CN101685048B - Purity detecting method and device for polysilicon - Google Patents
Purity detecting method and device for polysilicon Download PDFInfo
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- CN101685048B CN101685048B CN200810223000A CN200810223000A CN101685048B CN 101685048 B CN101685048 B CN 101685048B CN 200810223000 A CN200810223000 A CN 200810223000A CN 200810223000 A CN200810223000 A CN 200810223000A CN 101685048 B CN101685048 B CN 101685048B
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 20
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 20
- 239000004809 Teflon Substances 0.000 claims abstract description 31
- 229920006362 Teflon® Polymers 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000007789 sealing Methods 0.000 claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004033 plastic Substances 0.000 claims abstract description 15
- 229920003023 plastic Polymers 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 229920005862 polyol Polymers 0.000 claims abstract description 8
- 150000003077 polyols Chemical class 0.000 claims abstract description 8
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- 235000013312 flour Nutrition 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000005260 corrosion Methods 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- 235000009508 confectionery Nutrition 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 description 11
- 239000010703 silicon Substances 0.000 description 11
- 229910052796 boron Inorganic materials 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000003039 volatile agent Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000010186 staining Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000673 graphite furnace atomic absorption spectrometry Methods 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- -1 this Chemical compound 0.000 description 1
- 238000000624 total reflection X-ray fluorescence spectroscopy Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
本发明实施方式提供了一种多晶硅的纯度检测方法及装置，该方法及装置属于化工和太阳能领域，该方法包括：将硅粉混合均匀后，用二次去离子水洗涤，然后烘干至恒重；将烘干后的硅粉放入Teflon盘子中，加水润湿样品，并加入多羟基化合物溶液；将所述Teflon盘子放置在Teflon容器上并放置于密封体中，在所述密封体低部加入HF和HNO3，密封所述密封体后加热到110～120℃；当硅粉全部消解完全，并挥发至干燥后，加入HNO3溶解残渣后，转移至塑料容量瓶并定容后测定杂质元素的含量。本发明具体实施方式还提供一种实现多晶硅的纯度检测方法的专用装置，该方法及装置具有检测准确度高的优点。
The embodiment of the present invention provides a method and device for detecting the purity of polysilicon. The method and device belong to the fields of chemical industry and solar energy. Heavy; put the dried silicon powder into a Teflon dish, add water to wet the sample, and add the polyol solution; place the Teflon dish on the Teflon container and place it in the sealing body, and place it in the lower part of the sealing body Add HF and HNO3 partially, seal the sealing body and heat to 110-120°C; when the silicon powder is completely digested and volatilized to dryness, add HNO3 to dissolve the residue, transfer to a plastic volumetric flask and measure impurity elements after constant volume content. The specific embodiment of the present invention also provides a special device for realizing the method for detecting the purity of polysilicon, and the method and device have the advantage of high detection accuracy.
Description
Technical field
The present invention relates to chemical industry and field of solar energy, relate in particular to a kind of method for detecting purity and device of polysilicon.
Background technology
Along with expanding economy and quickening of urbanization process; Also increasing to demands for energy; And present employed main energy sources oil is a nonrenewable resources, and the waste gas that uses the back to produce is very big to the influence of environment, so each state all steps up the research to renewable resource such as sun power.Polysilicon is the main flow material of solar cell, and its supply/demand is restricting the development of solar energy industry, and the purity of polysilicon is to determine whether it can be used for the important indicator of solar cell.
In order to detect the purity of polysilicon, prior art provides a kind of method for detecting purity of polysilicon, and this method is as shown in Figure 1, comprising:
Step 11, to choose the phosphorus weight percentage be 0.0025～0.5% accurate solar-grade metallic silicon sample, places acid-resistant container;
Step 12, add 4～5mL distilled water, 15～20mL nitric acid, 4～6mL perchloric acid, mixing successively according to every gram metallic silicon sample;
Step 13, slowly add 1～2mL hydrofluorite, add 10～15mL hydrofluorite again according to every gram metallic silicon sample;
Step 14, when the dissolving of most of metallic silicon, move to temperature and be the surplus 0.5～1mL of heating evaporation to above-mentioned solution on 150～200 ℃ the electric hot plate;
Step 15, above-mentioned solution is taken off cooling, adding 12～14mL volumetric concentration by every gram metallic silicon sample is 10% nitric acid, adds distilled water again to 250mL, the content of mixing constant volume rear impurity element.
