CN101696514A - Method for producing polycrystal ingot - Google Patents
Method for producing polycrystal ingot Download PDFInfo
- Publication number
- CN101696514A CN101696514A CN200910035670A CN200910035670A CN101696514A CN 101696514 A CN101696514 A CN 101696514A CN 200910035670 A CN200910035670 A CN 200910035670A CN 200910035670 A CN200910035670 A CN 200910035670A CN 101696514 A CN101696514 A CN 101696514A
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- crucible
- barium
- salt
- coating liquid
- hydrated barta
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Abstract
The invention relates to a method for producing a polycrystal ingot, which comprises the following steps: preparing a solution of barium hydroxide or a barium salt serving as a coating solution; preheating a quartz ceramics crucible; uniformly coating the coating solution of the solution of the barium hydroxide or the barium salt on the inner surface of the preheated quartz ceramics crucible; baking the quartz ceramics crucible; spraying silicon nitride on the inner surface of the quartz ceramics crucible after baking and rotating the quartz ceramics crucible; filling a silicon material into the quartz ceramics crucible; putting the quartz ceramics crucible into a polycrystal furnace; vacuumizing the polycrystal furnace and adding a protective gas to the polycrystal furnace; heating the silicon material to smelt the silicon material; gradually crystallizing the melted silicon material from the bottom to the top by directional solidification; at last performing high temperature annealing to form the polycrystal ingot used for making a battery through slicing; slicing a crystal ingot into silicon slices; making the silicon slices into battery plates by making herbs into wool, diffusing, etching edges, PECVD filming, screen painting and sintering; and testing and grading the battery plates. The coating in the crucible prevents impurities in the crucible from diffusing to the silicon material, and improves the lifetime of minority carrier close to the crucible, the utilization rate of the crystal ingot and the battery conversion efficiency.
Description
Technical field
The present invention relates to a kind of production method of solar battery casting ingot, especially a kind of production method of polycrystalline ingot.
Background technology
Adopt the container of quartz ceramic crucible when producing the polycrystalline ingot casting at present as polycrystalline silicon ingot casting, by two warm areas or three-temperature-zone control, utilize crystal ingot thermograde up and down to realize directional freeze, adopting the alpha-silicon nitride powders coating is releasing agent, and this method is general is applied to the solar battery casting ingot industry.Monocrystalline is higher with quartz glass crucibles purity, and cost is bigger, also compares easy deformation; Polycrystalline crucible for casting ingots charging capacity is big, in order to obtain higher intensity, the quartz ceramic crucible that adopts contains a large amount of aluminium and alkaline-earth metal crystallization promoter, about 1500-2000ppmw, when ingot casting, generally at the high-purity silicon nitride of quartz ceramic crucible internal surface spraying, suppressed the reaction of silicon and quartz ceramic crucible, SiO in the industry
2+ Si=2SiO, reduced the introducing of oxygen in the silicon ingot, played demoulding effect simultaneously, but this silicon nitride layer can not effectively suppress metal impurities elemental diffusion in the quartz ceramic crucible, therefore the face foreign matter content height that contacts with quartz ceramic crucible of polycrystalline ingot, minority carrier life time is low, and this reason causes bottom flaw-piece and the crystal ingot removal amount generally up to 20-30%, therefore cause the utilization ratio of crystal ingot not high, battery efficiency also is affected.
Still unmatchful polycrystalline ingot casting quartz ceramic crucible study on the modification patent in the industry is less to the research that the diffusion of contaminants beyond the deoxygenation in the quartz ceramic crucible suppresses at present, and is more with the study on the modification of quartz glass crucibles to monocrystalline.Known have: the composition that promotes quartz crystals at single crystal quartz glass pot internal surface coating barium or aluminium etc., internal surface at crucible when pulling single crystal forms uniform quartz crystals layer, can prevent common single crystal quartz glass pot when long brilliant in the crucible release of bubble introduce impurity, cause long brilliant failure, thereby improve crystal forming rate and increase the crucible hot strength, with reference to 1997 No. 110590 communique of Japanese Patent Application Publication, 1996 No. 2932 communique of Japanese Patent Application Publication, 2002 No. 94542 communique of Japanese Patent Application Publication and Chinese patent application disclose communique 2003 No. 1448685, and the quartz glass crucibles that in the skin (bubble layer) of crucible, contains crystallization promoter, with reference to 1999 No. 171571 communique of Japanese Patent Application Publication, perhaps promotor is distributed in the quartz glass crucibles of crucible internal layer, with reference to 2003 No. 95687 communique of Japanese Patent Application Publication, perhaps contain the quartz glass crucibles of crystallization promoter, disclose communique 2008 No. 101316953 with reference to Chinese patent application in the stretched middle layer partly of crucible.
