CN1191520A - Process for producing high-purity silicon - Google Patents
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- CN1191520A CN1191520A CN 95197920 CN95197920A CN1191520A CN 1191520 A CN1191520 A CN 1191520A CN 95197920 CN95197920 CN 95197920 CN 95197920 A CN95197920 A CN 95197920A CN 1191520 A CN1191520 A CN 1191520A
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Abstract
A process for producing high-purity silicon suitable for solar battery at a low cost, comprises the step (a) of melt mixing crude silicon with calcium silicate at a temp. of 1544 deg.C or above to cause the boron contained in the silicon to migrate into the slag, the step(b)of leaving the liquid mixture obtained in the step(a)to stand still in an inert gas atmosphere to cause the separation into a lower slag layer and an upper molten silicon layer, followed by temp. adjustment to 1410 to 1544 deg.C to cause slag coagulation while keeping the molten silicon as such,the step(c)of dipping a cooling member in the molten silicon to cause highly purified silicon to deposit on the surface of the cooling member,followed by pulling-out of the member from the molten silicon and release of the deposited high-purity silicon lump from the member,and the step(d)of remelting the high-purity silicon obtained in the step(c)and vaccum treating the molten silicon to evaporate away the phosphorus therein.
Description
The present invention relates to the manufacture method of high purity silicon, in more detail, relate to the method that to make silicon for solar cell at an easy rate.
Silicon generally has Pure Silicon Metal that is made by carbon reduction by silica and the high purity silicon that obtains by silicomethane or this Pure Silicon Metal of trichlorosilane method refining in electric arc furnace, the latter is applied to semi-conductor.The employed silicon of semi-conductor is the high purity goods that are also referred to as 11 9 degree, and its price is extremely expensive.
On the one hand, though silicon for solar cell also requires high purity, its purity reaches 69 degree and gets final product.That is to say, its purity be the total concn of impurity element in the silicon in the concentration of the degree of 0.1～10ppm and phosphorus and boron respectively below 1ppm.After about 1980, states such as the U.S., West Germany, Japan begin big quantity research about making the technology of the high purity silicon with such solar battery grade purity at an easy rate.
For example, J.Dietl is at " the photocell preparation method II (1987) of silicon " (SiliconProcessing for Photovoltaics II, Elsevier Sci, Publ.B.V., 285 (1987)) comprehensively summarized in the past a large amount of relevant silicon purified results of study for the 285th page in, and at " the 8th European Economic Community's photoelectrical solar proceeding " (Proc.8th EC Photovoltaic Solar EnergyConf., FLorence (1988), in p.599) the 599th page have proposed to make quite at an easy rate a route of the metallurgy method of solar battery grade silicon.
That is, the route that J.Dietl proposed is made of 4 operations:
(1) utilize electric arc furnace that the Pure Silicon Metal of making through carbon reduction in the electric furnace is mixed with the Calucium Silicate powder liquation and contact, make in the silicon boron to silicic acid melt move in the calcium liquid take off the boron treatment process;
(2) leave standstill mixed molten liquid after chemical industry preface (1) is handled, thereby make heavy Calucium Silicate powder slag deposition be separated to the upper strata, and this silicon layer is cast to casting operation in the mould to lower floor, silicon;
(3) silico briquette to operation (2) gained carries out fragmentation, nitration mixture is washed, and makes impurity element dissolveds such as the iron that is segregated in silico briquette grain circle and calcium and carries out the purifying of silicon, be i.e. hydrometallurgy purifying method (hydrometallurgical refining process);
(4) the Powdered refined silicon of operation (3) gained is carried out dephosphorization by fusion, vacuum-treat after, be cast in the mould, thereby obtain the operation of solar battery grade silico briquette.
On the one hand, the spy opens and discloses a kind of effective Pure Silicon Metal method of refining in the clear 63-45112 communique, promptly under inert gas atmosphere, the hollow rotating cooling body is impregnated in the molten metal silicon, and high purity silicon is separated out in the outside surface crystallization of rotation cooling body.
