CN104152989A - Polycrystalline-silicon high-efficiency silicon ingot seeding plate and preparation method thereof - Google Patents

Polycrystalline-silicon high-efficiency silicon ingot seeding plate and preparation method thereof Download PDF

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Publication number
CN104152989A
CN104152989A CN201410455986.1A CN201410455986A CN104152989A CN 104152989 A CN104152989 A CN 104152989A CN 201410455986 A CN201410455986 A CN 201410455986A CN 104152989 A CN104152989 A CN 104152989A
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silicon
seeding
particle
plate core
seeding plate
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CN201410455986.1A
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Inventor
张军彦
侯炜强
吴洪坤
杜海文
陈国红
张瑾
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SHANXI BRANCH OF NEW ENERGY Co
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SHANXI BRANCH OF NEW ENERGY Co
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Abstract

The invention discloses a polycrystalline-silicon high-efficiency silicon ingot seeding plate and a preparation method thereof and solves the problem that an existing silicon crystal self-nucleation seeding plate is easy to cause nonuniform nucleation and low in crystal nucleus quality. The polycrystalline-silicon high-efficiency silicon ingot seeding plate comprises a seeding plate core (1) with a silicon purity of over 99.99999%; the seeding plate core (1) is of a square shape with a side length of 125 mm or 156 mm; a silicon carbide crushed particle or silicon nitride crushed particle adhesion coating (2) is adhered to the outer surface of the seeding plate core (1); the particle size of silicon carbide crushed particles or silicon nitride crushed particles in the adhesion coating (2) is smaller than or equal to 0.003 mm. The selected silicon carbide crushed particles are placed into a stirrer together with pure water and an adhesive to be stirred for 15 to 20 minutes so as to prepare silicon crushed particle pasty suspension with a density of over 2.33 g per cubic centimeter and the seeding plate core (1) is placed into the suspension to be coated and then is baked and cooled. The polycrystalline-silicon high-efficiency silicon ingot seeding plate is particularly suitable for the production process of producing a polycrystalline-silicon high-efficiency silicon ingot in a crucible.