In realizing process of the present invention, the inventor finds that there is following problem in prior art:
In the digestion process of the technical scheme that prior art provides to silicon appearance, reaction is violent, makes the solution boiling easily, causes the volatilization of elements such as As in the volatile compound, B, P, makes that the impurity content test result is on the low side, reduces the accuracy of analytical test.
Summary of the invention
Embodiment of the present invention provides a kind of method for detecting purity of polysilicon, and this method is checked for impurities content accurately, improves the advantage of the accuracy of analyzing and testing.
The specific embodiment of the invention provides a kind of method for detecting purity of polysilicon, and this method comprises:
A, silica flour mixed after, with secondary deionized water washing 2～5 times, dry then to constant weight;
B, dried silicon powder is put into the Teflon plate, add the water-wet sample, and to add 0.3mL～1mL concentration be the polyol solution of 2.5g/L;
C, said Teflon plate is placed on the Teflon container and is positioned in the seal, after said seal bottom adds the HF of 7mL～10mL top grade purity and the HNO3 of 2mL～3mL top grade purity, seals said seal, be heated to 110～120 ℃; Said seal is the closed container of heat-resisting acid corrosion-resistant;
D, all clear up fully, after opening said seal and evaporating into drying, in said Teflon plate, add 5mL～10mL HNO when silica flour
3Behind the dissolved residue, be transferred to the plastics volumetric flask;
Said 5mL～10mL HNO
3Be HNO
3With the volume ratio of water be 1: 1 HNO
3
E, with secondary deionized water to said plastics volumetric flask constant volume after, measure the content of impurity element.
Can find out that by the above-mentioned technical scheme that provides the technical scheme of the embodiment of the invention is decomposed through steam and cleared up silicon sample, and heating process all is in the environment of sealing, to carry out; So effectively avoided staining of silica flour, greatly eliminated the influence of impurity in the solvent, greatly reduced blank value; Eliminated the interference that matrix is brought when analytical test, reduced the volatilization of elements such as the As be present in the volatile compound, B, P, thereby improved the precision that detects; This method is arranged through selecting the volumetric flask of plastics for use again; Reduce the boron element that sticks on the bottle wall like this, further improved accuracy of detection, improved the accuracy of analytical test.
Description of drawings
The process flow diagram of the method for detecting purity of a kind of polysilicon that Fig. 1 provides for prior art.
Fig. 2 provides a kind of process flow diagram of method for detecting purity of polysilicon for the specific embodiment of the invention.
The process flow diagram of the method for detecting purity of a kind of polysilicon that Fig. 3 provides for present embodiment 1.
The structural drawing of the isolated plant of a kind of method for detecting purity of realizing polysilicon that Fig. 4 provides for the specific embodiment of the invention.
The A-A cut-open view of the isolated plant that Fig. 5 provides for the specific embodiment of the invention.
Embodiment
Embodiment of the present invention provides a kind of method for detecting purity of polysilicon, and this method is as shown in Figure 2, comprising:
Step 21, silica flour mixed after, with secondary deionized water washing 2～5 times, dry then to constant weight;
Step 22, dried silicon powder is put into the Teflon plate, add the water-wet sample, and to add 0.3mL～1mL concentration be the polyol solution of 2.5g/L;
The preferred sweet mellow wine of polyol in this step also can be other polyol certainly in actual conditions, like glycerine etc.
Step 23, this Teflon plate is placed on the Teflon container and is positioned in the seal, add the HF of 7mL～10mL top grade purity and the HNO of 2mL～3mL top grade purity in sealing body bottom
3, be heated to 110～120 ℃ behind the sealing sealing body;
Seal in this step can be the closed container of heat-resisting acid corrosion-resistant.
Step 24, after silica flour is all cleared up fully, is evaporated into drying, add 5mL～10mL HNO
3(1+1) dissolved residue is transferred to the plastics volumetric flask.
HNO in this step
3(1+1) expression HNO
3With the volume ratio of water be 1: 1.
Step 25, measure the content of impurity element after to this plastics volumetric flask constant volume with secondary deionized water.
