CN106365170A - Method of removing impurities from silicon ingot circulating material - Google Patents
Method of removing impurities from silicon ingot circulating material Download PDFInfo
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- CN106365170A CN106365170A CN201610727855.3A CN201610727855A CN106365170A CN 106365170 A CN106365170 A CN 106365170A CN 201610727855 A CN201610727855 A CN 201610727855A CN 106365170 A CN106365170 A CN 106365170A
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- silicon ingot
- cycle stock
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
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Abstract
The invention discloses a method of removing impurities from a silicon ingot circulating material. The method is characterized by including the steps of: 1) soaking the silicon ingot circulating material in an alkaline solution; 2) primarily cleaning and air-drying the soaked silicon ingot circulating material; 3) performing oriented polishing to the silicon ingot circulating material treated in the step 2); 4) secondarily cleaning the silicon ingot circulating material treated in the step 3) with hot water; 5) acid-pickling the silicon ingot circulating material treated in the step 4) in an acid solution; and 6) performing third-stage cleaning and drying to the silicon ingot circulating material treated in the step 5). The method can effectively remove the impurities from the silicon ingot circulating material and has high impurity removal effect.
Description
Technical field
The present invention relates to silicon ingot cycle stock purification technique field, more particularly, to a kind of side removing silicon ingot cycle stock impurity
Method.
Background technology
In order to tackle energy security and weather variation issue, the mankind have to become increasingly dependent on new forms of energy, thus new forms of energy
The long-run development trend of industry and its association industry is good.Wherein, solar energy power generating is new forms of energy most with prospects
Generation technology, from now on decades can constantly develop, and eventually become the main body of mankind's energy.Solar energy power generating has
There is following obvious advantage: 1) aboundresources, and will not be exhausted, it is renewable and clean energy resource.Particularly photovoltaic generation process is not
Water consumption, photovoltaic plant construction is not restricted by water resource, can any free time soil on, particularly can build in desert soil ground
If photovoltaic plant.2) photovoltaic cell is installed and is built simple, scaleable of installing, and operational management is convenient, both can be using spacious field
Ground is built it is also possible to be combined construction with building, and with little need for carrying out operation maintenance, the potentiality of exploitation are very big.
3) power producing characteristics of photovoltaic generation are substantially identical with power load characteristic, and in general, photovoltaic generation is the strongest in solar irradiation
Period at noon exerts oneself maximum, and the peak period of now also exactly electricity consumption, electricity can effectively be mitigated using solar energy power generating
The peak regulation pressure of Force system, is conducive to optimizing Operation of Electric Systems, saves fossil energy resources, realize target for energy-saving and emission-reduction.
Silicon ingot casting mostly is cycle stock and the collocation of primary polycrystalline uses at present.In actual production process, cycle stock is always
Recycle, if can not be clean by impurity treatment in it, this partial impurities will circulate in silicon ingot always, and constantly accumulate, and produce
Enrichment phenomenon is goed deep in life.And the presence of these impurity can substantially reduce the yield of silicon chip and the efficiency of silicon solar photovoltaic cell,
Thus the impurity removing in silicon ingot cycle stock is particularly important.
Traditional method removing the impurity in silicon ingot cycle stock mainly using the processing method of pickling again of first polishing, but
It is that the method can only remove the part of the surface impurity being exposed to silicon ingot cycle stock it is impossible to inner deep by silicon ingot cycle stock
Partial impurities remove.
Content of the invention
It is an object of the invention to proposing a kind of silicon ingot cycle stock impurity treatment method, can effectively remove silicon ingot cycle stock
Impurity, impurity-eliminating effect is preferable.
