CN105239163A - Polysilicon surface metal impurity content control method - Google Patents
Polysilicon surface metal impurity content control method Download PDFInfo
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- CN105239163A CN105239163A CN201510600414.2A CN201510600414A CN105239163A CN 105239163 A CN105239163 A CN 105239163A CN 201510600414 A CN201510600414 A CN 201510600414A CN 105239163 A CN105239163 A CN 105239163A
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- polycrystalline silicon
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Abstract
The invention discloses a polysilicon surface metal impurity content control method. The method comprises the following steps: 1, wrapping a cooled polysilicon product; 2, crushing the wrapped polysilicon product by using a breaking hammer, wherein the quality of the crushing hammer is controlled, an operation personnel wears sweat absorbing gloves, and the sweat absorbing gloves are sleeved with anti-cutting gloves; and 3, analyzing the metal content data of the surface of the crushed polysilicon product, and replacing or restoring the crushing hammer, the sweat absorbing gloves and the anti-cutting gloves when the surface metal content exceeds a standard. The polysilicon surface metal impurity content control method has the advantages of simple operation and low cost.
Description
Technical field
The present invention relates to polysilicon processing technique field, be specifically related to a kind of control method of metallic contaminants from surface of polycrystalline silicon content.
Background technology
The polysilicon product that polycrystalline silicon producing device is produced, from assembly of reduction furnace out after, in thousand Ji Huowanji clean rooms, adopt Mechanical Crushing or hand breaking, silicon rod is broken into bar-shaped, block, granular product, metal is had in this process, nonmetal, house dust contacts with polysilicon product, if do not controlled polysilicon surface cleanliness factor, the phenomenon of secondary pollution can be there is, directly affect monocrystal pulling, the minority carrier life time of the crystal block after ingot casting, have influence on the efficiency of conversion of cell piece further, assembly is caused to decay seriously in power generation process, affect generated energy, polycrystalline silicon material purity requirement needed for sun power industry is more than 99.9999%, that is, except this element of Si, and the minimizing that other element should be possible.
The source of other elements is mainly the material producing polysilicon product, and we are referred to as the in-vivo metal impurity of polycrystalline silicon material.Other elements of external environment fall into polysilicon surface, and we are referred to as the metallic contaminants from surface of polycrystalline silicon material.In-vivo metal impurity source is raw material silica flour, material pipe etc., and removed by other elements by rectificating method, but cannot remove completely, can only reduce as much as possible, main B, P, its content is the ppta order of magnitude.And metallic contaminants from surface source is environment, personnel, auxiliary material, mainly occur in the storage of silicon material, fragmentation, packaging link.The current whole world, the breaking method of silicon material has mechanical automatic crusher, artificial hand-crushed, due to machine automatization crusher costly, master is broken for by hand with artificial at present so domestic, the method of control surface metals content impurity general in industry carries out fragmentation for using wolfram varbide quartering hammer, prevents the metal impurity con polysilicon product surfaces such as Fe, Cu of quartering hammer.But because silicon rod density is comparatively large, quartering hammer is very easy to damage, and causes wolfram varbide position impaired.
In current reduction shattering process, the method for polysilicon surface metal content is generally: mode quartering hammer being damaged to less employing reparation carries out repairing quartering hammer; Quartering hammer damages the larger quartering hammer more renewed; Control the putting position of wolfram varbide quartering hammer: quartering hammer only has part for tungsten carbide material, other positions are stainless steel, wherein Fe content is very high, the analysis found that, in the metals content impurity on polysilicon product surface, Fe element is main source of pollution, after breaking, quartering hammer be put outside breaking tank, in order to avoid non-wolfram varbide position pollutes polysilicon product surface.Metallic contaminants from surface of polycrystalline silicon content is very easily increased in artificial charging, quantitative weighing process.General way in industry prevents personnel's hand to be scraped off, and personnel directly contact silicon material after wearing anti-cutting gloves, very easily increase metallic contaminants from surface of polycrystalline silicon content in this process.Or outside anti-cutting gloves, wear one deck pvc gloves again.
For the impact of the metal content on polysilicon product surface, bibliographical information is not had for concrete metallic element source and quartering hammer etc. thereof and crosses corresponding detection and management-control method.