Summary of the invention
The technical problem to be solved in the present invention is: the alpha-silicon nitride powders layer can not effectively suppress metal impurities elemental diffusion problem in the quartz ceramic crucible when solving the polycrystalline ingot casting, a kind of processing of ingot casting being carried out the surface with quartz ceramic crucible is proposed, prevent diffusion of contaminants in the crucible, thus the production method of a kind of polycrystalline ingot of the efficiency of conversion of the utilization ratio of raising ingot casting and battery.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of production method of polycrystalline ingot, this production method is as follows:
(1), the solution of the salt of preparation hydrated barta or barium is as coating liquid;
(2), quartz ceramic crucible is carried out preheating;
(3), on the internal surface of the quartz ceramic crucible after the preheating, apply the coating liquid of the salt of hydrated barta or barium equably, the coating liquid of the salt of hydrated barta or barium is cured;
(4), after quartz ceramic crucible cures again within it the surface carry out the spraying and the baking of silicon nitride;
(5), with the silicon material quartz ceramic crucible of packing into, put in the polycrystalline furnace, polycrystalline furnace vacuumized and add shielding gas, with silicon material heat fused;
(6), by directional freeze, make silicon material crystallization gradually from the bottom to top of fusing, final high temperature annealing is formed for cutting into slices and does the polycrystalline ingot of battery;
(7), crystal ingot is cut into silicon chip, by making herbs into wool, diffusion, the edge etching, the PECVD plated film, silk screen printing, sintering are made the battery sheet, the test stepping.
When better solving the polycrystalline ingot casting, metal impurities elemental diffusion problem in the quartz crucible, the coated weight of the salt of inner surface of crucible hydrated barta or barium is 5 * 10
-6-3 * 10
-5Mol/cm
2The weight percent of the salt of hydrated barta or barium in solvent is 2-15% in the coating liquid of the salt of hydrated barta or barium, the temperature of coating liquid of curing the salt of hydrated barta or barium is 50-1200 ℃, the time of curing is 0.5-10h, the coating liquid solvent for use of the salt of hydrated barta or barium is for making the water or the organic solvent of the metallic compound uniform dissolution in the coating liquid, and the hydrated barta coating liquid is a solvent with 20-70 ℃ pure water.
The invention has the beneficial effects as follows, the ingot casting treatment process of quartz ceramic crucible, it is the salt type coating that on inner surface of crucible, cures a kind of hydrated barta or barium, under the high temperature, barium compound can be decomposed to form barium oxide, barium oxide and quartz crucible reaction form fine and close barium silicate, simultaneously as crystallization promoter, the crucible top layer is further changed to low-density cristobalite, make its upper layer volumetric expansion, the more smooth densification in surface, suppress the purpose of the inner impurity of crucible thereby reach to the diffusion of silicon material, and then improve the minority carrier life time at close crucible position, improve the utilization ratio and the battery conversion efficiency of crystal ingot, because coating on inner surface may cause that crucible internal layer intensity further strengthens, but needn't worry can cause the crucible distortion, because the polycrystalline ingot casting is inconsistent with the quartz glass crucibles crystalline structure with quartz ceramic crucible and monocrystalline, quartz ceramic crucible is cristobalite substantially, can not produce excessive distortion and causes splitting crucible leakage silicon.
Embodiment
A kind of production method of polycrystalline ingot, this production method is as follows:
(1), the solution of the salt of preparation hydrated barta or barium is as coating liquid;
(2), quartz ceramic crucible is carried out preheating;
(3), on the internal surface of the quartz ceramic crucible after the preheating, apply the coating liquid of the salt of hydrated barta or barium equably, the coating liquid of the salt of hydrated barta or barium is cured;
(4), after quartz ceramic crucible cures again within it the surface carry out the spraying and the baking of silicon nitride;
(5), with the silicon material quartz ceramic crucible of packing into, put in the polycrystalline furnace, polycrystalline furnace vacuumized and add shielding gas, with silicon material heat fused;
(6), by directional freeze, make silicon material crystallization gradually from the bottom to top of fusing, final high temperature annealing is formed for cutting into slices and does the polycrystalline ingot of battery;
(7), crystal ingot is cut into silicon chip, by making herbs into wool, diffusion, the edge etching, the PECVD plated film, silk screen printing, sintering are made the battery sheet, the test stepping.
