CN103484935A - Quartz crucible and manufacturing method thereof - Google Patents
Quartz crucible and manufacturing method thereof Download PDFInfo
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- CN103484935A CN103484935A CN201310421585.XA CN201310421585A CN103484935A CN 103484935 A CN103484935 A CN 103484935A CN 201310421585 A CN201310421585 A CN 201310421585A CN 103484935 A CN103484935 A CN 103484935A
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- quartz crucible
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Abstract
The invention discloses a quartz crucible and a manufacturing method of the quartz crucible. A glass sand coating coats the inner surface of a common quartz crucible body and plays a role in shielding between the common quartz crucible body and polycrystalline silicon ingot crystals, the speed of metal impurities diffusing toward the polycrystalline silicon ingot crystals in the common quartz crucible body is reduced, then the content of the metal impurities in the polycrystalline silicon ingot crystals is reduced, and therefore the purpose of improving service life of a non-equilibrium minority carrier is achieved. On the basis of the manufacturing method, the number of unqualified parts of the bottom surface and the side faces in the manufactured qualified polycrystalline silicon ingot crystals is reduced, the usage rate is improved, and production cost is reduced.
Description
Technical field
The present invention relates to the solar silicon wafers field, especially for the splendid attire polycrystal silicon ingot, use quartz crucible and manufacture method thereof.
Background technology
Crystal silicon solar energy battery is on the base material of crystal silicon chip, the new-generation material formed by making the series of process such as PN junction, and wherein crystal silicon chip is the base mateiral of solar cell.According to the difference of internal crystal structure, crystal silicon chip is divided into polysilicon chip and monocrystalline silicon piece, and they are respectively to be formed by polycrystal silicon ingot crystal and silicon single crystal ingot crystal-cut.
Wherein the polycrystal silicon ingot crystal forms after being fired in polycrystalline ingot furnace: the internal surface of specifically polycrystalline silicon raw material being packed into scribbles in the quartz crucible of silicon nitride powder releasing agent, then quartz crucible is placed in polycrystalline ingot furnace, by heating, fusing, long brilliant, annealing and a series of processes such as cooling, obtains satisfactory polycrystal silicon ingot crystal.
Present stage, the battery conversion efficiency that improves polycrystal silicon cell is one of R&D direction main in industry, and the inner quality of polysilicon chip has a direct impact the efficiency of conversion of final battery.In the polycrystal silicon ingot crystal, metallic impurity are coincidence centers of non-equilibrium minority carrier, especially iron and aluminium etc. are the strong coincidence centers of non-equilibrium minority carrier, can reduce the life-span of non-equilibrium minority carrier, be reflected to that to using on its solar cell be made into as matrix be that solar energy converting becomes the efficiency of conversion of electric energy on the low side.
The formation of metallic impurity is that the manufacturing process due to the polycrystal silicon ingot crystal causes, and the inner quality of polysilicon chip depends on the quality of the polycrystal silicon ingot crystal before its excision forming.In polycrystalline cast ingot crystals, non-equilibrium minority carrier lifetime part on the low side can be divided into two zones by reason: a kind of is because the fusing of polycrystal silicon ingot crystal and long brilliant process are all to carry out in quartz crucible, and the purity of quartz crucible is lower with respect to the silicon material of polycrystal silicon ingot crystal, the part that the metallic impurity in quartz crucible at high temperature cause quartz crucible contact with the polycrystal silicon ingot plane of crystal to the diffusion of the silicon material of polycrystal silicon ingot crystal have many metallic impurity rich amass regional; Another kind is because the metallic impurity in the silicon material of polycrystal silicon ingot crystal are gathered in by the effect of segregation the rich long-pending zone of metallic impurity that the part of final set forms.The rich long-pending zone of the metallic impurity that form for the first reason is now concrete: the part 1) contacted with the quartz crucible bottom surface in polycrystal silicon ingot crystal bottom has higher metallic impurity Fu Ji district.For this part, can remove defective part by detecting non-equilibrium minority carrier lifetime actual value.2) part in polycrystal silicon ingot side and quartz crucible contacts side surfaces also has higher metallic impurity Fu Ji district, for this part, way conventional in industry is to remove the certain thickness flaw-piece in its side after the moulding of polycrystal silicon ingot crystal, but the method still can be stayed a part of metallic impurity in qualified polycrystal silicon ingot crystal, cause final crystal silicon chip " black surround " phenomenon to occur, when PL detects, obfuscation, be also that this part of efficiency of conversion is on the low side.Above-mentioned two kinds of removal methods all do not have from reducing in essence the rich long-pending zone of metallic impurity, and be only to have produced behind the rich long-pending zone of metallic impurity later stage remedial measures artificially, reduce the rate of utilization of polycrystalline cast ingot crystals significant part, and then affected the cost that polysilicon chip is manufactured.