Metallic contaminants from surface of polycrystalline silicon mainly comprises Na, Mg, Al, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Mo, W, Pb, amounts to 16 kinds of elements.After finding the source of element, then link removes control surface metallic impurity one by one, seems particularly important.
Summary of the invention
In view of this, the embodiment of the present invention provides the control method of metallic contaminants from surface of polycrystalline silicon content, can greatly reduce polycrystalline silicon material surface metal levels, have simple to operate, the advantage that cost is low.
A control method for metallic contaminants from surface of polycrystalline silicon content, is characterized in that, comprises the steps:
(1) polysilicon product after cooling is wrapped up;
(2) polysilicon product after parcel is broken with quartering hammer, the quality of quartering hammer described in management and control; Operator wear sweat-absorbing glove, and described sweat-absorbing glove also overlaps outward anti-cutting gloves;
(3) analyze the polysilicon product surface metal levels data after fragmentation, carry out replacing or the reparation of described quartering hammer, sweat-absorbing glove and anti-cutting gloves when described surface metal levels exceeds standard.
Further, the quality of described management and control quartering hammer specifically comprises the steps:
In polycrystalline silicon material shattering process, find that described quartering hammer damages repair immediately, at interval of 1h, described quartering hammer is checked, carry out repairing or changing if any breakage.
Further, the replacing construction≤1h of described sweat-absorbing glove.
Further, purging is carried out to described anti-cutting gloves outside surface and removes its metallic contaminants from surface, described purging the timed interval≤20min.
Further, described sweat-absorbing glove is textile material.
Further, described anti-cutting gloves also overlaps outward PVC glove.
Further, the replacing construction≤10min of described PVC glove.
Compared with prior art, the control method of metallic contaminants from surface of polycrystalline silicon content of the present invention has following beneficial effect:
In industry in prior art, the method for personnel's wearing gloves is, the first layer is anti-cutting gloves, and the second layer is PVC glove; Or directly just wear one deck anti-cutting gloves.In art methods, due to human hand easily perspire, unclean etc. larger to the pollution of polycrystalline silicon material, and operator's wearing gloves is three layers of gloves in the present patent application, namely in anti-cutting gloves, added sweat-absorbing glove, the metal content that can prevent sweat from causing like this increases.
The breaking tool used in industry is wolfram varbide quartering hammer, but quartering hammer in use can sustain damage, cause some the element pollution polycrystalline silicon material in the material of quartering hammer, Fe, W, Co element in polycrystalline silicon material metallic contaminants from surface content is caused to increase, by the real-time management and control to quartering hammer in the inventive method, can greatly reduce polysilicon product surface metal levels.
By carrying out data analysis to the polysilicon surface metal content after fragmentation, can guarantee that polysilicon surface metal content can not exceed standard.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but not as a limitation of the invention.
Embodiment 1
By carrying out metal content analysis to sweat and quartering hammer and the instrument that touches thereof, there are seven kinds of elements such as Na, Mg, Al, K, Ca, Fe, Zn in personnel; What derive from instrument (being mainly quartering hammer) has Mg, Al, K, Fe, Zn, Ti, Cr, Mn, Co, Ni, Cu, Zn, Mo, W, Pb.
Get appropriate silico briquette to rub on the wolfram varbide hammer surface of breakage, then friction 5-10min adopts instrument ICP-MS to analyze, by analysis, find that the metals content impurity value that element W, Co content on silico briquette surface exceedes normal silico briquette surface reaches tens times to hundred times, analyze through six groups of parallel tests, finally determine that damaged wolfram varbide hammer can increase polysilicon product metallic contaminants from surface content really.Through six groups of mensuration, the quartering hammer that analysis is damaged and unbroken quartering hammer are on the impact of polysilicon surface metal content, and table 1 is polysilicon surface metallic element contrast table, and quartering hammer is as shown in table 1 with or without the content influence of breakage to polysilicon surface W and Co element.
Table 1 polysilicon surface metallic element contrast table
Can find that the damage of quartering hammer increases greatly by making W and the Co content of polysilicon surface by table 1.