When better solving the polycrystalline ingot casting, metal impurities elemental diffusion problem in the quartz crucible, the coated weight of the salt of inner surface of crucible hydrated barta or barium is 5 * 10
-6-3 * 10
-5Mol/cm
2The weight percent of the salt of hydrated barta or barium in solvent is 2-15% in the coating liquid of the salt of hydrated barta or barium, the temperature of coating liquid of curing the salt of hydrated barta or barium is 50-1200 ℃, the time of curing is 0.5-10h, the coating liquid solvent for use of the salt of hydrated barta or barium is for making the water or the organic solvent of the metallic compound uniform dissolution in the coating liquid, in the hydrated barta coating liquid, be solvent with 20-70 ℃ pure water.
Its core is, the ingot casting treatment process of quartz ceramic crucible, be on inner surface of crucible, to cure a kind of barium metal compound coat, at high temperature, barium compound can be decomposed to form barium oxide, along with barium oxide and quartz crucible reaction form fine and close barium silicate, simultaneously as crystallization promoter, the crucible top layer is further changed to low-density cristobalite, make its upper layer volumetric expansion, the more smooth densification in surface suppresses the purpose of the inner impurity of crucible to the diffusion of silicon material thereby reach, and then improve the minority carrier life time at close crucible position, improve the utilization ratio and the battery conversion efficiency of crystal ingot.The segregation coefficient of barium is very little, be better than other metallic promoter agent such as calcium, magnesium, simultaneously because the iris action of silicon nitride between crucible and silicon material, barium can not be diffused in the silicon material substantially, therefore very effective to the diffusion that suppresses impurity in the crucible, particularly evident through detecting discovery to the restraining effect of iron, SiO
2-BaO-Fe
2O
3System at high temperature can generate BaSiO
3And BaFe
12O
19
When adopting hydrated barta to be coated material, the chemical reaction that takes place in its process has:
Ba(OH)
2+CO
2→BaCO
3+H
2O
BaCO
3→ BaO+CO
2(gas, following 1450 ℃ of high temperature)
BaCO
3+SiO
2→BaSiO
3+CO
2
BaO+SiO
2→BaSiO
3
3BaO+2Al→Al
2O
3+3Ba，
The quartz ceramic crucible coating that obtains is cured at crucible surface, it is adherent more intense, the crucible that effect is better than not curing, coating is by the salt of adhesiving metal compound such as hydrated barta or barium, and at high temperature cure and decompose this solution and form, metallic compound is preferably barium hydroxide octahydrate, the preferred 20-70 of solvent ℃ pure water, stir appropriate time and fully dissolve, the coated weight of the hydrated barta of inner surface of crucible or the salt of barium is 5 * 10
-6-3 * 10
-5Mol/cm
2The weight percent of the salt of hydrated barta or barium in solvent is that 2-15% is suitable in the coating liquid of the salt of hydrated barta or barium, content calculates with the amount of metallic compound, but coated weight is higher than or be not preferred when being lower than described scope, because coated weight suppresses the DeGrain to the diffusion of silicon liquid of impurity in the crucible very little, the too many crucible of coated weight and alpha-silicon nitride powders layer bonding is not firm easily comes off.
The utilization ratio of crystal ingot is standard with the minority carrier life time, in order to obtain higher crystal ingot utilization ratio, need do coating in the total inner surface of crucible, perhaps selectively do coating in the inwall part that the silicon material contacts with crucible, the method that applies can make spraying, dip-coating, brushing etc., but is not limited to these methods.After coating applied, the temperature and time that cures was by used metallic compound and solvent decision, and it is preferred curing described coating liquid 0.5-10h under 50-1200 ℃.
The present invention will describe by embodiment, but embodiment is not as to further restriction of the present invention.The crucible sample that present embodiment adopts is 845 * 845 * 420mm
3Quartz ceramic crucible, the barium coating is handled and non-coating is handled each one, charge amount 200-450kg silicon material uses brilliant technology of same length and battery production technology, finally compares the yield of the crystal ingot of producing and the transformation efficiency of battery effect of the present invention is described.
Quartz ceramic crucible adopts the barium compounds aqueous solution to do coating liquid, coating liquid concentration 2-10%, crucible is preheating to 50-70 ℃ and sprays before coating, coating liquid evenly is coated on the internal surface of crucible, cures described coating liquid 0.5-10h under 50-1200 ℃.
Embodiment A is to make the crucible of barium coating, and Comparative Examples B is the non-crucible that is coated with, and is the crucible of only doing common alpha-silicon nitride powders coating.The crystal ingot yield that employing barium is coated with crucible is apparently higher than conventional crystal ingot, and the minority carrier life time of crystal ingot afterbody obviously improves, and battery conversion efficiency improves 0.1-0.2%.From the detected result of silicon chip, barium is from the crucible surface stripping, to the silicon material without any influence.Impurity when the present invention adopts crucible to do the barium coating can effectively to suppress ingot casting in the crucible spreads to the silicon material.
