CN107572533A - The minimizing technology of impurity in a kind of silicon material flaw-piece - Google Patents
The minimizing technology of impurity in a kind of silicon material flaw-piece Download PDFInfo
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- CN107572533A CN107572533A CN201710800457.4A CN201710800457A CN107572533A CN 107572533 A CN107572533 A CN 107572533A CN 201710800457 A CN201710800457 A CN 201710800457A CN 107572533 A CN107572533 A CN 107572533A
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Abstract
This application discloses a kind of minimizing technology of impurity in silicon material flaw-piece, including：Silicon material flaw-piece is positioned in corrosive liquid and soaks preset time, removes the impurity on the silicon material flaw-piece surface, and embedded impurity is exposed to surface；The embedded impurity exposed to the silicon material flaw-piece surface is scrubbed off, using silicon material flaw-piece described in pure water rinsing in neutrality；The silicon material flaw-piece is carried out corroding cleaning and reuses pure water rinsing in neutrality；The silicon material flaw-piece is cleaned by ultrasonic and dried.The minimizing technology of impurity in above-mentioned silicon material flaw-piece, the impurity embedded in silicon material flaw-piece can be preferably removed, improve the quality of subsequent product.
Description
Technical field
The invention belongs to technical field of solar batteries, more particularly to a kind of minimizing technology of impurity in silicon material flaw-piece.
Background technology
Due to the influence of polycrystalline silicon raw material and ingot casting environment, some impurity are produced during polycrystalline silicon ingot casting, are such as carbonized
Silicon impurities or silicon nitride inclusions, this kind of impurity are gathered in silicon ingot upper and lower surface and surrounding, silicon in the presence of directional solidification impurities removal
Ingot by evolution, go end to end after can produce largely contain above-mentioned impurity edge skin material, this part silicon material is due to impurity content mistake
It is more, it is impossible to directly melt down, and impurity is embedded in polycrystalline silicon ingot casting edge skin material, the impurity of current polycrystal silicon ingot edge skin material is gone
Except method, pickling or alkali cleaning mode typically are used, i.e., by nitric/hydrofluoric or concentrated base under the high temperature conditions to silico briquette surface
Corroded so that impurities on surface of silicon chip comes off from silico briquette matrix.Using the above method, for the polycrystal silicon ingot that surface is impure
Edge skin material can play preferable impurity elimination effect, but for embedding the polysilicon edge skin material of solid impurity, removal effect is not
Good, this just influences the quality of subsequent product.
The content of the invention
To solve the above problems, the invention provides a kind of minimizing technology of impurity in silicon material flaw-piece, can preferably go
Except the impurity embedded in silicon material flaw-piece, the quality of subsequent product is improved.
The minimizing technology of impurity in a kind of silicon material flaw-piece provided by the invention, including：
Silicon material flaw-piece is positioned in corrosive liquid and soaks preset time, removes the impurity on the silicon material flaw-piece surface, and will
Embedded impurity is exposed to surface；
The embedded impurity exposed to the silicon material flaw-piece surface is scrubbed off, using silicon material flaw-piece described in pure water rinsing into being in
Property；
The silicon material flaw-piece is carried out corroding cleaning and reuses pure water rinsing in neutrality；
The silicon material flaw-piece is cleaned by ultrasonic and dried.
Preferably, it is described to scrub off exposed to the silicon material flaw-piece in above-mentioned silicon material flaw-piece in the minimizing technology of impurity
The embedded impurity on surface, using silicon material flaw-piece described in pure water rinsing to after in neutrality, in addition to：
Sandblasting is carried out to the silicon material flaw-piece, removes the embedded impurity for remaining in the silicon material flaw-piece surface.
Preferably, it is described that silicon material flaw-piece is positioned in corrosive liquid in above-mentioned silicon material flaw-piece in the minimizing technology of impurity
Soaking preset time is：
Silicon material flaw-piece is positioned in acid corrosion liquid or caustic corrosion liquid and soaks preset time.
Preferably, it is described to scrub off exposed to the silicon material flaw-piece in above-mentioned silicon material flaw-piece in the minimizing technology of impurity
The embedded impurity on surface is：
The embedded impurity exposed to the silicon material flaw-piece surface is scrubbed off using brush.
Preferably, it is described that the silicon material flaw-piece corrode clearly in above-mentioned silicon material flaw-piece in the minimizing technology of impurity
Wash for：
It is 1 using volume range:7 to 1:10 hydrofluoric acid and nitric acid carries out corrosion cleaning to the silicon material flaw-piece.