Analyzed by the sweat to people, PVC glove surface and polysilicon surface metal content, find that seven kinds of elements such as Na, Mg, Al, K, Ca, Fe, Zn of polysilicon surface are mainly derived from the sweat of staff;
The metal element content on polysilicon product surface is controlled by the quality of management and control quartering hammer, the quality concrete steps of management and control quartering hammer are: find the quartering hammer repaired immediately or more renew that quartering hammer damages, the ultimate analysis of metallic contaminants from surface content is carried out according to instrument, the quality of timely management and control quartering hammer, the quality of controlled fragmentation hammer, run into damaged reparation in time or replacing, W, Co metallic element in silicon material metallic contaminants from surface can be reduced.
Prevent sweat from controlling polysilicon product surface metal levels by the control of staff's wearing gloves: during employee's wearing gloves, the first layer wears sweat-absorbing glove; The second layer wears anti-cutting gloves; Third layer wears pvc gloves.Sweat-absorbing glove changes twice every day, runs into the damaged sweat-absorbing glove more renewed in time, and anti-cutting gloves breakage also needs the gloves more renewed, and pvc gloves need to change once every 10min.Table 2 is polysilicon product surface main metal element content balance table, the polysilicon surface main metal element content balance that the inventive method and existing breaking method obtain is as shown in table 2, wherein numbering 1-7 is the polysilicon product surface metal levels data that existing method obtains, and numbering 8-13 is the polysilicon surface metal content data that the inventive method obtains.
Wherein, the metallic element of following nucleidic mass is detected: Na:22.99, Mg:23.99, Al:26.98, K:38.96, Ca:39.96, Fe:55.93, Co:58.93, Zn:93.93, W:183.95.
Table 2 polysilicon product surface main metal element content balance table
This programme finds through analysis of experiments, and metallic contaminants from surface of polycrystalline silicon Na element, Ca element, be mainly derived from sweat, in gloves, in air.Na element source is in sweat on hand, wear the first layer sweat-absorbing glove, most Na element can be filtered out, and second layer anti-cutting gloves does not possess perspiration removing function, therefore third layer pvc gloves are worn, the damaged degree of third layer pvc gloves must be controlled, prevent Na element from polluting polysilicon product surface further by damaged pvc gloves.And Ca element also derives from pvc gloves, because personnel understand other article in exposure chamber unavoidably wearing pvc gloves, as article such as the PE bag outside of quartering hammer handle, packaging polycrystalline product, broken frids, the Ca element in gloves is caused to increase, pollution polysilicon product surface, the mode of the cleanliness factor and damaged degree that therefore control third layer PVC glove is: once glove surface blackout or damaged, personnel need change immediately, prevents Ca element pollution polysilicon product surface.The first layer is that sweat-absorbing glove can by Na, Ca metallic element in silicon material metallic contaminants from surface; Wear third layer pvc gloves can reduce Mg, Al, Zn, karat gold in silicon material metallic contaminants from surface and belong to element; If do not worn third layer pvc gloves, but by cleaning, purging second layer anti-cutting gloves, also can control Mg, Al, Zn, K element in silicon material metallic contaminants from surface, but not wear the effective of third layer pvc gloves.
Embodiment 2
Be that we are in the process controlled with the difference of embodiment 1, adopt the method for third layer pvc gloves of not wearing, and by constantly cleaning, the method purging second layer anti-cutting gloves, also can control surface metals content impurity; Every 20min purges an anti-cutting gloves, changes an anti-cutting gloves, clean every 1 hour.
Embodiment 3
A control method for metallic contaminants from surface of polycrystalline silicon content, comprises the steps:
(1) after polysilicon product production terminates, in assembly of reduction furnace, after temperature is reduced to certain temperature, by operator, PE bag is enclosed within polycrystalline silicon rod surface, then with a large cloth bag, every a pair product is wrapped up, with driving, every a pair silicon rod is sling, put into dolly, also have now and directly adopt mechanical manipulator, after directly exposed polycrystalline silicon rod being clamped, unload, put into dolly;
(2) polysilicon product after parcel is broken with quartering hammer, in polycrystalline silicon material shattering process, find that described quartering hammer damages repair immediately, at interval of 1h, described quartering hammer is checked, carry out repairing or changing if any breakage; Operator wear textile material sweat-absorbing glove, and described sweat-absorbing glove also overlaps outward anti-cutting gloves; Replacing construction≤the 1h of described sweat-absorbing glove, carries out purging to described anti-cutting gloves outside surface and removes its metallic contaminants from surface, described purging the timed interval≤20min;
(3) analyze the polysilicon product surface metal levels data after fragmentation, carry out replacing or the reparation of described quartering hammer and gloves when described surface metal levels exceeds standard; Data analysing method operates according to GBT24582-2009.