For reaching this purpose, the present invention employs the following technical solutions:
A kind of internal impurity treatment method of silicon ingot cycle stock, comprises the following steps:
1) silicon ingot cycle stock is put in alkaline solution and soak；
2) take out described step 1) in process after silicon ingot cycle stock, it is once cleaned and is air-dried；
3) to described step 2) in process after silicon ingot cycle stock be oriented polishing；
4) using hot water to described step 3) in process after silicon ingot cycle stock carry out secondary cleaning；
5) by described step 4) in process after silicon ingot cycle stock put into and in acid solution, carry out pickling；
6) take out described step 5) in process after silicon ingot cycle stock, carry out three times and clean and dry.
Wherein, described step 1) in alkaline solution be 30%～40% for concentration sodium hydroxide solution, and hydroxide
The purity of sodium is at least 99%.
Preferably, the concentration of sodium hydroxide solution can for 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%,
38%th, 39% or 40%.
Wherein, described step 1) in immersion be room temperature under soak, soak time be 4h～5h.
Preferably, soak time in alkaline solution for the silicon ingot cycle stock can for 4h, 4.1h, 4.2h, 4.3h, 4.4h,
4.5h, 4.6h, 4.7h, 4.8h, 4.9h or 5h.
Wherein, described step 2) in once cleaning use deionized water rinsing to aqueous solution be in neutrality.
Wherein, described step 3) in using grinding wheel to described step 2) in process after silicon ingot cycle stock be oriented
Polishing.
Wherein, described step 4) in secondary cleaning use hot water temperature be 90 DEG C～100 DEG C, followed with removing silicon ingot
The impurity of the surface attachment of ring material；Be conducive to improving the efficiency of follow-up pickling simultaneously.
Preferably, the temperature of hot water can for 90 DEG C, 91 DEG C, 92 DEG C, 93 DEG C, 94 DEG C, 95 DEG C, 96 DEG C, 97 DEG C, 98 DEG C, 99
DEG C or 100 DEG C.
Wherein, described step 5) in acid solution be 45%～49% by concentration Fluohydric acid. and concentration be 65%～
69% nitric acid mixes；The volume proportion of Fluohydric acid. and nitric acid is 1:6～10, can remove silicon ingot cycle stock by pickling
The oxide on surface and non-silicon impurity.
Preferably, the concentration of Fluohydric acid. can be 45%, 46%, 47%, 48% or 49%；The concentration of nitric acid can for 65%,
66%th, 67%, 68% or 69%；The volume proportion of Fluohydric acid. and nitric acid can be 1:6,1:7,1:8,1:9 or 1:10.
Wherein, described step 5) in the pickling of silicon ingot cycle stock time be 30～90s.
Preferably, pickling time can for 30s, 35s, 40s, 45s, 50s, 55s, 60s, 65s, 70s, 75s, 80s, 85s or
90s.
Wherein, described step 6) in three cleanings comprise the following steps: i) to described step 5) in process after silicon ingot
Cycle stock carries out deionized water rinsing, and the silicon ingot cycle stock after rinsing is immersed in pure water, to avoid silicon ingot cycle stock straight
Connect ingress of air；Ii) ultrasound wave cleaning is carried out to the silicon ingot cycle stock being immersed in pure water in described step i).
Wherein, described step ii) in ultrasound wave cleaning technological parameter be set to: the temperature of deionized water be 30 DEG C～
50 DEG C, scavenging period is 50min～60min.
Preferably, the temperature of deionized water can be 30 DEG C, 40 DEG C, 50 DEG C；Scavenging period can for 50min, 51min,
52min, 53min, 54min, 55min, 56min, 57min, 58min, 59min or 60min.
Wherein, described step 6) in the technological parameter of drying be set to: oven temperature is 120 DEG C～140 DEG C, during drying
Between be 2h～3h.
Preferably, oven temperature can be 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C or 140 DEG C；Drying time can for 2h,
2.1h, 2.2h, 2.3h, 2.4h, 2.5h, 2.6h, 2.7h, 2.8h, 2.9h or 3h.