Preferably, it is described that ultrasound is carried out to the silicon material flaw-piece clearly in above-mentioned silicon material flaw-piece in the minimizing technology of impurity
Wash for：
The silicon material flaw-piece be cleaned by ultrasonic 40 minutes to 60 minutes.
Preferably, it is described drying is carried out to the silicon material flaw-piece to be in above-mentioned silicon material flaw-piece in the minimizing technology of impurity：
Drying is carried out to the silicon material flaw-piece and continues 50 minutes to 80 minutes.
By foregoing description, the minimizing technology of impurity in above-mentioned silicon material flaw-piece provided by the invention, due to including inciting somebody to action
Silicon material flaw-piece, which is positioned in corrosive liquid, soaks preset time, removes the impurity on the silicon material flaw-piece surface, and embedded impurity is sudden and violent
It is exposed at surface；The embedded impurity exposed to the silicon material flaw-piece surface is scrubbed off, using silicon material flaw-piece described in pure water rinsing to being in
It is neutral；The silicon material flaw-piece is carried out corroding cleaning and reuses pure water rinsing in neutrality；The silicon material flaw-piece is carried out
It is cleaned by ultrasonic and drying, the process of this immersion can be removed preferably in silicon material flaw-piece than cleaning process of the prior art
Embedded impurity, improve the quality of subsequent product.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
The embodiment of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
The accompanying drawing of offer obtains other accompanying drawings.
Fig. 1 is the schematic diagram of the minimizing technology of impurity in the first silicon material flaw-piece that the embodiment of the present application provides.
Embodiment
The core concept of the present invention can preferably remove silicon in a kind of minimizing technology of the impurity in silicon material flaw-piece is provided
Expect the impurity embedded in flaw-piece, improve the quality of subsequent product.
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
The minimizing technology of impurity is as shown in figure 1, Fig. 1 is the application in the first silicon material flaw-piece that the embodiment of the present application provides
The schematic diagram of the minimizing technology of impurity, this method comprise the following steps in the first silicon material flaw-piece that embodiment provides：
S1：Silicon material flaw-piece is positioned in corrosive liquid and soaks preset time, removes the impurity on the silicon material flaw-piece surface, and
Embedded impurity is exposed to surface；
Referred to herein as impurity include but is not limited to carborundum, silicon nitride and metal impurities, in the prior art for surface
Impure polycrystal silicon ingot edge skin material be using nitration mixture (hydrofluoric acid and nitric acid) directly cleaning 30s to 45s after cross pure water, ultrasound and
Drying, it can play preferable impurity elimination effect, but for embedding the polysilicon edge skin material of solid impurity, can not be located
Reason, so as to cause the waste of such resource, and in the step of the application, the mode soaked using corrosive liquid is impure to surface
Polycrystal silicon ingot edge skin material corroded so that embedded impurity is exposed from polycrystal silicon ingot edge skin material surface, plus follow-up step
It is rapid just to reach the effect for removing impurity.
S2：The embedded impurity exposed to the silicon material flaw-piece surface is scrubbed off, using silicon material flaw-piece described in pure water rinsing extremely
In neutrality；
It should be noted that some embedded impurity exposed can be removed by way of scrub, and another portion
Dividing can not then remove, then needs to be removed using subsequent step.
S3：The silicon material flaw-piece is carried out corroding cleaning and reuses pure water rinsing in neutrality；
Cleaned specifically, silicon material in the gaily decorated basket is put into the nitration mixture prepared, the scavenging period 40-60 seconds；Will cleaning
Good material takes to be suspended on liquid level from nitration mixture drips acid, drips the sour time 2-3 seconds；Material is immediately placed in water and used after acid will be dripped in the gaily decorated basket
The cold water flush acid solution 10-35 seconds；Material is put into overflow tank and rinsed after water is rinsed, and material is put into ultrasound after having rinsed
On area's loading bay.
S4：The silicon material flaw-piece is cleaned by ultrasonic and dried.
Specifically, ultrasonic procedure utilizes cavitation, acceleration effect and the direct flow effect pair of ultrasonic wave in a liquid
Liquid and dirt carry out direct or indirect effect, crud layer is disperseed, emulsified, is peeled off and reach cleaning purpose.The ultrasound
Step includes：Pure water is piled into ultrasonic pond, material screen cloth will be poured into the charging aperture gaily decorated basket and place into ultrasonic pond, it is ensured that pure water is by silicon
Material submergence, and keep pure water spillway discharge 2.75-3.25L/min in ultrasonic procedure；After material is well placed, ultrasonic device switch is pressed
Start ultrasound, and the ultrasonic device duration is set；The good silicon material of ultrasound is taken out from ultrasonic pond.