Description

The efficient silicon ingot seeding of polysilicon plate and preparation method thereof
Technical field
The present invention relates to the seeding plate of the efficient silicon ingot of a kind of polysilicon, particularly seeding plate of a kind of efficient silicon ingot of polysilicon using in high efficient crucible and preparation method thereof, is applicable to photovoltaic industry casting ingot process link.
Background technology
The front end of polycrystalline silicon casting ingot process link in photovoltaic industry industrial chain, plays conclusive effect to production links such as follow-up silicon chip, cell pieces.Polycrystalline silicon ingot casting is generally the method that adopts directional freeze, by electrically heated, the silicon material being loaded in quartz crucible is melted, and recycles certain processing method and starts forming core, long brilliant from crucible bottom, the final polycrystal silicon ingot meeting the demands that forms.At present, the forming core method of efficient silicon ingot mainly contains two kinds, first method is to utilize the unfused silicon material that is laid on crucible bottom to carry out forming core, with silicon crystal spontaneous nucleation seeding particle, carry out forming core, the definite of not melted silicon material height who lays in crucible bottom is to depend on manual operation, have the poor shortcoming of consistence, silicon ingot is must material rate low, and cost is high; Second method is to utilize the polymorphic structure of crucible bottom to carry out forming core, and crucible bottom polymorphic structure easily causes the sticky crucible in bottom, and has the problem of returns subsequent disposal difficulty.
Summary of the invention
The invention provides the efficient silicon ingot seeding of a kind of polysilicon plate and preparation method thereof, solved existing silicon crystal spontaneous nucleation seeding particle and easily caused heterogeneous nucleation and the low technical problem of nucleus quality.
The present invention solves above technical problem by the following technical programs:
The efficient silicon ingot seeding of a kind of polysilicon plate; comprise the seeding plate core that silicon purity is greater than 99.99999%; seeding plate core is that the length of side is the square plate core that the square plate core of 125 millimeters or the length of side are 156 millimeters; on the outside surface of seeding plate core, be bonded with the bonding coating layer of silicon carbide particle or silicon nitride particle, the silicon carbide particle in bonding coating layer or the particle diameter of silicon nitride particle are less than or equal to 0.003 millimeter.
The volume of seeding plate core is 1:2-1:5 with the ratio of the volume of bonding coating layer.
A preparation method for the efficient silicon ingot seeding of polysilicon plate, comprises the following steps:
The first step, choose silicon purity be greater than 99.99999% the length of side be 125 millimeters or the length of side be 156 millimeters seeding plate core;
Second step, choose the silicon carbide particle that particle diameter is less than or equal to 0.003 millimeter;
The 3rd step, choose resistivity and be greater than the pure water of 18M Ω .cm and metal content lower than the tackiness agent of 30ppma;
Together with the pure water that the 4th step, the silicon carbide particle that second step is chosen are chosen with the 3rd step and tackiness agent, put in agitator and stir 15-20 minute, make the silicon carbide particle pasty state suspension liquid that density is greater than 2.33 grams/cubic centimeter;
The 5th step, the seeding plate core that the first step is chosen are put in the silicon carbide particle pasty state suspension liquid that the 4th step obtains and are soaked 2-5 minute;
The 6th step, seeding plate core the 5th step is soaked and that be coated with silicon carbide particle pasty state suspension layers are placed in argon gas atmosphere, dry to burn to make its temperature reach 150-200 ℃, and keep 10-30 minute; Then make it in argon gas atmosphere, naturally cool to room temperature;
The 7th step, choose the finished product that the ratio of the volume of seeding plate core and the volume of bonding coating layer is 1:2-1:5, obtain the efficient silicon ingot seeding of polysilicon plate.
A preparation method for the efficient silicon ingot seeding of polysilicon plate, comprises the following steps:
The first step, choose silicon purity be greater than 99.99999% the length of side be 125 millimeters or the length of side be 156 millimeters seeding plate core;
Second step, choose the silicon nitride particle that particle diameter is less than or equal to 0.003 millimeter;
The 3rd step, choose resistivity and be greater than the pure water of 18M Ω .cm and metal content lower than the tackiness agent of 30ppma;
Together with the pure water that the 4th step, the silicon nitride particle that second step is chosen are chosen with the 3rd step and tackiness agent, put in agitator and stir 15-20 minute, make the silicon nitride particle pasty state suspension liquid that density is greater than 2.33 grams/cubic centimeter;
The 5th step, the seeding plate core that the first step is chosen are put in the silicon nitride particle pasty state suspension liquid that the 4th step obtains and are soaked 2-5 minute;
The 6th step, seeding plate core the 5th step is soaked and that be coated with silicon nitride particle pasty state suspension layers are placed in argon gas atmosphere, dry to burn to make its temperature reach 150-200 ℃, and keep 10-30 minute; Then make it in argon gas atmosphere, naturally cool to room temperature;
The 7th step, choose the finished product that the ratio of the volume of seeding plate core and the volume of bonding coating layer is 1:2-1:5, obtain the efficient silicon ingot seeding of polysilicon plate.