The invention has the benefit that a kind of silicon ingot cycle stock impurity treatment method proposed by the present invention, first by silicon ingot
Cycle stock is put in alkaline solution, and the silicon ingot cycle stock of the periphery of the impurity being enriched in silicon ingot cycle stock is corroded, so that
Obtain impurity to expose, then the impurity exposing is oriented with polishing to go the removal of impurity, reuses hot water and the silicon ingot after polishing is followed
Ring material is carried out, and then passes through the oxidation on the surface of mixed acid solution corrosion removing silicon ingot cycle stock of Fluohydric acid. and nitric acid again
Thing and non-silicon impurity, remove the acid residual on silico briquette surface finally by cleaning and stoving process, thus greatly reducing silicon ingot circulation
Impurity in material, impurity-eliminating effect is preferable.
Brief description
Fig. 1 is the flow chart of a kind of method of removal silicon ingot cycle stock impurity that the present invention provides.
Specific embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by specific embodiment.
As shown in figure 1, a kind of method removing silicon ingot cycle stock impurity, comprise the following steps:
1) silicon ingot cycle stock is put in alkaline solution and soak, so that the impurity of the enrichment in silicon ingot cycle stock exposes；
2) take out step 1) in process after silicon ingot cycle stock, it is once cleaned and is air-dried；
3) to step 2) in process after silicon ingot cycle stock be oriented polishing；
4) using hot water to step 3) in process after silicon ingot cycle stock carry out secondary cleaning；
5) by step 4) in process after silicon ingot cycle stock put into and in acid solution, carry out pickling；
6) take out step 5) in process after silicon ingot cycle stock, carry out three times and clean and dry.
Embodiment 1
A kind of method removing silicon ingot cycle stock impurity proposed by the present invention, comprises the following steps:
1) silicon ingot cycle stock is put in 30% sodium hydroxide solution, soak 5h at normal temperatures；
2) take out step 1) in process after silicon ingot cycle stock, it is once cleaned and is air-dried；When once cleaning, use
Deionized water rinsing is in neutrality to aqueous solution；
3) to step 2) in process after silicon ingot cycle stock be oriented polishing, thus impurity is removed；
4) hot water the use of temperature being 90 DEG C is to step 3) in process after silicon ingot cycle stock carry out secondary cleaning, with remove
The impurity of the surface attachment of silicon ingot cycle stock；Be conducive to improving the efficiency of follow-up pickling simultaneously.
5) by step 4) in process after silicon ingot cycle stock to put into the Fluohydric acid. being 47% by concentration and concentration be 67%
Pickling 90s in the acid solution that nitric acid is mixed with volume proportion for 1:6.
6) take out step 5) in process after silicon ingot cycle stock, deionized water rinse to aqueous solution be in neutrality, and
Silicon ingot cycle stock after rinsing is immersed in pure water；Then carry out ultrasound wave cleaning.The technological parameter setting of ultrasound wave cleaning
For: the temperature of deionized water is 30 DEG C, and scavenging period is 60min.Oven for drying, the technological parameter of drying is used after ultrasound wave cleaning
It is set to: oven temperature is 120 DEG C, drying time is 3h.
The testing result of the silicon ingot cycle stock that the present embodiment 1 obtains is shown in Table 1.
Embodiment 2
1) silicon ingot cycle stock is put in 35% sodium hydroxide solution, soak 4.5h at normal temperatures；
2) take out step 1) in process after silicon ingot cycle stock, it is once cleaned and is air-dried；When once cleaning, use
Deionized water rinsing is in neutrality to aqueous solution；
3) to step 2) in process after silicon ingot cycle stock be oriented polishing, thus impurity is removed；
4) hot water the use of temperature being 95 DEG C is to step 3) in process after silicon ingot cycle stock carry out secondary cleaning, with remove
The impurity of the surface attachment of silicon ingot cycle stock；Be conducive to improving the efficiency of follow-up pickling simultaneously.
5) by step 4) in process after silicon ingot cycle stock to put into the Fluohydric acid. being 45% by concentration and concentration be 65%
Pickling 75s in the acid solution that nitric acid is mixed with volume proportion for 1:10.
