CN108754614A - A kind of quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer - Google Patents
A kind of quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer Download PDFInfo
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- CN108754614A CN108754614A CN201810687268.5A CN201810687268A CN108754614A CN 108754614 A CN108754614 A CN 108754614A CN 201810687268 A CN201810687268 A CN 201810687268A CN 108754614 A CN108754614 A CN 108754614A
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- barrier layer
- crucible
- quasi
- monocrystalline silicon
- silicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/002—Crucibles or containers
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The base inner surface of the quasi-monocrystalline silicon crucible for casting ingots that the invention discloses a kind of using silica membrane as barrier layer, the crucible is equipped with silicon nitride coating and barrier layer, and the barrier layer is surface has SiO by thermal oxidation method growth2The solar level monocrystalline silicon substrate of film.The quasi-monocrystalline silicon ingot casting bottom red sector width of the quasi-monocrystalline silicon crucible for casting ingots casting using silica membrane as barrier layer provided through the invention can be restricted to about 4mm or so, and the minority carrier life time of ingot casting is more than 2 μ s；Effectively increase the utilization rate of mono-like silicon ingot.Quasi- monocrystalline ingot provided by the invention is cut into silicon chip, the impurity concentration in silicon chip is relatively low, and the minority carrier life time of silicon chip is higher, and it is higher to be made the efficiency after battery, and the transfer efficiency that is averaged is 18%~18.5%.
Description
Technical field
The invention belongs to quasi-monocrystalline silicon ingot casting fields, and in particular to a kind of using silica membrane as barrier layer
Quasi-monocrystalline silicon crucible for casting ingots.
Background technology
Solar energy as renewable and clean energy resource, because its have safe and reliable, noiseless, it is pollution-free, restrict less, failure
Advantage not available for other conventional energy resources such as rate is low, maintenance is simple, resource is wide, have been widely used generate electricity by way of merging two or more grid systems, it is civilian
Power generation, communal facility and integrated energy-saving building etc..And in field of solar thermal power generation, crystalline silicon photovoltaic electricity generation system accounts for
According to the main status in new energy photovoltaic generation market.Market to influence photovoltaic generation raw material --- the quality of mono-/multi- crystal silicon is wanted
Ask increasingly strict.
In current quasi- monocrystalline casting/polycrystalline casting process, due to meetings such as the impurity in crucible under high temperature such as iron, oxygen, carbon
Silicon ingot is diffused into, the wherein metal impurities such as iron can seriously reduce the minority carrier life time of silicon ingot, cause silicon ingot bottom to occur wider
Minority carrier life time is less than the region of 2 μ s, i.e. red sector.Wider red sector can cause the efficiency of manufactured solar cell piece significantly to drop
It is low, seriously affect the utilization rate of ingot casting.
The existing method for reducing casting mono-like silicon ingot/polycrystal silicon ingot bottom red sector width is mainly the following：1, it adopts
With high-purity crucible.2, using high purity silicon nitride silicon coating.3, using high pure raw material etc..But it reduces silicon ingot bottom red sector width
Effect all than relatively limited, and ingot casting cost is improved using high-purity material.
It is quartzy that the Chinese patent of Patent No. CN104651932B discloses a kind of polycrystalline that inner wall is equipped with quartz sand coating
Ceramic crucible carries out polycrystalline silicon ingot casting with it, can effectively reduce inside quartz ceramic crucible impurity element to expanding inside silicon ingot
It dissipates, experimental result is shown, the red sector width of polycrystalline silicon ingot casting can be down to 10mm or less.
Therefore, it is necessary to develop new coating or barrier material, silicon ingot bottom red sector width is effectively reduced, is improved accurate
The utilization rate of monocrystal silicon, and then promote the theCourse of PV Industry of monocrystalline silicon.
Invention content
Present invention aims at provide a kind of quasi-monocrystalline silicon ingot casting earthenware using silica membrane as barrier layer
Crucible, silicon ingot bottom red sector width can effectively be reduced by being used for quasi-monocrystalline silicon casting with it, improve the utilization rate of mono-like silicon ingot.
A kind of quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer, the base portion of the crucible
Inner surface is equipped with silicon nitride coating, and silicon nitride coating is equipped with barrier layer, and the barrier layer, which is surface growth, SiO2Film
Substrate.
The preparation method on the barrier layer is：SiO is grown by thermal oxidation method on substrate2Film, reactant O2；Heat
The technological parameter of oxidizing process is：Annealing temperature is 900~1100 DEG C, annealing time is 15~30min.
The substrate is solar level monocrystalline silicon piece.The purity of solar level monocrystalline silicon piece is 99.9999%, for tool
The silicon single crystal for having perfect lattice structure, almost without any impurity, using it as the substrate of barrier layer, it is ripe with depositing operation
And the advantages that not influencing ingot casting growth course.
Substrate for use of the present invention need to use after the pretreatments such as standard RCA clean, pickling, washing, drying, to remove
Substrate surface organic matter and metal impurities.Preferably, the diluted hydrofluoric acid that acid is 5~10% used in acid cleaning process.