Seeding plate of the present invention provides controlled nucleating center for the non-spontaneous nucleation of silicon crystal, and guides the heterogeneous nucleation of silicon crystal, reaches the effect that produces good uniformity and the high high-quality nucleus of consistence, for the production of follow-up high-quality cell piece lays the foundation.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail:
The efficient silicon ingot seeding of a kind of polysilicon particle; comprise the seeding plate core 1 that silicon purity is greater than 99.99999%; seeding plate core 1 is that the length of side is the square plate core that the square plate core of 125 millimeters or the length of side are 156 millimeters; on the outside surface of seeding plate core 1, be bonded with the bonding coating layer 2 of silicon carbide particle or silicon nitride particle, the silicon carbide particle in bonding coating layer 2 or the particle diameter of silicon nitride particle are less than or equal to 0.003 millimeter.
The volume of seeding plate core 1 is 1:2-1:5 with the ratio of the volume of bonding coating layer 2.Also laminated coating layer can be set.
A preparation method for the efficient silicon ingot seeding of polysilicon plate, comprises the following steps:
The first step, choose silicon purity be greater than 99.99999% the length of side be 125 millimeters or the length of side be 156 millimeters seeding plate core 1;
Second step, choose the silicon carbide particle that particle diameter is less than or equal to 0.003 millimeter;
The 3rd step, choose resistivity and be greater than the pure water of 18M Ω .cm and metal content lower than the tackiness agent of 30ppma;
Together with the pure water that the 4th step, the silicon carbide particle that second step is chosen are chosen with the 3rd step and tackiness agent, put in agitator and stir 15-20 minute, make the silicon carbide particle pasty state suspension liquid that density is greater than 2.33 grams/cubic centimeter;
The 5th step, the seeding plate core 1 that the first step is chosen are put in the silicon carbide particle pasty state suspension liquid that the 4th step obtains and are soaked 2-5 minute;
The 6th step, seeding plate core 1 the 5th step is soaked and that be coated with silicon carbide particle pasty state suspension layers are placed in argon gas atmosphere, dry to burn to make its temperature reach 150-200 ℃, and keep 10-30 minute; Then make it in argon gas atmosphere, naturally cool to room temperature;
The 7th step, choose the finished product that the ratio of the volume of seeding plate core 1 and the volume of bonding coating layer 2 is 1:2-1:5, obtain the efficient silicon ingot seeding of polysilicon plate.
A preparation method for the efficient silicon ingot seeding of polysilicon plate, comprises the following steps:
The first step, choose silicon purity be greater than 99.99999% the length of side be 125 millimeters or the length of side be 156 millimeters seeding plate core 1;
Second step, choose the silicon nitride particle that particle diameter is less than or equal to 0.003 millimeter;
The 3rd step, choose resistivity and be greater than the pure water of 18M Ω .cm and metal content lower than the tackiness agent of 30ppma;
Together with the pure water that the 4th step, the silicon nitride particle that second step is chosen are chosen with the 3rd step and tackiness agent, put in agitator and stir 15-20 minute, make the silicon nitride particle pasty state suspension liquid that density is greater than 2.33 grams/cubic centimeter;
The 5th step, the seeding plate core 1 that the first step is chosen are put in the silicon nitride particle pasty state suspension liquid that the 4th step obtains and are soaked 2-5 minute;
The 6th step, seeding particle cores 1 the 5th step is soaked and that be coated with silicon nitride particle pasty state suspension layers are placed in argon gas atmosphere, dry to burn to make its temperature reach 150-200 ℃, and keep 10-30 minute; Then make it in argon gas atmosphere, naturally cool to room temperature;
The 7th step, choose the finished product that the ratio of the volume of seeding plate core 1 and the volume of bonding coating layer 2 is 1:2-1:5, obtain the efficient silicon ingot seeding of polysilicon plate.
Silicon carbide particle in bonding coating layer 2 involved in the present invention or the particle diameter of silicon nitride particle are less than or equal to 0.003 millimeter; also can select the identical with crystalline silicon lattice parameter or close of other; and fusing point is higher than 1430 degrees Celsius, the particle that density is greater than 2.33 grams/cc.The most handy tackiness agent identical or close with crystalline silicon lattice parameter of tackiness agent involved in the present invention, the metal content of this tackiness agent will be lower than 30ppma.Bonding coating layer involved in the present invention is not limited to 2 layers.
Seeding plate of the present invention has the physical property close with silicon materials; This seeding plate can effectively reduce the required forming core merit of forming core, has greatly strengthened the ability of heterogeneous nucleation; This seeding plate provides controlled nucleating center for the non-spontaneous nucleation of silicon crystal.The invention solves at present, the efficient silicon ingot early growth period of current fine melt seeding material embeds silicon crystal, causes the later stage to split the problem of ingot; Solved the long brilliant initial stage seed crystal fusing degree of the efficient silicon ingot of current fritting wayward, and the later stage must the low problem of material rate; The present invention has reduced forming core condition, has promoted the mode of non-spontaneous nucleation, has solved the uncontrollable problem of forming core causing due to factors such as thermal field, crucibles in nucleation process.