6) take out step 5) in process after silicon ingot cycle stock, deionized water rinse to aqueous solution be in neutrality, and
Silicon ingot cycle stock after rinsing is immersed in pure water；Then carry out ultrasound wave cleaning.The technological parameter setting of ultrasound wave cleaning
For: the temperature of deionized water is 50 DEG C, and scavenging period is 50min.Oven for drying, the technological parameter of drying is used after ultrasound wave cleaning
It is set to: oven temperature is 140 DEG C, drying time is 2h.
The testing result of the silicon ingot cycle stock that the present embodiment 2 obtains is shown in Table 1.
Embodiment 3
1) silicon ingot cycle stock is put in 40% sodium hydroxide solution, soak 4h at normal temperatures；
2) take out step 1) in process after silicon ingot cycle stock, it is once cleaned and is air-dried；When once cleaning, use
Deionized water rinsing is in neutrality to aqueous solution；
3) to step 2) in process after silicon ingot cycle stock be oriented polishing, thus impurity is removed；
4) hot water the use of temperature being 100 DEG C is to step 3) in process after silicon ingot cycle stock carry out secondary cleaning, to go
Impurity except the surface attachment of silicon ingot cycle stock；Be conducive to improving the efficiency of follow-up pickling simultaneously.
5) by step 4) in process after silicon ingot cycle stock to put into the Fluohydric acid. being 49% by concentration and concentration be 69%
Pickling 60s in the acid solution that nitric acid is mixed with volume proportion for 1:8.
6) take out step 5) in process after silicon ingot cycle stock, deionized water rinse to aqueous solution be in neutrality, and
Silicon ingot cycle stock after rinsing is immersed in pure water；Then carry out ultrasound wave cleaning.The technological parameter setting of ultrasound wave cleaning
For: the temperature of deionized water is 40 DEG C, and scavenging period is 60min.Oven for drying, the technological parameter of drying is used after ultrasound wave cleaning
It is set to: oven temperature is 130 DEG C, drying time is 3h.
The testing result of the silicon ingot cycle stock that the present embodiment 3 obtains is shown in Table 1.
Comparative example 1
Other operating procedures of this comparative example 1 and parameter are such as embodiment 1, except for the difference that, no step 1), step 2), step
Rapid 3) and step 4).The testing result of the silicon ingot cycle stock that this comparative example 1 obtains is shown in Table 1.
Comparative example 2
Other operating procedures of this comparative example 2 and parameter are such as embodiment 2, except for the difference that, no step 1), step 2), step
Rapid 3) and step 4).The testing result of the silicon ingot cycle stock that this comparative example 2 obtains is shown in Table 1.
Comparative example 3
Other operating procedures of this comparative example 3 and parameter are such as embodiment 3, except for the difference that, no step 1), step 2), step
Rapid 3) and step 4).The testing result of the silicon ingot cycle stock that this comparative example 3 obtains is shown in Table 1.
Table 1 embodiment 1 to 3 and the test result of comparative example 1 to 3
Describe the know-why of the present invention above in association with specific embodiment.These descriptions are intended merely to explain the present invention's
Principle, and limiting the scope of the invention can not be construed to by any way.Based on explanation herein, the technology of this area
Personnel do not need to pay other specific embodiments that performing creative labour can associate the present invention, and these modes fall within
Within protection scope of the present invention.
Claims (9)
1. a kind of method removing silicon ingot cycle stock impurity is it is characterised in that comprise the following steps:
1) silicon ingot cycle stock is put in alkaline solution and soak；
2) take out described step 1) in process after silicon ingot cycle stock, it is once cleaned and is air-dried；
3) to described step 2) in process after silicon ingot cycle stock be oriented polishing；
4) using hot water to described step 3) in process after silicon ingot cycle stock carry out secondary cleaning；
5) by described step 4) in process after silicon ingot cycle stock put into and in acid solution, carry out pickling；
6) take out described step 5) in process after silicon ingot cycle stock, carry out three times and clean and dry.