But, in the metallurgy method of utilizing the segregated solidification principle of above-mentioned J.Dietl, owing to include the hydrometallurgy purifying method, so the low problem of productivity is arranged.In addition, the spy opens in the described method of clear 63-45112 communique, and the low problem of decreasing ratio of boron is arranged.
Therefore, reality be also untapped go out can the mass production silicon for solar cell technology, what use in solar cell is the bits of the used high purity silicon of semi-conductor.
In view of the foregoing, the object of the present invention is to provide a kind of method that can make solar battery grade silicon at an easy rate, and supply with silicon for solar cell at an easy rate.
Because the spy opens the described cooling body pickling process of clear 63-45112 communique and can remove the little impurity element of segregation coefficient expeditiously to solidifying by folk prescription, if thereby can be combined in one with (2)～(3) process of the silicon method of refining that constitutes by above-mentioned 4 sections operations of J.Dietl, can estimate that so whole technology can raise the efficiency significantly, and can make solar battery grade silicon more at an easy rate.That is to say, if can substitute the operation (3) of carrying out leaching by the fragmentation and the pickling of silico briquette, and the molten silicon of operation (2) gained is solidified the purified words by the cooling body dipping, so just can establish the effective silicon method of refining of the degree of in the past not expected.
But the inventor is being undertaken by (1), (2) when Pure Silicon Metal takes off boron, finds owing to use the Calucium Silicate powder liquation, has caused that the concentration of calcium increases in the silicon, thereby can flood the purifying method decalcification by cooling body and just become quite important.Because the past was not reported the segregation coefficient as the calcium of impurity in the silicon, so it be unclear that the effect of utilizing this method of refining decalcification.
The inventor removes the processing by (1), (2) between the fusing point of fusing point～Calucium Silicate powder that molten silicon behind the boron remains on rough silicon, the slag of the Calucium Silicate powder that is separated to the bottom is solidified, then the hollow rotating cooling body of graphite system is impregnated in the molten silicon.Drawing is separated out and adherent silico briquette, dismounting at the cooling body surface crystallization, analyzes the concentration of the concentration of the calcium in the silicon and iron, aluminium etc., find with molten silicon in compare, the concentration of calcium and iron, aluminium reduce equally significantly.That is, compare with the described method of the clear 63-45112 communique of method and the Te Kai of J.Dietl, the inventor has found to make effectively, at an easy rate significantly the method for solar battery grade silicon.
That is, the 1st of high purity silicon of the present invention the kind of manufacture method comprises:
(a) melting mixing under the temperature more than the Calucium Silicate powder fusing point rough silicon and Calucium Silicate powder is moved to boron in the silicon and is taken off the boron treatment process in the Calucium Silicate powder slag;
(b) in inert gas atmosphere, leave standstill the mixed solution of operation (a) gained, the Calucium Silicate powder molten slag layer of lower floor is separated with the fusion silicon layer on upper strata, then temperature is set between the fusing point of fusing point～Calucium Silicate powder of rough silicon, when the Calucium Silicate powder slag is solidified silicon is remained on the separation circuit of molten state;
(c) under inert gas atmosphere, cooling body is impregnated in the molten silicon of operation (b) gained, the silicon crystallization of high purifying is separated out stick to the cooling body outside surface, from molten silicon, draw this cooling body then and operation is separated out in the silicon crystallization that the high purity silico briquette that crystallization is separated out is pulled down from cooling body;
(d) the high purity silicon fusion again of operation (c) gained, thus the vacuum-treat molten silicon evaporates the dephosphorization treatment operation that removes the phosphorus in the high purity silicon then.
In the aforesaid method, when carrying out operation (c), both can be impregnated into cooling body in the fusion silicon layer above the Calucium Silicate powder molten slag layer, and also can move on to other groove to the fusion silicon layer earlier and then cooling body is impregnated into wherein.