Claims (4)

1. the efficient silicon ingot seeding of a polysilicon plate; comprise the seeding plate core (1) that silicon purity is greater than 99.99999%; it is characterized in that; seeding plate core (1) is that the length of side is the square plate core that the square plate core of 125 millimeters or the length of side are 156 millimeters; on the outside surface of seeding plate core (1), be bonded with the bonding coating layer (2) of silicon carbide particle or silicon nitride particle, the silicon carbide particle in bonding coating layer (2) or the particle diameter of silicon nitride particle are less than or equal to 0.003 millimeter.
2. the efficient silicon ingot seeding of a kind of polysilicon according to claim 1 plate, is characterized in that, the ratio of the volume of the volume of seeding plate core (1) and bonding coating layer (2) is 1:2-1:5.
3. a preparation method for the efficient silicon ingot seeding of polysilicon plate, comprises the following steps:
The first step, choose silicon purity be greater than 99.99999% the length of side be 125 millimeters or the length of side be 156 millimeters seeding plate core (1);
Second step, choose the silicon carbide particle that particle diameter is less than or equal to 0.003 millimeter;
The 3rd step, choose resistivity and be greater than the pure water of 18M Ω .cm and metal content lower than the tackiness agent of 30ppma;
Together with the pure water that the 4th step, the silicon carbide particle that second step is chosen are chosen with the 3rd step and tackiness agent, put in agitator and stir 15-20 minute, make the silicon carbide particle pasty state suspension liquid that density is greater than 2.33 grams/cubic centimeter;
The 5th step, the seeding plate core (1) that the first step is chosen are put in the silicon carbide particle pasty state suspension liquid that the 4th step obtains and are soaked 2-5 minute;
The 6th step, seeding plate core (1) the 5th step is soaked and that be coated with silicon carbide particle pasty state suspension layers are placed in argon gas atmosphere, dry to burn to make its temperature reach 150-200 ℃, and keep 10-30 minute; Then make it in argon gas atmosphere, naturally cool to room temperature;
The finished product that the ratio of the volume of the 7th step, the volume of choosing seeding plate core (1) and bonding coating layer (2) is 1:2-1:5, obtains the efficient silicon ingot seeding of polysilicon plate.
4. a preparation method for the efficient silicon ingot seeding of polysilicon plate, comprises the following steps:
The first step, choose silicon purity be greater than 99.99999% the length of side be 125 millimeters or the length of side be 156 millimeters seeding plate core (1);
Second step, choose the silicon nitride particle that particle diameter is less than or equal to 0.003 millimeter;
The 3rd step, choose resistivity and be greater than the pure water of 18M Ω .cm and metal content lower than the tackiness agent of 30ppma;
Together with the pure water that the 4th step, the silicon nitride particle that second step is chosen are chosen with the 3rd step and tackiness agent, put in agitator and stir 15-20 minute, make the silicon nitride particle pasty state suspension liquid that density is greater than 2.33 grams/cubic centimeter;
The 5th step, the seeding plate core (1) that the first step is chosen are put in the silicon nitride particle pasty state suspension liquid that the 4th step obtains and are soaked 2-5 minute;
The 6th step, seeding particle cores (1) the 5th step is soaked and that be coated with silicon nitride particle pasty state suspension layers are placed in argon gas atmosphere, dry to burn to make its temperature reach 150-200 ℃, and keep 10-30 minute; Then make it in argon gas atmosphere, naturally cool to room temperature;
The finished product that the ratio of the volume of the 7th step, the volume of choosing seeding plate core (1) and bonding coating layer (2) is 1:2-1:5, obtains the efficient silicon ingot seeding of polysilicon particle.
CN201410455986.1A 2014-09-10 2014-09-10 Polycrystalline-silicon high-efficiency silicon ingot seeding plate and preparation method thereof Pending CN104152989A (en)

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Publication number Priority date Publication date Assignee Title
CN104630884A (en) * 2015-01-23 2015-05-20 东海晶澳太阳能科技有限公司 Seed crystal for full-molten efficient polycrystalline silicon ingot, as well as preparation method and application thereof
CN105568374A (en) * 2016-03-16 2016-05-11 常熟华融太阳能新型材料有限公司 Selective all-melting high-efficiency crucible for polycrystal cast ingots
CN106222734A (en) * 2016-09-12 2016-12-14 江西赛维Ldk太阳能高科技有限公司 A kind of crystalline silicon ingot casting seed crystal and preparation method thereof and crystalline silicon and preparation method thereof

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CN103911658A (en) * 2012-12-28 2014-07-09 中美硅晶制品股份有限公司 Seed crystal for producing silicon crystal ingot
CN204111923U (en) * 2014-09-10 2015-01-21 山西中电科新能源技术有限公司 Polysilicon efficient silicon ingot seeding plate

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WO2005007938A1 (en) * 2003-07-17 2005-01-27 National University Corporation Tohoku University METHOD FOR GROWING Si BASED CRYSTAL, Si BASED CRYSTAL, Si BASED CRYSTAL SUBSTRATE AND SOLAR CELL
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104630884A (en) * 2015-01-23 2015-05-20 东海晶澳太阳能科技有限公司 Seed crystal for full-molten efficient polycrystalline silicon ingot, as well as preparation method and application thereof
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Application publication date: 20141119