2. a kind of method removing silicon ingot cycle stock impurity according to claim 1 is it is characterised in that described step 1) in
Alkaline solution be 30%～40% for concentration sodium hydroxide solution.
3. a kind of method removing silicon ingot cycle stock impurity according to claim 2 is it is characterised in that described step 1) in
Immersion be room temperature under soak, soak time be 4h～5h.
4. a kind of method removing silicon ingot cycle stock impurity according to claim 1 is it is characterised in that described step 4) in
Secondary cleaning use hot water temperature be 90 DEG C～100 DEG C.
5. a kind of method removing silicon ingot cycle stock impurity according to claim 1 is it is characterised in that described step 5) in
Acid solution be 45%～49% by concentration Fluohydric acid. and nitric acid that concentration is 65%～69% mix；Fluohydric acid. and
The volume proportion of nitric acid is 1:6～10.
6. according to claim 1 or 5 a kind of method removing silicon ingot cycle stock impurity it is characterised in that described step
5) in pickling time be 30～90s.
7. a kind of method removing silicon ingot cycle stock impurity according to claim 1 is it is characterised in that described step 6) in
Three cleanings comprise the following steps: i) to described step 5) in process after silicon ingot cycle stock carry out deionized water rinsing, and
Silicon ingot cycle stock after rinsing is immersed in pure water, to avoid silicon ingot cycle stock directly contact air；Ii) to described step i)
In the silicon ingot cycle stock that is immersed in pure water carry out ultrasound wave cleaning.
8. a kind of method removing silicon ingot cycle stock impurity according to claim 7 is it is characterised in that described step ii)
In ultrasound wave cleaning technological parameter be set to: the temperature of deionized water be 30 DEG C～50 DEG C, scavenging period be 50min～
60min.
9. a kind of method removing silicon ingot cycle stock impurity according to claim 1 is it is characterised in that described step 6) in
The technological parameter of drying be set to: oven temperature is 120 DEG C～140 DEG C, and drying time is 2h～3h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107572533A (en) * | 2017-09-07 | 2018-01-12 | 晶科能源有限公司 | The minimizing technology of impurity in a kind of silicon material flaw-piece |
| CN109137065A (en) * | 2018-10-24 | 2019-01-04 | 镇江环太硅科技有限公司 | One kind is for the silicon material recovery and treatment method that gives up |
| CN109848122A (en) * | 2018-12-29 | 2019-06-07 | 晶能光电（江西）有限公司 | The cleaning method of SiC panel surface AlN film layer |
| CN109860040A (en) * | 2019-01-30 | 2019-06-07 | 西安奕斯伟硅片技术有限公司 | Silicon etch process, silico briquette, pulling of crystals method of pulling up and monocrystalline |
| CN115505934A (en) * | 2022-10-21 | 2022-12-23 | 同创普润(上海)机电高科技有限公司 | Pretreatment method for remelting and utilizing ultra-pure aluminum ingot for semiconductor |
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| CN107572533A (en) * | 2017-09-07 | 2018-01-12 | 晶科能源有限公司 | The minimizing technology of impurity in a kind of silicon material flaw-piece |
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| CN109848122A (en) * | 2018-12-29 | 2019-06-07 | 晶能光电（江西）有限公司 | The cleaning method of SiC panel surface AlN film layer |
| CN109860040A (en) * | 2019-01-30 | 2019-06-07 | 西安奕斯伟硅片技术有限公司 | Silicon etch process, silico briquette, pulling of crystals method of pulling up and monocrystalline |
| CN109860040B (en) * | 2019-01-30 | 2022-02-01 | 西安奕斯伟材料科技有限公司 | Silicon etching method, silicon ingot, pulling method of Czochralski single crystal, and single crystal |
| CN115505934A (en) * | 2022-10-21 | 2022-12-23 | 同创普润(上海)机电高科技有限公司 | Pretreatment method for remelting and utilizing ultra-pure aluminum ingot for semiconductor |
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Application publication date: 20170201 |