Drying course therein preheats including baking oven, first opens oven equipment and is preheated, the baking car for installing material is pushed away
Enter and drying operation is carried out in baking oven, and material batch number is recorded on baking oven record sheet, set suitable drying time, so
Confirm that material has been dried in the gaily decorated basket afterwards, then discharge, extend drying time if not drying, extending the time can be actual according to material scene
Situation is determined, the material dried is pulled out from baking oven, is positioned on drying channel and cools down；Baking car equipped with silicon material is pushed away
Enter by dust-free workshop sorting table, then silicon material networking cloth in the gaily decorated basket is put into sorting table together；It is comprehensive to the silicon material on sorting table
Check surface of material outward appearance, it is abnormal to pick out dirty, oxidation, rubbish etc., it is hidden split, crack need to be knocked open, confirm whether have in crack
It is dirty；Sorting qualified material is loaded and is cased with watt gram bucket of free-bag or dustless inframe, weighs and tightens sack with band；Confirm
Unqualified material moves back front end process and handled again, and anomalies charge, weight etc. are remembered on pickling data logger in dustless move back
Abnormal information.
The minimizing technology of impurity in the first the silicon material flaw-piece provided by foregoing description, the embodiment of the present application, by
In soaking preset time including silicon material flaw-piece is positioned in corrosive liquid, the impurity on the silicon material flaw-piece surface is removed, and by
Embedding impurity is exposed to surface；The embedded impurity exposed to the silicon material flaw-piece surface is scrubbed off, utilizes silicon material described in pure water rinsing
Flaw-piece is in neutrality；The silicon material flaw-piece is carried out corroding cleaning and reuses pure water rinsing in neutrality；To the silicon material
Flaw-piece is cleaned by ultrasonic and dried, and the process of this immersion can preferably remove silicon than cleaning process of the prior art
Expect the impurity embedded in flaw-piece, improve the quality of subsequent product.
The minimizing technology of impurity, is on the first above-mentioned silicon material side in second of silicon material flaw-piece that the embodiment of the present application provides
In skin on the basis of the minimizing technology of impurity, in addition to following technical characteristic：
It is described to scrub off the embedded impurity exposed to the silicon material flaw-piece surface, using silicon material flaw-piece described in pure water rinsing extremely
After neutrality, in addition to：
Sandblasting is carried out to the silicon material flaw-piece, removes the embedded impurity for remaining in the silicon material flaw-piece surface.
Specifically, can by the sand-blasting machine sandblasting of the polycrystalline silicon material after flushing, by one layer of impurity on surface peel off with up to
To the purpose for removing embedded impurity.
The minimizing technology of impurity, is on the first above-mentioned silicon material side in the third silicon material flaw-piece that the embodiment of the present application provides
In skin on the basis of the minimizing technology of impurity, in addition to following technical characteristic：
It is described by silicon material flaw-piece be positioned in corrosive liquid soak preset time be：
Silicon material flaw-piece is positioned in acid corrosion liquid or caustic corrosion liquid and soaks preset time.
Specifically, acid corrosion liquid can be hydrofluoric acid+nitric acid or hydrofluoric acid+hydrochloric acid, the time range of immersion is chosen as
10-20 minutes, caustic corrosion liquid can be the solution of the main group of sodium hydroxide, potassium hydroxide etc. first, and the time range of immersion is optional
For 6-12 hours.
The minimizing technology of impurity, is on the first above-mentioned silicon material side in the 4th kind of silicon material flaw-piece that the embodiment of the present application provides
In skin on the basis of the minimizing technology of impurity, in addition to following technical characteristic：
The embedded impurity that scrubs off exposed to the silicon material flaw-piece surface is：
The embedded impurity exposed to the silicon material flaw-piece surface is scrubbed off using brush.
It should be noted that brush is a kind of conventional scrubbing tool, it is easily obtained and cost is relatively low, certainly here also simultaneously
It is not construed as limiting, can also be scrubbed using other kinds of instrument, as long as removal that can be strong embeds impurity.
The minimizing technology of impurity, is on the first above-mentioned silicon material side in the 5th kind of silicon material flaw-piece that the embodiment of the present application provides
In skin on the basis of the minimizing technology of impurity, in addition to following technical characteristic：
It is described to the silicon material flaw-piece carry out corrode cleaning be：
It is 1 using volume range:7 to 1:10 hydrofluoric acid and nitric acid carries out corrosion cleaning to the silicon material flaw-piece.
Specifically, first adding nitric acid 50kg (2 barrels of 35L) into acid tank, then fluoric acid 3.5-5L is hydrogenated with into acid tank with measuring cup, mixed
Sour configuration proportion is acid solution volume ratio, hydrofluoric acid：Nitric acid=1:7-1:10.