The 2nd kind of manufacture method of high purity silicon of the present invention comprises:
(a) melting mixing under the temperature more than the Calucium Silicate powder fusing point rough silicon and Calucium Silicate powder is moved to boron in the silicon and is taken off the boron treatment process in the Calucium Silicate powder slag;
(b) in inert gas atmosphere, leave standstill the mixed solution of operation (a) gained, the Calucium Silicate powder molten slag layer of lower floor is separated with the fusion silicon layer on upper strata, then temperature is set between the fusing point of fusing point～Calucium Silicate powder of rough silicon, when the Calucium Silicate powder slag is solidified silicon is remained on the separation circuit of molten state;
(c) molten silicon of operation (b) gained is moved on to the vacuum-treat groove, thereby carry out the dephosphorization treatment operation that the vacuum-treat evaporation removes the phosphorus in the molten silicon;
(d) under inert gas atmosphere, cooling body is impregnated in the molten silicon of operation (c) gained, the silicon crystallization of high purifying is separated out stick to the cooling body outside surface, from molten silicon, draw this cooling body then and operation is separated out in the silicon crystallization that the high purity silico briquette that crystallization is separated out is pulled down from cooling body.
The fusing point of pure silicon is 1410 ℃, and the fusing point of pure Calucium Silicate powder is 1544 ℃.
Among the present invention, separate out the used cooling body of operation, can use the ducted body that constitutes with the good material of molten silicon reaction and heat conductivity by not as silicon crystallization in the present invention.That is the ducted body that constitutes by potteries such as silicon nitride or graphite.By to delivering to ducted body inside silicon can being separated out at the cooling body outside surface in crystallization.
In the present invention, preferred limit rotation cooling body, the limit is separated out the silicon crystallization of high purifying.Carry out crystallization by rotation cooling body limit, limit and separate out, not only can improve the production efficiency of silicon, and can improve the decreasing ratio of impurity elements such as iron, calcium, aluminium, copper, and can produce more highly purified silicon.The circumferential speed of rotation cooling body is preferably more than 500cm/min, more preferably more than 1000cm/min.Under occasion with such circumferential speed rotation cooling body, stick to thickization of crystallization grain growing of the silicon of cooling body outside surface, the impurity element quantity that is concentrated in a boundary reduces, and simultaneously intragranular impurity element concentration reduces.Can think, silicon purified principle is the impurity element that removes the place, grain circle that is concentrated in the silico briquette that is solidified in the mold with sour dissolved in the hydrometallurgy method, but because compare the impurity concentration of its intracrystalline with the inventive method very big, so compare its final impurity removal percentage with the inventive method low.
Among the present invention, the method that the dismounting crystallization is separated out at the high purity silicon of cooling body outside surface is by mechanical means abate or makes its fusion again.
In addition, dephosphorization treatment operation of the present invention is well-known dephosphorization treatment, also can remove the vacuum-treat that phosphorus substitutes molten silicon by the reaction with at least a gas that is selected from oxygen, water vapour, carbon monoxide and carbon dioxide.
According to the manufacture method of high purity silicon of the present invention, to compare with the hydrometallurgy purifying method that is considered to past the best way, the time is shorter, efficient is very good, and can make more highly purified silicon.Therefore, method of the present invention is of great use as the method that can make solar battery grade silicon at an easy rate.
Fig. 1 is the process flow sheet of the summary of expression the inventive method.
Fig. 2 is the longitudinal sectional drawing of expression cooling body structure.
Fig. 3 is the process flow sheet of the summary of expression the inventive method.
Specifically describe embodiments of the invention with reference to the accompanying drawings.Embodiment 1
Fig. 1 is the process flow sheet of the 1st kind of method summary of expression the present invention.
Rough Pure Silicon Metal contains iron 4500ppm, aluminium 600ppm, copper 185ppm, boron 18ppm, calcium 150ppm and the phosphorus 45ppm as impurity element.It and Calucium Silicate powder powder in the electric arc furnace of packing into (1), stir (operation (a)) 1650 ℃ of following melting mixing with 1: 1 mixed of weight ratio.Leave standstill this mixed solution in inert gas atmosphere, Calucium Silicate powder slag and silicon melt are because difference of specific gravity is separated into 2 layers.Then temperature is dropped to 1480 ℃, the Calucium Silicate powder slag is solidified, silicon remains on molten state (operation (b)).
Aluminium content in this silicon melt layer is that 40ppm, boron content are 1ppm, and its aluminium content and boron content reduce respectively, and calcium contents is increased to 420ppm from 150ppm, but the content of other metallic impurity elements does not almost have change.
