the inductively coupled plasma mass spectrometer comprises a high salt tolerant sample injection system.
Preferably, the first preset time is 12 h.
Preferably, the second preset time is 5 min.
In order to achieve the aim, the invention provides a method for measuring metal impurities in a solar-grade polycrystalline silicon substrate, which comprises the following steps: 1) preparing a sample, namely crushing a polycrystalline silicon sample into particles, adding a mixed acid soaking solution to soak for a first preset time, and then cleaning and drying; 2) sample treatment, namely weighing 0.4-0.5g of the sample prepared in the step 1), placing the sample in a microwave digestion tank, adding ultrapure water and mixed acid solution, wherein the volume ratio of the ultrapure water to the mixed acid solution is 1:4, and then placing the digestion tank in a microwave digestion instrument for digestion; 3) taking out the digestion tank after digestion, cooling, pouring the digestion solution into an acid dispelling tank, placing the acid dispelling tank in an acid dispelling device with constant temperature of 180 ℃ to dispel SiF4After the sample is evaporated to dryness, 2mL of ultrapure hydrofluoric acid is added, evaporation to dryness is continued, the sample is taken out for cooling, and 2g of nitric acid solution is added; 4) preparing a sample blank according to the steps 2) to 3) without adding a sample; 5) preparing standard use solution, adding 0, 25, 75, 125 and 250 mu l of mixed standard solution into five volumetric flasks respectively, quantifying to 25g, shaking up, wherein the concentrations of iron, chromium, nickel, copper and zinc in the series of mixed standard solution are 1, 3, 5 and 10 mu g/ml respectively; 6) testing the standard use solution prepared in the step 5) by using an inductively coupled plasma mass spectrometer and drawing a working curve; 7) measuring the content of metal elements in the sample obtained in the step 3) to obtain a sample measurement value; 8) adding 2.0g of nitric acid solution into the blank of the sample prepared in the step 4), standing for a second preset time, and testing the content of each metal element in the blank of the sample; 9) calculating an analysis result; according to the measuring method, the microwave digestion instrument is used for processing the polycrystalline silicon sample, the inductively coupled plasma mass spectrometer (ICP-MS) is used for measuring the content of trace elements Fe, Cr, Ni, Cu and Zn in the solar-grade polycrystalline silicon substrate, the content of each metal impurity in the polycrystalline silicon sample can be accurately measured, and guidance is provided for production of solar-grade polycrystalline silicon.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method for measuring metal impurities in a solar-grade polysilicon substrate according to an embodiment of the present invention.
Detailed Description
The core of the invention is to provide a method for measuring metal impurities in a solar-grade polycrystalline silicon substrate, which can accurately measure the content of the metal impurities in the solar-grade polycrystalline silicon.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the method for measuring metal impurities in a solar-grade polysilicon matrix according to an embodiment of the present invention includes:
step1, preparing a sample, namely crushing the polysilicon sample into particles, adding a mixed acid soaking solution, soaking for a first preset time, and then cleaning and drying;
simultaneously preparing reagents, materials and instruments, comprising:
high-purity argon gas: the purity is more than or equal to 99.999 percent;
high-purity hydrogen: the purity is more than or equal to 99.999 percent;
high purity helium gas: the purity is more than or equal to 99.999 percent;
ultrapure water: the resistivity is more than or equal to 18.2 MOmega, the TOC is less than or equal to 5ppb, and each element is less than 20 ng/L;
ultra-pure nitric acid: the concentration of HNO3 is 65-68%, and the impurity of each metal element is lower than 10 ng/L;
ultrapure hydrofluoric acid: the concentration of HF is 49%, and the impurity of each metal element is lower than 10 ng/L;
standard stock solutions: the concentrations of iron, chromium, nickel, copper and zinc are all 1mg/mL, and certified standard substances which can be traced back by quantitative values at home and abroad are adopted;
mixing standard solutions: diluting standard stock solutions of iron, chromium, nickel, copper and zinc step by step to prepare a mixed standard solution, wherein the concentration of each element in the mixed standard solution is 1 mu g/ml;
nitric acid solution: the mass ratio of the ultrapure nitric acid to the ultrapure water is MHNO3：MH20＝3：97；
Mixed acid solution: the mass ratio of the ultrapure nitric acid to the ultrapure hydrofluoric acid is MHNO3：MHF＝1：3；
Mixed acid soaking solution: the mass ratio of the ultrapure nitric acid to the ultrapure hydrofluoric acid to the ultrapure water is MHNO3：MHF：MH20＝6： 18；76；
Breaking hammer: a tungsten cobalt alloy.