Summary of the invention
The technical problem solved: for the deficiencies in the prior art, the invention provides a kind of quartz crucible and manufacture method thereof, solve the surface that can contact with quartz crucible at the polycrystal silicon ingot crystal when the common quartz crucible that utilizes existing suitability for industrialized production is directly made the polycrystal silicon ingot crystal and form the rich long-pending regional technical problem of metallic impurity.
Technical scheme: for solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of quartz crucible, comprise common quartz crucible body, the internal surface of described common quartz crucible body scribble quartz sand purity be greater than 99.99% and concentration of iron lower than the glass sand coating of 3PPM.
A kind of manufacture method of quartz crucible comprises the following steps of carrying out in turn:
Step 1: be greater than 99.99% in quartz sand purity, concentration of iron is to add the pure water of its 3～5 times of weight to carry out fully stirring in 300-600 purpose molten state glass sand to form slurries lower than 3PPM and particle diameter, churning time is greater than 24 hours, and notes keeping clean not bringing impurity into;
Step 2: by the standing 2-10 minute of the slurries that are stirred in step 1, after the quartz sand precipitated and separated, remove supernatant liquid, stay the dense thick slurries of quartz sand;
Step 3: the dense thick slurry volume 1-3 electronic-grade silica sol doubly to pouring quartz sand in the dense thick slurries of quartz sand in step 2 into, fully stir 10-60 minute;
Step 4: by the mode of brushing, round brush or spraying, the slurries that obtain in step 3 are evenly spread upon on the internal surface of common quartz crucible body, thickness is the 0.1-0.5 millimeter;
Step 5: the quartz crucible after making in step 4 is put into to sintering oven, and design temperature is 200-300 degree centigrade, sintering 1～3 hour;
Step 6: the glass sand coating after the inspection sintering, if be extremely salable product without be full of cracks, bubble etc.
As preferably, in the present invention, in described step 4, the smearing thickness of slurries is 0.15 millimeter.Experiment showed, and both met the purpose of complete isolating metal impurity when thickness is 0.15 millimeter, can not cause the glass sand coating in use to come off because coating is too thick again.
Beneficial effect:
The quartz crucible that the present invention makes, apply one deck glass sand coating in common quartz crucible body internal surface, play certain shielding effect between common quartz crucible body and polycrystal silicon ingot crystal, reduce the speed that the metallic impurity in common quartz crucible body spread to polycrystalline cast ingot crystals, and then reach metals content impurity in the reduction polycrystalline cast ingot crystals, thereby improve the purpose of non-equilibrium minority carrier lifetime.
Concrete, on the one hand, non-equilibrium minority carrier lifetime part on the low side in polycrystal silicon ingot crystal bottom can obviously reduce, it is the 10mm left and right that produced single polysilicon ingot crystal can reduce defective length, also can be each polycrystal silicon ingot crystal increases the part used of 14KG, the polycrystal silicon ingot crystal that is 500KG for every weight, also improved 2.8% In-commission Rate.
On the other hand, the non-equilibrium minority carrier lifetime of polycrystal silicon ingot crystal on side face also obviously reduces than lower part, can obviously improve the crystal mass of polycrystal silicon ingot crystal on side face, reduces " black surround " ratio on final crystal silicon chip, improves whole efficiency of conversion.
The accompanying drawing explanation
Non-equilibrium minority carrier lifetime test curve in the polycrystal silicon ingot crystal that Fig. 1 is quartz crucible manufacture of the present invention;
Non-equilibrium minority carrier lifetime test curve in the polycrystal silicon ingot crystal that Fig. 2 is common quartz crucible manufacture.
Embodiment
Get common quartz crucible that Traditional Industrialization produces as manufacturing common quartz crucible body of the present invention, within it surface scribble quartz sand purity be greater than 99.99% and concentration of iron lower than the glass sand coating of 3PPM.