Realize this step method can for; Measure the content of impurity element with ICP-AES; Certainly in actual conditions, also can use other method of the prior art (like GFAAS; IC, TXRF etc.) measure the content of impurity element, the specific embodiment of the invention is not limited to the concrete grammar of measuring impurity content.
For the principle of work of each system better is described, combine specific embodiment and accompanying drawing that the method for refining of a kind of metallic silicon provided by the invention is carried out detailed explanation at present.
Embodiment 1: the specific embodiment of the invention 1 provides a kind of method for detecting purity of polysilicon, and the technological scene of present embodiment is that present embodiment is broken with the polycrystal silicon ingot of 10g, through pulverizing, ball milling, obtains silica flour; The deionized water that present embodiment is selected for use is a distilled water; The polyol that present embodiment is selected for use can be sweet mellow wine.This method is as shown in Figure 3: comprising:
Step 31, with silica flour with second distillation water washing 3 times after, dry to constant weight;
Step 32, the silica flour that takes by weighing 0.5000g are positioned in the Teflon plate, add the water-wet sample, and to add 0.5mL concentration be the mannitol solution of 2.5g/L;
The weight that takes by weighing silica flour in this step is accurate to 0.1mg.
Step 33, the Teflon plate is placed with Teflon container top and placed in the seal, add 10mL hydrofluorite (GR), 2～3mL nitric acid (GR) back sealing sealing body in sealing body bottom;
GR in this step representes top grade purity, and its concrete standard can be referring to " State Standard of the People's Republic of China's chemical reagent "
The sealing body can be the airtight container of heat-resisting acid corrosion-resistant.
Step 34, the sealing body is heated to 110～120 ℃;
Step 35, after the silica flour in the Teflon plate is cleared up fully and is evaporated into drying, open the sealing body, in the Teflon plate, add 5mL HNO
3(1+1) behind the dissolved residue, be transferred to 50ml plastics volumetric flask;
Step 36, with second distillation water washing Teflon plate 2～5 times, and inject 50mL plastics volumetric flask;
Plastics volumetric flask in this step also can use other capacity, like 100mL or 200mL, present embodiment does not limit to its concrete capacity.
Step 37, with redistilled water to 50mL plastics volumetric flask constant volume after, adopt ICP-AES to measure the content of impurity element.
The beneficial effect of present embodiment is described through the principle of work of present embodiment below, and the boron in the present embodiment forms BF in digestion process
3, volatile, sweet mellow wine then forms more stable complex compound with boric acid, and the complex compound that forms is not volatile, has avoided the loss of boron like this, thus improved the precision that detects; It is to utilize the steam decomposition method to clear up silicon sample that this method is arranged again; And heating process all is in the environment of sealing, to carry out, so effectively avoided staining of silica flour, has greatly eliminated the influence of impurity in the solvent; Greatly reduced blank value; Eliminated the interference that matrix is brought when analytical test, reduced the volatilization of elements such as the As be present in the volatile compound, B, P, thereby further improved the precision that detects.Volumetric flask in this method adopts the volumetric flask of plastics, has reduced the boron element that sticks on the bottle wall like this, has improved accuracy of detection.
The method that the specific embodiment of the invention provides is decomposed through steam and to be cleared up silicon sample, and heating process all is in the environment of sealing, to carry out; So effectively avoided staining of silica flour, greatly eliminated the influence of impurity in the solvent, greatly reduced blank value; Eliminated the interference that matrix is brought when analytical test, reduced the volatilization of elements such as the As be present in the volatile compound, B, P, thereby improved the precision that detects; This method is arranged through selecting the volumetric flask of plastics for use again; Reduce the boron element that sticks on the bottle wall like this, further improved accuracy of detection, improved the accuracy of analytical test.
The specific embodiment of the invention also provides a kind of isolated plant of realizing the method for detecting purity of polysilicon; This device is like Fig. 4 and shown in Figure 5; Comprise: Teflon plate 51, Teflon container 52 and seal 53; Teflon plate 51 is placed on the Teflon container 52 and is positioned in the seal 53, and seal 53 can and can seal Teflon plate 51 and Teflon container 52 for the closed container of heat-resisting acid corrosion-resistant.
The isolated plant of the method for detecting purity of the realization polysilicon that the specific embodiment of the invention provides comprises: Teflon plate 51, Teflon container 52 and seal 53; Sealing body 53 can and can seal Teflon plate 51 and Teflon container 52 for the closed container of heat-resisting acid corrosion-resistant, thereby has supported the realization of above-mentioned detection method.