A crushing plate: tungsten cobalt alloy
Volumetric flask: 60ml in specification and made of fep. Before use, the mixture is soaked in 20% nitric acid solution for more than 24h, washed with ultrapure water and dried under the protection of argon;
acid removing tank: the PTFE material with the specification of 70mL is soaked in 20% nitric acid solution for more than 24 hours before use, washed by ultrapure water and dried under the protection of argon;
beaker: the standard is 100ml, the material PTFE or FEP material is soaked in 20% nitric acid for more than 24h before use, washed with ultrapure water and dried under the protection of argon;
an ultra-pure water machine: the water inlet requirement is more than 16M omega, the water outlet is 18.2M omega, the TOC is less than or equal to 5ppb, and each element is less than 20 ng/L;
a liquid transferring gun: specification: 10-100 μ L.
A liquid transferring gun: specification: 100-.
Acid-expelling device: the temperature difference between the holes is less than or equal to +/-1 ℃ and @100 ℃.
Analytical balance: the sensory dose is 0.0001 g.
A microwave digestion instrument;
a microwave digestion tank: specification: 70ml, model: the inner wall and the inner cover of the digestion tank are soaked in 20 percent nitric acid solution for more than 24 hours before use and are cleaned by ultrapure water;
an inductively coupled plasma mass spectrometer equipped with a high salt tolerant sample introduction system (HMI);
a hundred-level fume hood;
an electric hot plate;
a quartz cover: the material is as follows: high-purity quartz with air inlet and outlet;
when preparing a sample, selecting a polysilicon silicon block with a compact surface and the middle part of a silicon rod, wherein the diameter of the silicon block is about 3cm, then placing the silicon block on a crushing plate, crushing the silicon block into silicon particles by using a crushing hammer, in the embodiment of the invention, crushing a polysilicon sample into the silicon particles with the diameter of 2mm-4mm, placing the silicon particles in a beaker, adding 20ml of mixed acid soaking solution, soaking for 12 hours, then cleaning the silicon particles by using ultrapure water, placing the beaker on an electric heating plate with the temperature of 105 ℃, covering a quartz cover, introducing argon, and drying for later use.
Step2, sample treatment, namely weighing 0.4-0.5g of the sample prepared in the Step 1), placing the sample into a microwave digestion tank, and adding ultrapure water and mixed acid solution, wherein the volume ratio of the ultrapure water to the mixed acid solution is 1:4 (2 ml: 8ml), then placing the digestion tank into a microwave digestion instrument for digestion, wherein the mass of the sample silicon briquette treated by microwave digestion is controlled to be 0.4-0.5g, too much digestion tank pressure is too large in the digestion process, and too little error is increased;
the digestion procedure was as follows:
step3, taking out the digestion tank after digestion, cooling, pouring the digestion solution into an acid removing tank, placing the acid removing tank in an acid removing device with constant temperature of 180 ℃ to remove SiF4After the sample is evaporated to dryness, 2mL of ultrapure hydrofluoric acid is added, evaporation to dryness is continued, the sample is taken out for cooling, and 2g of nitric acid solution is added;
the acid removal process is carried out in a hundred-grade fume hood.
Step4, preparing a sample blank according to the Step 2-the Step3 without adding a sample;
step5, preparing standard use solution, adding 0, 25, 75, 125 and 250 mu l of mixed standard solution into five volumetric flasks respectively, quantifying to 25g, shaking up, wherein the concentrations of iron, chromium, nickel, copper and zinc in the series of mixed standard solution are 1, 3, 5 and 10 mu g/ml respectively; the prepared standard use liquid series should be as close as possible to the concentration value of the element to be detected in the sample.
Step6, testing the standard use solution prepared in the Step5 by using an inductively coupled plasma mass spectrometer and drawing a working curve;
before using the inductively coupled plasma mass spectrometer, it is enough to ensure argon gas, high-purity oxygen volume to start circulating water machine, press from both sides the peristaltic pump and press from both sides, ignite the inductively coupled plasma mass spectrometer, after equipment is stable, debugging equipment, equipment main set up the parameter as follows:
step7, measuring the content of metal elements in the sample obtained in the Step3 to obtain a sample measurement value;
after the working curve is drawn, sequentially measuring, independently testing for three times, and taking an arithmetic mean value as a sample measurement value;
step8, adding 2.0g of nitric acid solution into the blank of the sample prepared in the Step4, standing for a second preset time, and testing the content of each metal element in the blank of the sample;
the second preset time is 5 min.
Step9, calculating the analysis result, and calculating the content of the metal elements in the polysilicon according to the formula (1):
in the formula:
omega-metal impurity content in the polysilicon, unit nanogram per gram (ng/g); c1-value determined for metal impurities in the sample in nanograms per gram (ng/g); c2-measured value of metallic impurities in the blank sample, in nanograms per gram (ng/g); 2-quantitative value of sample and sample blank solution, unit g; m 1-sample weight, unit g.