The minimizing technology of impurity, is on the first above-mentioned silicon material side in the 6th kind of silicon material flaw-piece that the embodiment of the present application provides
In skin on the basis of the minimizing technology of impurity, in addition to following technical characteristic：
It is described ultrasonic cleaning is carried out to the silicon material flaw-piece to be：
The silicon material flaw-piece be cleaned by ultrasonic 40 minutes to 60 minutes.
Specifically, be cleaned by ultrasonic substantially can remove embedded impurity totally for 40 minutes to 60 minutes, certainly can be with root
Factually the cleaning performance on border extends or shortens the time, is not intended to limit herein.
The minimizing technology of impurity in the 7th kind of silicon material flaw-piece that the embodiment of the present application provides, be it is above-mentioned the first to the 6th
In kind of silicon material flaw-piece it is any in the minimizing technology of impurity on the basis of, in addition to following technical characteristic：
It is described drying is carried out to the silicon material flaw-piece to be：
Drying is carried out to the silicon material flaw-piece and continues 50 minutes to 80 minutes.
It should be noted that the drying course of this time range is generally possible to all remove the moisture of silicon material flaw-piece, protect
Card does not have a negative impact, and can also extend or shorten as the case may be certainly this drying time, be not intended to limit herein.
In summary, the method provided using the application, can remove the impurity being embedded in polycrystalline silicon ingot casting edge skin material,
Processing method is simple, easy to operate, and raw material availability improves, and cost is low.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (7)
- A kind of 1. minimizing technology of impurity in silicon material flaw-piece, it is characterised in that including：Silicon material flaw-piece is positioned in corrosive liquid and soaks preset time, removes the impurity on the silicon material flaw-piece surface, and will be embedded Impurity is exposed to surface；The embedded impurity exposed to the silicon material flaw-piece surface is scrubbed off, using silicon material flaw-piece described in pure water rinsing in neutrality；The silicon material flaw-piece is carried out corroding cleaning and reuses pure water rinsing in neutrality；The silicon material flaw-piece is cleaned by ultrasonic and dried.
- 2. the minimizing technology of impurity in silicon material flaw-piece according to claim 1, it is characterised in that described scrub off is exposed to The embedded impurity on the silicon material flaw-piece surface, using silicon material flaw-piece described in pure water rinsing to after in neutrality, in addition to：Sandblasting is carried out to the silicon material flaw-piece, removes the embedded impurity for remaining in the silicon material flaw-piece surface.
- 3. the minimizing technology of impurity in silicon material flaw-piece according to claim 1, it is characterised in that described to put silicon material flaw-piece Being placed in immersion preset time in corrosive liquid is：Silicon material flaw-piece is positioned in acid corrosion liquid or caustic corrosion liquid and soaks preset time.
- 4. the minimizing technology of impurity in silicon material flaw-piece according to claim 1, it is characterised in that described scrub off is exposed to The embedded impurity on the silicon material flaw-piece surface is：The embedded impurity exposed to the silicon material flaw-piece surface is scrubbed off using brush.
- 5. the minimizing technology of impurity in silicon material flaw-piece according to claim 1, it is characterised in thatIt is described to the silicon material flaw-piece carry out corrode cleaning be：It is 1 using volume range:7 to 1:10 hydrofluoric acid and nitric acid carries out corrosion cleaning to the silicon material flaw-piece.
- 6. the minimizing technology of impurity in silicon material flaw-piece according to claim 1, it is characterised in thatIt is described ultrasonic cleaning is carried out to the silicon material flaw-piece to be：The silicon material flaw-piece be cleaned by ultrasonic 40 minutes to 60 minutes.
- 7. the minimizing technology of impurity in the silicon material flaw-piece according to claim any one of 1-6, it is characterised in thatIt is described drying is carried out to the silicon material flaw-piece to be：Drying is carried out to the silicon material flaw-piece and continues 50 minutes to 80 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114127011A (en) * | 2019-08-29 | 2022-03-01 | 瓦克化学股份公司 | Method for producing silicon blocks |
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| WO2012002665A2 (en) * | 2010-07-01 | 2012-01-05 | 연세대학교 산학협력단 | Method for removing impurities from mg-si using acid leaching for producing silicon for solar batteries |
| CN104451871A (en) * | 2014-05-14 | 2015-03-25 | 浙江溢闳光电科技有限公司 | Method of improving quality of polysilicon material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114127011A (en) * | 2019-08-29 | 2022-03-01 | 瓦克化学股份公司 | Method for producing silicon blocks |
| CN114127011B (en) * | 2019-08-29 | 2024-03-08 | 瓦克化学股份公司 | Method for producing silicon blocks |
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Application publication date: 20180112 |