The SiO that the present invention is prepared by thermal oxidation method2Film has the advantage that purity is high, compact structure and uniformity are good,
The SiO2The thickness of film is 10~40nm.
The barrier layer is bonded in by binder on silicon nitride coating, preferably, the binder is that silicon is molten
Glue.Further preferably high-purity silicasol.
The barrier layer is adapted with the crucible for casting ingots bottom, can flexibly be adjusted according to crucible for casting ingots bottom shape
It is whole.
The barrier layer of crucible for casting ingots bottom provided by the invention setting can effectively obstruct the impurity in ingot casting container to
It is conveyed in silicon ingot/silicon melt, reduces the red sector width of silicon ingot, the minority carrier life time of mono-like silicon ingot is provided, improve mono-like silicon ingot
Utilization rate.
It is demoulded for ease of ingot casting, one layer of silicon nitride coating, institute can be arranged before setting barrier layer in ingot casting crucible bottom again in advance
State the bottom interior surface that silicon nitride coating is coated on crucible with spraying method.
The quasi- monocrystalline ingot casting of the ingot casting crucible casting provided through the invention, bottom red sector width is low, minority carrier life time
It is high.Quasi- monocrystalline ingot provided by the invention is cut into silicon chip, the impurity concentration in silicon chip is relatively low, and the minority carrier life time of silicon chip is higher,
It is higher that the efficiency after battery is made, average transfer efficiency may be up to 18.5%.
Compared with prior art, the invention has the advantages that：
Ingot casting crucible provided by the invention is used for the casting of quasi- monocrystalline ingot casting, efficiently reduces silicon ingot bottom red sector width,
Red sector width can be restricted to about 4mm or so, and the minority carrier life time of ingot casting is more than 2 μ s；Effectively increase the utilization of mono-like silicon ingot
Rate.It is higher to be sliced the efficiency after battery is made.
Description of the drawings
Fig. 1 is the quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer in the embodiment of the present invention 1
Structural schematic diagram；
Wherein, 1 is crucible body, and 2 be silicon nitride coating, and 3 be barrier layer.
Fig. 2 is the minority carrier life time figure of mono-like silicon ingot obtained in the embodiment of the present invention 3.
Specific implementation mode
As described below is the preferred embodiment of the present invention, however the present invention is not limited thereto.For the general of this field
For logical technical staff, in the case where not departing from the principle of the present invention, various improvement and deformations can be made, these improvement and deformations
It is also considered as protection scope of the present invention.
SiO in following embodiment of the present invention2The thickness of film is obtained by following calculation formula：
Wherein, x is the oxide thickness grown, and D is the diffusion coefficient of oxidant, C0For surface oxidation agent concentration, C1
For the oxidizer molecule number in unit volume silica, surface oxidation rate constant when к is oxidation, τ in formulaIndicate that time coordinate caused by initial oxidation layer translates, d0For the thickness of initial oxidation layer, t is oxygen
Change the time.
Embodiment 1
(1) it is 175*175mm to provide internal diameter, is highly the crucible of 190mm, and one layer is sprayed in the base inner surface of crucible
Silicon nitride coating, naturally dry；
(2) one piece of thickness 0.2mm is provided, specification is the solar level monocrystalline silicon piece of 170*170mm；
(3) it is annealed at 900 DEG C 15min by thermal oxidation method on above-mentioned solar level monocrystalline silicon piece, two-sided growth two
Silica, and bottom in crucible is pasted onto by high-purity silicasol；
The SiO2The thickness of film is 10nm；
(4) and then in the crucible seed crystal is set in bottom barrier, then on seed crystal after setting silicon material, heated,
Fusing, long brilliant, annealing, cooling quasi-monocrystalline silicon ingot casting.
Facilities schematic diagram such as Fig. 1 institutes of the silicon nitride coating of crucible, barrier layer, seed crystal and silicon material in the present embodiment
It is shown.
The bottom section minority carrier life time of mono-like silicon ingot obtained by the present embodiment is more than 2 μ s, red sector width 8mm.
The average transfer efficiency that quasi- monocrystalline ingot made from the present embodiment is made to solar cell through series of processes is
18%.
Embodiment 2
(1) it is 175*175mm to provide internal diameter, is highly the crucible of 190mm, and one layer is sprayed in the base inner surface of crucible
Silicon nitride coating, naturally dry；
(2) one piece of thickness 0.2mm is provided, specification is the solar level monocrystalline silicon piece of 170*170mm；
(3) it is annealed at 900 DEG C 30min by thermal oxidation method on above-mentioned solar level monocrystalline silicon piece, two-sided growth two
Silica, and bottom in crucible is pasted onto by high-purity silicasol；
The SiO2The thickness of film is 15nm；
(4) and then in the crucible seed crystal is set in bottom barrier, then on seed crystal after setting silicon material, heated,
Fusing, long brilliant, annealing, cooling quasi-monocrystalline silicon ingot casting.