In sum, the technical scheme that the specific embodiment of the invention provides has the accuracy in detection height, has improved the advantage of the accuracy of analytical test.
The above; Be merely the preferable embodiment of the present invention; But protection scope of the present invention is not limited thereto; Any technician who is familiar with the present technique field is in the technical scope that the embodiment of the invention discloses, and the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (2)
1. the method for detecting purity of a polysilicon is characterized in that, said method comprises:
A, silica flour mixed after, with secondary deionized water washing 2～5 times, dry then to constant weight;
B, dried silicon powder is put into the Teflon plate, add the water-wet sample, and to add 0.3mL～1mL concentration be the polyol solution of 2.5g/L;
C, said Teflon plate is placed on the Teflon container and is positioned in the seal, add the HF of 7mL～10mL top grade purity and the HNO of 2mL～3mL top grade purity in said seal bottom
3, be heated to 110～120 ℃ after sealing said seal; Said seal is the closed container of heat-resisting acid corrosion-resistant;
D, all clear up fully, after opening said seal and evaporating into drying, in said Teflon plate, add 5mL～10mL HNO when silica flour
3Behind the dissolved residue, be transferred to the plastics volumetric flask;
Said 5mL～10mL HNO
3Be HNO
3With the volume ratio of water be the HNO of 1:1
3
E, with secondary deionized water to said plastics volumetric flask constant volume after, measure the content of impurity element;
Said polyol is sweet mellow wine or glycerine.
2. method according to claim 1 is characterized in that, said method also comprises before the step e carrying out: with said Teflon plate with secondary deionized water washing 2～5 times and be injected into said plastics volumetric flask.
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| CN200810223000A CN101685048B (en) | 2008-09-25 | 2008-09-25 | Purity detecting method and device for polysilicon |
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|---|---|---|---|
| CN200810223000A CN101685048B (en) | 2008-09-25 | 2008-09-25 | Purity detecting method and device for polysilicon |
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| CN101685048A CN101685048A (en) | 2010-03-31 |
| CN101685048B true CN101685048B (en) | 2012-10-24 |
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| CN103344471B (en) * | 2013-07-09 | 2016-05-25 | 青岛隆盛晶硅科技有限公司 | A kind of polysilicon preprocess method of adjusting nitric acid dropping concentration |
| CN104568535A (en) * | 2013-10-29 | 2015-04-29 | 中芯国际集成电路制造(上海)有限公司 | VPD sample collection method |
| CN107764625A (en) * | 2017-09-28 | 2018-03-06 | 广州中科检测技术服务有限公司 | One heavy metal species Water bath pre-treatment apparatus |
| CN110398402B (en) * | 2019-07-22 | 2020-12-11 | 中国科学院地球环境研究所 | A method for purifying rocks or sand-like quartz with different mineral compositions |
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| JP2658863B2 (en) * | 1993-12-29 | 1997-09-30 | 日本電気株式会社 | Method for analyzing impurities in silicon thin films |
| CN1962435A (en) * | 2006-10-31 | 2007-05-16 | 锦州新世纪石英玻璃有限公司 | Production process of solar energy grade polysilicon |
| CN200957306Y (en) * | 2006-10-09 | 2007-10-10 | 张和清 | Pallet for microwave closed extractor |
| CN101061065A (en) * | 2004-11-30 | 2007-10-24 | 日本宇宙能源株式会社 | Process for producing polycrystalline silicon bar |
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2008
- 2008-09-25 CN CN200810223000A patent/CN101685048B/en not_active Expired - Fee Related
Patent Citations (4)
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|---|---|---|---|---|
| JP2658863B2 (en) * | 1993-12-29 | 1997-09-30 | 日本電気株式会社 | Method for analyzing impurities in silicon thin films |
| CN101061065A (en) * | 2004-11-30 | 2007-10-24 | 日本宇宙能源株式会社 | Process for producing polycrystalline silicon bar |
| CN200957306Y (en) * | 2006-10-09 | 2007-10-10 | 张和清 | Pallet for microwave closed extractor |
| CN1962435A (en) * | 2006-10-31 | 2007-05-16 | 锦州新世纪石英玻璃有限公司 | Production process of solar energy grade polysilicon |
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