Carry out surface metal levels analysis to the polycrystalline silicon material that above-mentioned control program obtains, its metal content all meets the standard entered silicon materials more at present and use,
Above embodiment is only exemplary embodiment of the present invention, and be not used in restriction the present invention, protection scope of the present invention is defined by the claims.Those skilled in the art can in essence of the present invention and protection domain, and make various amendment or equivalent replacement to the present invention, this amendment or equivalent replacement also should be considered as dropping in protection scope of the present invention.
Claims (7)
1. a control method for metallic contaminants from surface of polycrystalline silicon content, is characterized in that, comprises the steps:
(1) polysilicon product after cooling is wrapped up;
(2) polysilicon product after parcel is broken with quartering hammer, the quality of quartering hammer described in management and control; Operator wear sweat-absorbing glove, and described sweat-absorbing glove also overlaps outward anti-cutting gloves;
(3) analyze the polysilicon product surface metal levels data after fragmentation, carry out replacing or the reparation of described quartering hammer, sweat-absorbing glove and anti-cutting gloves when described surface metal levels exceeds standard.
2. the control method of metallic contaminants from surface of polycrystalline silicon content according to claim 1, is characterized in that, the quality of described management and control quartering hammer specifically comprises the steps:
In polycrystalline silicon material shattering process, find that described quartering hammer damages repair immediately, at interval of 1h, described quartering hammer is checked, carry out repairing or changing if any breakage.
3. the control method of metallic contaminants from surface of polycrystalline silicon content according to claim 1, is characterized in that, the replacing construction≤1h of described sweat-absorbing glove.
4. the control method of metallic contaminants from surface of polycrystalline silicon content according to claim 1, is characterized in that, carries out purging remove its metallic contaminants from surface to described anti-cutting gloves outside surface, described purging the timed interval≤20min.
5. the control method of metallic contaminants from surface of polycrystalline silicon content according to claim 1, is characterized in that, described sweat-absorbing glove is textile material.
6. the control method of metallic contaminants from surface of polycrystalline silicon content according to claim 1, is characterized in that, described anti-cutting gloves also overlaps outward PVC glove.
7. the control method of metallic contaminants from surface of polycrystalline silicon content according to claim 6, is characterized in that, the replacing construction≤10min of described PVC glove.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106076460A (en) * | 2016-06-15 | 2016-11-09 | 亚洲硅业（青海）有限公司 | A kind of device processing polycrystalline silicon rod and using method thereof |
| CN110124837A (en) * | 2019-05-17 | 2019-08-16 | 西安奕斯伟硅片技术有限公司 | A kind of breaking method and annealing device of silicon crystal |
| CN110940721A (en) * | 2019-12-20 | 2020-03-31 | 内蒙古通威高纯晶硅有限公司 | Method for measuring metal impurities on surface of crushing tool |
| CN115445704A (en) * | 2022-09-22 | 2022-12-09 | 新特能源股份有限公司 | Metal treatment method of polycrystalline silicon crushing and screening system |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH106242A (en) * | 1996-06-25 | 1998-01-13 | Tokuyama Corp | Hammer |
| CN101376242A (en) * | 2007-08-27 | 2009-03-04 | 三菱麻铁里亚尔株式会社 | Hammer for breaking polycrystalline silicon |