The graphite system of tubular hollow rotating cooling body (2) is impregnated in this silicon melt layer above molten slag layer, and making it is to rotate 10 minutes under the 2000cm/min in circumferential speed, makes silicon separate out adhesion (operation (c)) in the crystallization of cooling body outside surface.As shown in Figure 2, the part that is impregnated in the molten silicon of at this moment used hollow rotating cooling body (2) becomes taper shape.In addition, dispose cooling fluid supply-pipe (3) in the hollow rotating cooling body (2).On cooling fluid supply-pipe (3), when cooling body (2) floods, on the circumferential wall of molten silicon liquid level, have a lot of cooling fluids and blow out hole (4) with the upper/lower positions part.
Analyze the silico briquette of gained, the content of iron, aluminium, copper, boron and calcium all drops to below the 1ppm.Phosphorus content is 22ppm.
To this silico briquette carry out fusion again, thereby vacuum-treat obtains high purity silicon (operation (d)).The phosphorus content of this high purity silicon drops to below the 1ppm.Embodiment 2～5
Except the circumferential speed of hollow rotating cooling body (2) rotation is set in 0cm/min (embodiment 2), 300cm/min (embodiment 3), 1000cm/min (embodiment 4), 3000cm/min (embodiment 5) respectively, carry out technology similarly to Example 1, obtain high purity silicon.
The foreign matter content of the high purity silicon of gained is listed in the table 1.
Table 1
Embodiment 6
| Rotation round speed (cm/min) | Impurity content (ppm) Al Fe Cu B P Ca | Purity (pct) | |
| Embodiment 2 embodiment 3 embodiment 4 embodiment 1 embodiment 5 | ????0 ????300 ????1000 ????2000 ????3000 | ????150??????????1520?????????48?????????＜1???????＜1???????1720 ????75???????????180??????????18?????????＜1???????＜1???????120 ????＜1??????????2????????????＜1????????＜1???????＜1???????＜1 ????＜1??????????＜1??????????＜1????????＜1???????＜1???????＜1 ????＜1??????????＜1??????????＜1????????＜1???????＜1???????＜1 | ????99.65 ????99.9600 ????99.9998 ????99.9999 ????99.9999 |
| The rough Pure Silicon Metal of raw material | ????600??????????4500?????????185????????18????????45????????150 | ||
| The balance segregation coefficient | ????2×10 -3?????8×10 -6?????4×10 -4???0.8???????0.35??????500 | ||
Fig. 3 is the process flow sheet of the summary of the 2nd kind of method of expression the present invention.
Rough Pure Silicon Metal contains iron 4200ppm, aluminium 450ppm, copper 190ppm, boron 15ppm, calcium 130ppm and the phosphorus 35ppm as impurity element.It and Calucium Silicate powder powder in the electric arc furnace of packing into (1), stir (operation (a)) 1660 ℃ of following melting mixing with 6: 4 mixed of weight ratio.Leave standstill this mixed solution in inert gas atmosphere, Calucium Silicate powder slag and silicon melt are because difference of specific gravity is separated into 2 layers.Then temperature is dropped to 1520 ℃, the Calucium Silicate powder slag is solidified, silicon remains on molten state (operation (b)).
This silicon melt decant(-ation) in vacuum-treat groove (5), is carried out 10 hours vacuum-treat (operation (c)).At this moment the boron content in the silicon is that 1ppm is following, phosphorus content is that 2ppm, aluminium content reduce to 30ppm, calcium contents is increased to 500ppm, but the content of other metallic impurity elements does not almost have change.
Then vacuum-treat groove (5) is placed inert gas atmosphere, identical hollow rotating cooling body (2) used among the embodiment (1) is impregnated into the silicon melt layer, in circumferential speed is to make its rotation 10 minutes under the 5000cm/min, allows the silicon crystallization separate out and sticks to cooling body outside surface (operation (d)).