Compared with the prior art, the method for measuring the metal impurities in the solar-grade polycrystalline silicon matrix provided by the embodiment of the invention has the advantages that the polycrystalline silicon sample is processed by using the microwave digestion instrument, the contents of trace elements Fe, Cr, Ni, Cu and Zn in the solar-grade polycrystalline silicon matrix are measured by using the inductively coupled plasma mass spectrometer (ICP-MS), the contents of the metal impurities in the polycrystalline silicon sample can be accurately measured, and guidance is provided for the production of solar-grade polycrystalline silicon.
It should be noted that the environment of the laboratory and the cleanliness of the container have a great influence on the experimental results, and can be eliminated by deducting the blank of the sample.
In the measuring process, Si element has large interference on measuring elements, and proper isotopes can be selected for element measurement according to the response intensity and interference condition of the elements, wherein the recommended isotopes of each element are as follows:
the embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for measuring metal impurities in a solar-grade polycrystalline silicon substrate is characterized by comprising the following steps:
1) preparing a sample, namely crushing a polycrystalline silicon sample into particles, adding a mixed acid soaking solution, soaking for a first preset time, and then cleaning and drying;
2) sample treatment, namely weighing 0.4-0.5g of the sample prepared in the step 1), placing the sample in a microwave digestion tank, adding ultrapure water and mixed acid solution, wherein the volume ratio of the ultrapure water to the mixed acid solution is 1:4, and then placing the digestion tank in a microwave digestion instrument for digestion;
3) taking out the digestion tank after digestion, cooling, pouring the digestion solution into an acid dispelling tank, placing the acid dispelling tank in an acid dispelling device with constant temperature of 180 ℃ to dispel SiF4After the sample is evaporated to dryness, 2mL of ultrapure hydrofluoric acid is added, evaporation to dryness is continued, the sample is taken out for cooling, and 2g of nitric acid solution is added;
4) preparing a sample blank according to the steps 2) to 3) without adding a sample;
5) preparing standard use solution, respectively adding 0, 25, 75, 125 and 250 mu l of mixed standard solution into five volumetric flasks, quantifying to 25g, shaking up, wherein the concentrations of iron, chromium, nickel, copper and zinc in the series of mixed standard solution are respectively 1, 3, 5 and 10 mu g/ml;
6) testing the standard use solution prepared in the step 5) by using an inductively coupled plasma mass spectrometer and drawing a working curve;
7) measuring the content of metal elements in the sample obtained in the step 3) to obtain a sample measured value;
8) adding 2.0g of nitric acid solution into the blank of the sample prepared in the step 4), standing for a second preset time, and testing the content of each metal element in the blank of the sample;
9) and (3) calculating an analysis result, wherein the content of the metal elements in the polycrystalline silicon is calculated according to the formula (1):
in the formula:
omega-metal impurity content in the polysilicon, unit nanogram per gram (ng/g); c1-value determined for metal impurities in the sample in nanograms per gram (ng/g); c2-measured value of metallic impurities in the blank sample, in nanograms per gram (ng/g); 2-quantitative value of sample and sample blank solution, unit g; m 1-sample weight, unit g.
2. The method for measuring the solar-grade polysilicon matrix metal impurities according to claim 1, wherein in the step 1), the polysilicon sample is crushed into silicon grains with the diameter of 2mm-4 mm.
3. The method for measuring the metal impurities in the solar-grade polysilicon matrix according to claim 1, wherein the mixed acid soaking solution is prepared from ultrapure nitric acid, ultrapure hydrofluoric acid and ultrapure water according to a mass ratio MHNO3：MHF：MH206: 18; 76 are mixed and configured.
4. The method for measuring the metal impurities in the solar-grade polysilicon matrix according to claim 1, wherein the mixed acid solution is prepared by mixing ultrapure nitric acid and ultrapure hydrofluoric acid according to a mass ratio MHNO3：MHF1: 3 are mixed and prepared.
5. The method for measuring metal impurities in a solar-grade polysilicon substrate according to any one of claims 1 to 4, wherein the step 1) of drying is performed under argon protection.
6. The method as claimed in any one of claims 1 to 4, wherein in the step 7), the measurement of the metal impurities in the solar-grade polysilicon substrate is performed at least three times, and then the arithmetic mean value is taken as a final measurement value of the sample.
7. The method as claimed in any one of claims 1 to 4, wherein the acid-removing process in step 3) is performed in a hundred-class fume hood.
8. The method of any one of claims 1 to 4, wherein the inductively coupled plasma mass spectrometer comprises a high salt tolerant sample injection system.
9. The method as claimed in any one of claims 1 to 4, wherein the first predetermined time is 12 hours.
10. The method as claimed in any one of claims 1 to 4, wherein the second predetermined time is 5 min.
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Application publication date: 20200424 |