| CN101495682A (en) * | 2006-07-28 | 2009-07-29 | 瓦克化学股份公司 | Method and device for producing classified high-purity polycrystalline silicon fragments |
| CN101623672A (en) * | 2008-11-26 | 2010-01-13 | 江西赛维Ldk太阳能高科技有限公司 | Method for sorting silicon material mixed with impurities |
| CN102001663A (en) * | 2010-12-10 | 2011-04-06 | 云南乾元光能产业有限公司 | Method for removing impurities on surface of metal silicon |
| CN102152411A (en) * | 2010-12-31 | 2011-08-17 | 常州天合光能有限公司 | Method for reducing impurity ratio of polycrystalline ingot |
| CN102320608A (en) * | 2011-07-14 | 2012-01-18 | 西安华晶电子技术股份有限公司 | A kind of silicon material is purified and is produced with crystal fracture device and breaking method thereof |
| CN102862989A (en) * | 2012-10-11 | 2013-01-09 | 包头市山晟新能源有限责任公司 | Pretreatment method for purifying polycrystalline silicon by metallurgic method |
| CN103204279A (en) * | 2013-04-02 | 2013-07-17 | 新特能源股份有限公司 | Polysilicon breaking and packaging line and polysilicon broken packaging method |
| CN103418459A (en) * | 2013-08-30 | 2013-12-04 | 昆山奥德鲁自动化技术有限公司 | Crushing device |
| CN103570021A (en) * | 2012-08-06 | 2014-02-12 | 瓦克化学股份公司 | Polycrystalline silicon chunks and method for producing them |
| CN104150055A (en) * | 2014-07-31 | 2014-11-19 | 中国恩菲工程技术有限公司 | Automatic polycrystalline silicon crushing and packaging equipment |
-
2015
- 2015-09-21 CN CN201510600414.2A patent/CN105239163A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH106242A (en) * | 1996-06-25 | 1998-01-13 | Tokuyama Corp | Hammer |
| CN101495682A (en) * | 2006-07-28 | 2009-07-29 | 瓦克化学股份公司 | Method and device for producing classified high-purity polycrystalline silicon fragments |
| CN101376242A (en) * | 2007-08-27 | 2009-03-04 | 三菱麻铁里亚尔株式会社 | Hammer for breaking polycrystalline silicon |
| CN101623672A (en) * | 2008-11-26 | 2010-01-13 | 江西赛维Ldk太阳能高科技有限公司 | Method for sorting silicon material mixed with impurities |
| CN102001663A (en) * | 2010-12-10 | 2011-04-06 | 云南乾元光能产业有限公司 | Method for removing impurities on surface of metal silicon |
| CN102152411A (en) * | 2010-12-31 | 2011-08-17 | 常州天合光能有限公司 | Method for reducing impurity ratio of polycrystalline ingot |
| CN102320608A (en) * | 2011-07-14 | 2012-01-18 | 西安华晶电子技术股份有限公司 | A kind of silicon material is purified and is produced with crystal fracture device and breaking method thereof |
| CN103570021A (en) * | 2012-08-06 | 2014-02-12 | 瓦克化学股份公司 | Polycrystalline silicon chunks and method for producing them |
| CN102862989A (en) * | 2012-10-11 | 2013-01-09 | 包头市山晟新能源有限责任公司 | Pretreatment method for purifying polycrystalline silicon by metallurgic method |
| CN103204279A (en) * | 2013-04-02 | 2013-07-17 | 新特能源股份有限公司 | Polysilicon breaking and packaging line and polysilicon broken packaging method |
| CN103418459A (en) * | 2013-08-30 | 2013-12-04 | 昆山奥德鲁自动化技术有限公司 | Crushing device |
| CN104150055A (en) * | 2014-07-31 | 2014-11-19 | 中国恩菲工程技术有限公司 | Automatic polycrystalline silicon crushing and packaging equipment |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106076460A (en) * | 2016-06-15 | 2016-11-09 | 亚洲硅业（青海）有限公司 | A kind of device processing polycrystalline silicon rod and using method thereof |
| CN106076460B (en) * | 2016-06-15 | 2018-04-13 | 亚洲硅业（青海）有限公司 | A kind of device and its application method for handling polycrystalline silicon rod |
| CN110124837A (en) * | 2019-05-17 | 2019-08-16 | 西安奕斯伟硅片技术有限公司 | A kind of breaking method and annealing device of silicon crystal |
| CN110940721A (en) * | 2019-12-20 | 2020-03-31 | 内蒙古通威高纯晶硅有限公司 | Method for measuring metal impurities on surface of crushing tool |
| CN115445704A (en) * | 2022-09-22 | 2022-12-09 | 新特能源股份有限公司 | Metal treatment method of polycrystalline silicon crushing and screening system |
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