Concrete manufacturing step is: order is carried out following steps and is manufactured quartz crucible of the present invention:
Step 1: be greater than 99.99% in quartz sand purity, concentration of iron is to add the pure water of its 4 times of weight to carry out fully stirring in 300-600 purpose molten state glass sand to form slurries lower than 3PPM and particle diameter, churning time is greater than 24 hours, and noting keeps clean does not bring impurity into, otherwise can affect the quality of the complete rear glass sand coating of sintering.
Step 2: by standing 8 minutes of the slurries that are stirred in step 1, after the quartz sand precipitated and separated, remove supernatant liquid, stay the dense thick slurries of quartz sand.
Step 3: the dense thick slurry volume 1-3 electronic-grade silica sol doubly to pouring quartz sand in the dense thick slurries of quartz sand in step 2 into, fully stir 45 minutes; This step can fully merge electronic-grade silica sol and the dense thick slurries of quartz sand of 1-3 times, while making the later stage smear, can closely adhere to meticulously the internal surface of quartz crucible body.
Step 4: by the mode of brushing, round brush or spraying, the slurries that obtain in step 3 are evenly spread upon on the internal surface of quartz crucible body, thickness is 0.15 millimeter.Experiment showed, and both met the purpose of complete isolating metal impurity when thickness is 0.15 millimeter, can not cause the glass sand coating in use to come off because coating is too thick again.
Step 5: the quartz crucible after making in step 4 is put into to sintering oven, and design temperature is 250 degrees centigrade, sintering 2.5 hours;
Step 6: the glass sand coating after the inspection sintering, if be extremely salable product without be full of cracks, bubble etc.
The quartz crucible using method that after sintering completes, qualified quartz crucible is produced with Traditional Industrialization is the same, as broad as long.
Get quartz crucible of the present invention and common quartz crucible is manufactured respectively the polycrystal silicon ingot crystal, and to test these two kinds be the life-span of the non-equilibrium minority carrier in bottom in the produced polycrystal silicon ingot crystal of quartz crucible, obtain respectively curve as depicted in figs. 1 and 2, in figure, the left side of curve means the life situations of the non-equilibrium minority carrier in bottom of polycrystal silicon ingot crystal.
For life-span of non-equilibrium minority carrier, lower than the polycrystal silicon ingot crystal block section of 3 microseconds, be judged to be defectively, the qualified part of the bottom of the larger expression polycrystal silicon ingot of the absolute value crystal of the transverse axis numerical value on the curve left side that 3 microseconds of the longitudinal axis are corresponding is more.In Fig. 1, the point on the curve left side corresponding to 3 microseconds is-120mm, and in Fig. 2, the point on the curve left side corresponding to 3 microseconds is-108mm.The produced polycrystal silicon ingot crystal of visible quartz crucible of the present invention can increase the qualified part of 12mm with respect to the bottom of the produced polycrystal silicon ingot crystal of common quartz crucible.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (3)
1. a quartz crucible is characterized in that: comprise common quartz crucible body, the internal surface of described common quartz crucible body scribble quartz sand purity be greater than 99.99% and concentration of iron lower than the glass sand coating of 3PPM.
2. the manufacture method of a kind of quartz crucible according to claim 1 is characterized in that: comprise the following steps of carrying out in turn:
Step 1: be greater than 99.99% in quartz sand purity, concentration of iron is to add the pure water of its 3～5 times of weight to carry out fully stirring in 300-600 purpose molten state glass sand to form slurries lower than 3PPM and particle diameter, churning time is greater than 24 hours, and notes keeping clean not bringing impurity into;
Step 2: by the standing 2-10 minute of the slurries that are stirred in step 1, after the quartz sand precipitated and separated, remove supernatant liquid, stay the dense thick slurries of quartz sand;
Step 3: the dense thick slurry volume 1-3 electronic-grade silica sol doubly to pouring quartz sand in the dense thick slurries of quartz sand in step 2 into, fully stir 10-60 minute;
Step 4: by the mode of brushing, round brush or spraying, the slurries that obtain in step 3 are evenly spread upon on the internal surface of common quartz crucible body, thickness is the 0.1-0.5 millimeter;
Step 5: the quartz crucible after making in step 4 is put into to sintering oven, and design temperature is 200-300 degree centigrade, sintering 1～3 hour;
Step 6: the glass sand coating after the inspection sintering, if be extremely salable product without be full of cracks, bubble etc.