The bottom section minority carrier life time of mono-like silicon ingot obtained by the present embodiment is more than 2 μ s, red sector width 6mm.It incite somebody to action this
The average transfer efficiency that solar cell is made through series of processes for quasi- monocrystalline ingot made from embodiment is 18.2%.
Embodiment 3
(1) it is 175*175mm to provide internal diameter, is highly the crucible of 190mm, and one layer is sprayed in the base inner surface of crucible
Silicon nitride coating, naturally dry；
(2) one piece of thickness 0.2mm is provided, specification is the solar level monocrystalline silicon piece of 170*170mm；
(3) it is annealed at 1000 DEG C 30min by thermal oxidation method on above-mentioned solar level monocrystalline silicon piece, two-sided growth
Silica, and bottom in crucible is pasted onto by high-purity silicasol；
The SiO2The thickness of film is 30nm；
(4) and then in the crucible seed crystal is set in bottom barrier, then on seed crystal after setting silicon material, heated,
Fusing, long brilliant, annealing, cooling 160*160*128mm quasi-monocrystalline silicon ingot castings.
The crucible wall surrounding flaw-piece and the quasi-monocrystalline silicon ingot casting (80*80* behind polycrystalline for cutting off no barrier layer protection
Minority carrier life time figure 128mm) is as shown in Fig. 2, as shown in Figure 2, the bottom section of the mono-like silicon ingot obtained by the present embodiment is few
The sub- service life is more than 2 μ s, red sector width 4mm.
The average transfer efficiency that quasi- monocrystalline ingot made from the present embodiment is made to solar cell through series of processes is
18.5%.
Embodiment 4
(1) it is 175*175mm to provide internal diameter, is highly the crucible of 190mm, and one layer is sprayed in the base inner surface of crucible
Silicon nitride coating, naturally dry；
(2) one piece of thickness 0.2mm is provided, specification is the solar level monocrystalline silicon piece of 170*170mm；
(3) it is annealed at 1100 DEG C 15min by thermal oxidation method on above-mentioned solar level monocrystalline silicon piece, two-sided growth
Silica, and bottom in crucible is pasted onto by high-purity silicasol；
The SiO2The thickness of film is 40nm；
(4) and then in the crucible seed crystal is set in bottom barrier, then on seed crystal after setting silicon material, heated,
Fusing, long brilliant, annealing, cooling quasi-monocrystalline silicon ingot casting.
The bottom section minority carrier life time of mono-like silicon ingot obtained by the present embodiment is more than 2 μ s, red sector width 5mm.
The average transfer efficiency that quasi- monocrystalline ingot made from the present embodiment is made to solar cell through series of processes is
18.2%.
Claims (8)
1. a kind of quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer, which is characterized in that the crucible
Base portion inner surface be equipped with silicon nitride coating, silicon nitride coating be equipped with barrier layer, the barrier layer be surface growth have
SiO2The substrate of film.
2. the quasi-monocrystalline silicon crucible for casting ingots according to claim 1 using silica membrane as barrier layer, special
Sign is that the preparation method on the barrier layer is：SiO is grown by thermal oxidation method on substrate2Film, reactant O2；Hot oxygen
The technological parameter of change method is：Annealing temperature is 900~1100 DEG C, annealing time is 15~30min.
3. the quasi-monocrystalline silicon crucible for casting ingots according to claim 1 using silica membrane as barrier layer, special
Sign is, the SiO2The thickness of film is 10~40nm.
4. the quasi-monocrystalline silicon crucible for casting ingots according to claim 1 using silica membrane as barrier layer, special
Sign is that the substrate is solar level monocrystalline silicon piece.
5. the quasi-monocrystalline silicon crucible for casting ingots according to claim 1 using silica membrane as barrier layer, special
Sign is that the barrier layer is bonded in by binder on silicon nitride coating.
6. the quasi-monocrystalline silicon crucible for casting ingots according to claim 5 using silica membrane as barrier layer, special
Sign is that the binder is Ludox.
7. being used to cast the crucible of quasi-monocrystalline silicon ingot casting according to claim 1 or 5, which is characterized in that the barrier layer
It is adapted with the crucible for casting ingots bottom.
8. the quasi-monocrystalline silicon crucible for casting ingots according to claim 1 using silica membrane as barrier layer, special
Sign is that the silicon nitride coating is coated on crucible bottom inner surface with spraying method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810687268.5A CN108754614A (en) | 2018-06-28 | 2018-06-28 | A kind of quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer |
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| CN201810687268.5A CN108754614A (en) | 2018-06-28 | 2018-06-28 | A kind of quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer |
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| CN201810687268.5A Pending CN108754614A (en) | 2018-06-28 | 2018-06-28 | A kind of quasi-monocrystalline silicon crucible for casting ingots using silica membrane as barrier layer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102019206489A1 (en) * | 2019-05-06 | 2020-11-12 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method and crucible for the production of particle-free and nitrogen-free silicon ingots by means of directional solidification, silicon ingot and the use of the crucible |
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Application publication date: 20181106 |