Analyze the silico briquette of gained, the content of iron, aluminium, copper, boron, calcium and phosphorus is all below 1ppm.Embodiment 7～10
Except the circumferential speed of hollow rotating cooling body (2) rotation is set in 0cm/min (embodiment 7), 300cm/min (embodiment 8), 1500cm/min (embodiment 9), 3000cm/min (embodiment 10) respectively, carry out technology similarly to Example 6, obtain high purity silicon.
The foreign matter content of the high purity silicon of gained is listed in the table 2.
Table 2
| Rotation round speed (cm/min) | Impurity content (ppm) Al Fe Cu B P Ca | Purity (pct) | |
| Embodiment 7 embodiment 8 embodiment 9 embodiment 10 embodiment 6 | ????0 ????300 ????1500 ????3000 ????5000 | ????130???????????1460????????50?????????＜1????????＜1???????220 ????72????????????176?????????20?????????＜1????????＜1???????46 ????＜1???????????＜1?????????＜1????????＜1????????＜1???????＜1 ????＜1???????????＜1?????????＜1????????＜1????????＜1???????＜1 ????＜1???????????＜1?????????＜1????????＜1????????＜1???????＜1 | ????99.81 ????99.96 ????99.9999 ????99.9999 ????99.9999 |
| The rough Pure Silicon Metal of raw material | ????450???????????4200????????190????????15?????????35????????130 | ||
| The balance segregation coefficient | ????2×10 -3??????8×10 -6????4×10 -4???0.8????????0.35??????500 | ||
As shown in Table 1 and Table 2, the silicon of prepared in accordance with the method for the present invention all is high purity.In addition, preferably set more than 1000cm/min, can obtain more highly purified silicon by preferred rotation cooling body and rotation round speed.
The present invention can be used as the manufacture method of high purity silicon, in more detail, can be used as the method for making silicon for solar cell at an easy rate.
Claims (4)
1, a kind of manufacture method of high purity silicon comprises:
(a) melting mixing under the temperature more than the Calucium Silicate powder fusing point rough silicon and Calucium Silicate powder is moved to boron in the silicon and is taken off the boron treatment process in the Calucium Silicate powder slag;
(b) in inert gas atmosphere, leave standstill the mixed solution of operation (a) gained, the Calucium Silicate powder molten slag layer of lower floor is separated with the fusion silicon layer on upper strata, then temperature is set between the fusing point of fusing point～Calucium Silicate powder of rough silicon, when the Calucium Silicate powder slag is solidified silicon is remained on the separation circuit of molten state;
(c) under inert gas atmosphere, cooling body is impregnated in the molten silicon of operation (b) gained, make the silicon of high purifying separate out adhesion, from molten silicon, draw this cooling body then and operation is separated out in the silicon crystallization that crystalline high purity silico briquette is pulled down from cooling body in the crystallization of cooling body outside surface;
(d) high purity silicon of fusion operation again (c) gained, thus the vacuum-treat molten silicon evaporates the dephosphorization treatment operation that removes the phosphorus in the high purity silicon then.
2, a kind of manufacture method of high purity silicon comprises:
(a) melting mixing under the temperature more than the Calucium Silicate powder fusing point rough silicon and Calucium Silicate powder is moved to boron in the silicon and is taken off the boron treatment process in the Calucium Silicate powder slag;
(b) in inert gas atmosphere, leave standstill the mixed solution of operation (a) gained, the Calucium Silicate powder molten slag layer of lower floor is separated with the fusion silicon layer on upper strata, then temperature is set between the fusing point of fusing point～Calucium Silicate powder of rough silicon, when the Calucium Silicate powder slag is solidified silicon is remained on the separation circuit of molten state;
(c) operation (b) thus the molten silicon of gained moves on to the vacuum-treat groove carries out the dephosphorization treatment operation that vacuum-treat evaporation removes the phosphorus in the molten molten silicon;
(d) under inert gas atmosphere, cooling body is impregnated in the molten silicon of operation (c) gained, the silicon of high purifying is adhered in the crystallization of cooling body outside surface, from molten silicon, draw this cooling body then and operation is separated out in the silicon crystallization that the high purity silico briquette that crystallization is separated out is pulled down from cooling body.
3, according to the manufacture method of the high purity silicon of claim 1 or 2, wherein in the silicon Crystallization Procedure, limit rotation cooling body, the limit is separated out the silicon crystallization of high purifying.
