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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Abstract
The implementation mode in the invention provides a purity detecting method and a device for polysilicon, which belongs to the fields of chemical industry and solar energy. The method comprises the following steps: after evenly mixing silicon powder, washing with secondary deionized water, and drying to constant weight; putting the dried silicon powder on a Teflon tray, adding water to moisturize the sample, and adding a polyol solution; putting the Teflon tray on a Teflon container, putting the Teflon container in a seal body, adding HF and HNO3 into the lower part of the seal body, sealing the seal body, and heating to 110-120 DEG C; and after the silicon powder is completely dissolved and volatilized to the dry state, adding HNO3 to dissolve residues, transferring to a plastic volumetric flask, and measuring the content of impurity elements after the volume becomes constant. The specific implementation mode in the invention also provides a special device for realizing the purity detecting method for polysilicon. The method and the 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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| Application Number | Priority Date | Filing Date | Title |
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| CN200810223000A CN101685048B (en) | 2008-09-25 | 2008-09-25 | Purity detecting method and device for polysilicon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 | Quartz purification method suitable for rock or sand sample with different mineral compositions |
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 |
| 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 |
-
2008
- 2008-09-25 CN CN200810223000A patent/CN101685048B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| Title |
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| 张琪 等.高压密闭消解_原子吸收光度法同时测定土壤中的铜_锌_铅_镉_镍_铬.《化学分析剂量》.2007,第16卷(第5期),48-50. * |
| 杜萍 等.密闭微波消解技术概述.《中国卫生检验杂志》.2008,第18卷(第8期),1701-1703. * |
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