Annotate: the coated weight of Ba coating is with BaSiO
3Thickness characterizes; The Ba/Fe detection method of content is ICPMS, and＜DL refers to be lower than below the detectability ppbw.
Among the embodiment, to cure 30 minutes at least under 800 ℃ the temperature be preferred to shown barium hydroxide octahydrate coating being higher than.The alpha-silicon nitride powders coating of too short then follow-up spraying of the time of curing adheres to not firm easily, if the alpha-silicon nitride powders coating adheres to the not firm silicon liquid of then falling into easily, crucible and silicon liquid react and cause the introducing of oxygen, cause finally the effectively demoulding simultaneously and split ingot, influence the utilization ratio of crystal ingot on the contrary, and the introducing of silicon nitride and oxygen can influence the crystal ingot quality.Because coating on inner surface may cause that crucible internal layer intensity further strengthens, but needn't worry can cause the crucible distortion, because the polycrystalline ingot casting is inconsistent with the quartz glass crucibles crystalline structure with quartz ceramic crucible and monocrystalline, quartz ceramic crucible is cristobalite substantially, can not produce excessive distortion and causes splitting crucible and leak silicon.
Claims (7)
1. the production method of a polycrystalline ingot, this production method is as follows:
(1), the solution of the salt of preparation hydrated barta or barium is as coating liquid;
(2), quartz ceramic crucible is carried out preheating;
(3), on the internal surface of the quartz ceramic crucible after the preheating, apply the coating liquid of the salt of hydrated barta or barium equably, the coating liquid of the salt of hydrated barta or barium is cured;
(4), after quartz ceramic crucible cures again within it the surface carry out the spraying and the baking of silicon nitride;
(5), with the silicon material quartz ceramic crucible of packing into, put in the polycrystalline furnace, polycrystalline furnace vacuumized and add shielding gas, with silicon material heat fused;
(6), by directional freeze, make silicon material crystallization gradually from the bottom to top of fusing, final high temperature annealing is formed for cutting into slices and does the polycrystalline ingot of battery;
(7), crystal ingot is cut into silicon chip, by making herbs into wool, diffusion, the edge etching, the PECVD plated film, silk screen printing, sintering are made the battery sheet, the test stepping.
2. the production method of a kind of polycrystalline ingot according to claim 1, it is characterized in that: the coated weight of the salt of described inner surface of crucible hydrated barta or barium is 5 * 10
-6-3 * 10
-5Mol/cm
2
3. the production method of a kind of polycrystalline ingot according to claim 2, it is characterized in that: the weight percent of the salt of hydrated barta or barium in solvent is 2-15% in the coating liquid of the salt of described hydrated barta or barium.
4. the production method of a kind of polycrystalline ingot according to claim 1, it is characterized in that: described quartz-ceramics preheating temperature is 30-100 ℃.
5. the production method of a kind of polycrystalline ingot according to claim 1 is characterized in that: the temperature of the coating liquid of the described salt that cures hydrated barta or barium is 50-1200 ℃, and the time of curing is 0.5-10h.
6. the production method of a kind of polycrystalline ingot according to claim 1 is characterized in that: the coating liquid solvent for use of the salt of described hydrated barta or barium is for making the water or the organic solvent of the metallic compound uniform dissolution in the coating liquid.
7. the production method of a kind of polycrystalline ingot according to claim 6, it is characterized in that: described hydrated barta coating liquid is a solvent with 20-70 ℃ pure water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910035670A CN101696514A (en) | 2009-09-30 | 2009-09-30 | Method for producing polycrystal ingot |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910035670A CN101696514A (en) | 2009-09-30 | 2009-09-30 | Method for producing polycrystal ingot |
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| Publication Number | Publication Date |
|---|---|
| CN101696514A true CN101696514A (en) | 2010-04-21 |
Family
ID=42141638
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|---|---|---|---|
| CN200910035670A Pending CN101696514A (en) | 2009-09-30 | 2009-09-30 | Method for producing polycrystal ingot |
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| CN102260902A (en) * | 2011-07-15 | 2011-11-30 | 江苏晶鼎电子材料有限公司 | Method for preparing quartz crucible coating |
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| CN108796617A (en) * | 2017-04-28 | 2018-11-13 | 友达晶材股份有限公司 | Crucible structure and manufacturing method thereof, and silicon crystal structure and manufacturing method thereof |
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