3. the manufacture method of a kind of quartz crucible according to claim 2, it is characterized in that: in described step 4, the smearing thickness of slurries is 0.15 millimeter.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104018219A (en) * | 2014-06-17 | 2014-09-03 | 镇江环太硅科技有限公司 | Preparation method of high-efficiency polycrystalline silicon chip with narrow black edge |
| CN104032368A (en) * | 2014-05-05 | 2014-09-10 | 镇江环太硅科技有限公司 | Preparation method of high-efficiency polycrystalline silicon ingots |
| CN104328490A (en) * | 2014-11-07 | 2015-02-04 | 江苏美科硅能源有限公司 | Preparation method of black-edge-free high-efficiency polycrystalline silicon ingot |
| CN104651932A (en) * | 2015-03-17 | 2015-05-27 | 江西中昱新材料科技有限公司 | Polycrystalline quartz ceramic crucible and preparation method thereof |
| CN105648528A (en) * | 2016-03-15 | 2016-06-08 | 常熟华融太阳能新型材料有限公司 | Novel high-purity quartz crucible and preparation method thereof |
| CN106278302A (en) * | 2016-07-22 | 2017-01-04 | 常州天合光能有限公司 | A kind of preparation technology of the high-purity fused silica crucible of gradient |
| CN107299392A (en) * | 2017-07-12 | 2017-10-27 | 晶科能源有限公司 | A kind of high fine and close silica crucible barrier layer preparation method and polycrystalline ingot furnace |
| CN107326445A (en) * | 2017-07-24 | 2017-11-07 | 宜昌南玻硅材料有限公司 | A kind of method for changing crucible structure to improve ingot quality |
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| CN102080256A (en) * | 2011-03-02 | 2011-06-01 | 镇江荣德新能源科技有限公司 | Quartz crucible |
| CN102409405A (en) * | 2011-08-23 | 2012-04-11 | 周浪 | Carbon pollution prevention coating of carbon material for polycrystalline silicon ingot furnace and preparation process thereof |
| CN202913087U (en) * | 2012-10-30 | 2013-05-01 | 烟台核晶陶瓷新材料有限公司 | Ceramic crucible for polycrystalline silicon ingot |
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| CN102080256A (en) * | 2011-03-02 | 2011-06-01 | 镇江荣德新能源科技有限公司 | Quartz crucible |
| CN102409405A (en) * | 2011-08-23 | 2012-04-11 | 周浪 | Carbon pollution prevention coating of carbon material for polycrystalline silicon ingot furnace and preparation process thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104032368A (en) * | 2014-05-05 | 2014-09-10 | 镇江环太硅科技有限公司 | Preparation method of high-efficiency polycrystalline silicon ingots |
| CN104032368B (en) * | 2014-05-05 | 2016-05-25 | 镇江环太硅科技有限公司 | A kind of preparation method of efficient polycrystal silicon ingot |
| CN104018219A (en) * | 2014-06-17 | 2014-09-03 | 镇江环太硅科技有限公司 | Preparation method of high-efficiency polycrystalline silicon chip with narrow black edge |
| CN104018219B (en) * | 2014-06-17 | 2016-08-24 | 镇江环太硅科技有限公司 | A kind of preparation method of narrow black surround high-efficiency polycrystalline silicon chip |
| CN104328490A (en) * | 2014-11-07 | 2015-02-04 | 江苏美科硅能源有限公司 | Preparation method of black-edge-free high-efficiency polycrystalline silicon ingot |
| CN104651932A (en) * | 2015-03-17 | 2015-05-27 | 江西中昱新材料科技有限公司 | Polycrystalline quartz ceramic crucible and preparation method thereof |
| CN105648528A (en) * | 2016-03-15 | 2016-06-08 | 常熟华融太阳能新型材料有限公司 | Novel high-purity quartz crucible and preparation method thereof |
| CN106278302A (en) * | 2016-07-22 | 2017-01-04 | 常州天合光能有限公司 | A kind of preparation technology of the high-purity fused silica crucible of gradient |
| CN106278302B (en) * | 2016-07-22 | 2019-01-04 | 天合光能股份有限公司 | Preparation process of gradient high-purity fused quartz crucible |
| CN107299392A (en) * | 2017-07-12 | 2017-10-27 | 晶科能源有限公司 | A kind of high fine and close silica crucible barrier layer preparation method and polycrystalline ingot furnace |
| CN107326445A (en) * | 2017-07-24 | 2017-11-07 | 宜昌南玻硅材料有限公司 | A kind of method for changing crucible structure to improve ingot quality |
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Application publication date: 20140101 |