4, according to the manufacture method of each described high purity silicon in the claim 1～3, wherein in the dephosphorization treatment operation, remove the vacuum-treat that phosphorus substitutes molten silicon by reaction with at least a gas that is selected from oxygen, water vapour, carbon monoxide and carbon dioxide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN95197920A CN1083396C (en) | 1995-07-14 | 1995-07-14 | Process for producing high-purity silicon |
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| CN95197920A CN1083396C (en) | 1995-07-14 | 1995-07-14 | Process for producing high-purity silicon |
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| CN1191520A true CN1191520A (en) | 1998-08-26 |
| CN1083396C CN1083396C (en) | 2002-04-24 |
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| CN95197920A Expired - Fee Related CN1083396C (en) | 1995-07-14 | 1995-07-14 | Process for producing high-purity silicon |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1095441C (en) * | 2000-07-07 | 2002-12-04 | 中山大学 | Preparation of nanometer-level silicon material |
| CN1307094C (en) * | 2002-05-22 | 2007-03-28 | 埃尔凯姆公司 | A calcium-silicate based slag for treatment of molten silicon |
| CN1313368C (en) * | 2003-10-10 | 2007-05-02 | 曹文兴 | Production equipment and method of silicon used for solar battery |
| CN100372762C (en) * | 2006-01-25 | 2008-03-05 | 昆明理工大学 | Method for preparing solar grade polysilicon |
| US7455822B2 (en) | 2002-07-23 | 2008-11-25 | Nippon Steel Corporation | Method for production of silicon |
| CN100457613C (en) * | 2003-12-29 | 2009-02-04 | 埃尔凯姆有限公司 | Silicon feedstock for solar cells |
| CN100595352C (en) * | 2007-07-17 | 2010-03-24 | 佳科太阳能硅(龙岩)有限公司 | Method for preparing big ingot of polysilicon in level of solar energy |
| CN101636823B (en) * | 2006-12-04 | 2012-09-05 | 埃尔凯姆太阳能公司 | Multicrystalline P type wafer, Phosphorus diffusion, phosphorus gettering method, and solar panel including same |
| CN102674365A (en) * | 2012-04-23 | 2012-09-19 | 锦州新世纪石英（集团）有限公司 | Method for removing metal impurities in polycrystalline silicon |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4612179A (en) * | 1985-03-13 | 1986-09-16 | Sri International | Process for purification of solid silicon |
| JPH0753569B2 (en) * | 1986-08-07 | 1995-06-07 | 昭和アルミニウム株式会社 | Silicon purification method |
-
1995
- 1995-07-14 CN CN95197920A patent/CN1083396C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1095441C (en) * | 2000-07-07 | 2002-12-04 | 中山大学 | Preparation of nanometer-level silicon material |
| CN1307094C (en) * | 2002-05-22 | 2007-03-28 | 埃尔凯姆公司 | A calcium-silicate based slag for treatment of molten silicon |
| US7455822B2 (en) | 2002-07-23 | 2008-11-25 | Nippon Steel Corporation | Method for production of silicon |
| CN1313368C (en) * | 2003-10-10 | 2007-05-02 | 曹文兴 | Production equipment and method of silicon used for solar battery |
| CN100457613C (en) * | 2003-12-29 | 2009-02-04 | 埃尔凯姆有限公司 | Silicon feedstock for solar cells |
| CN100372762C (en) * | 2006-01-25 | 2008-03-05 | 昆明理工大学 | Method for preparing solar grade polysilicon |
| CN101636823B (en) * | 2006-12-04 | 2012-09-05 | 埃尔凯姆太阳能公司 | Multicrystalline P type wafer, Phosphorus diffusion, phosphorus gettering method, and solar panel including same |
| CN100595352C (en) * | 2007-07-17 | 2010-03-24 | 佳科太阳能硅(龙岩)有限公司 | Method for preparing big ingot of polysilicon in level of solar energy |
| CN102674365A (en) * | 2012-04-23 | 2012-09-19 | 锦州新世纪石英（集团）有限公司 | Method for removing metal impurities in polycrystalline silicon |
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