CN103361722A - Polycrystalline silicon ingots and preparation method thereof, polycrystalline silicon chips and polycrystalline silicon ingot casting crucible - Google Patents
Polycrystalline silicon ingots and preparation method thereof, polycrystalline silicon chips and polycrystalline silicon ingot casting crucible Download PDFInfo
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- CN103361722A CN103361722A CN2013103111247A CN201310311124A CN103361722A CN 103361722 A CN103361722 A CN 103361722A CN 2013103111247 A CN2013103111247 A CN 2013103111247A CN 201310311124 A CN201310311124 A CN 201310311124A CN 103361722 A CN103361722 A CN 103361722A
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Abstract
The invention provides a preparation method of polycrystalline silicon ingots. The preparation method comprises the following steps: before or after the inner wall of a crucible is sprayed with a silicon nitride layer, a barrier layer is arranged on the inner side of the side wall of the crucible, wherein the barrier layer is a silicon powder coating layer, or a quartz powder coating layer, or a silicon powder and quartz powder mixed coating layer, and purities of silicon powder and quartz powder are above 99.99%; then a molten silicon material is arranged in the crucible; temperature in the crucible is controlled to increase gradually, along a direction which is perpendicular to the bottom of the crucible and is upward, to form a temperature gradient to make the molten silicon material to begin crystallization; and after the crystallization is finished, and the polycrystalline silicon ingots are obtained through annealing and cooling . The invention also provides the high quality polycrystalline silicon ingots obtained by the preparation method, and polycrystalline silicon chips prepared from the polycrystalline silicon ingots and the polycrystalline silicon ingot casting crucible. The polycrystalline silicon ingots prepared by the preparation method are characterized in that crystalline grains near areas of crucible wall are smaller, uniform and regular, dislocation density is low, and impurities is less.
Description
Technical field
The present invention relates to the polycrystalline silicon ingot casting field, relate in particular to polycrystal silicon ingot and preparation method thereof, polysilicon chip and crucible used for polycrystalline silicon ingot casting.
Background technology
At present, directional solidification system method (being called for short DSS) the stove crystal technique that adopts GT Solar to provide is provided the preparation method of polycrystal silicon ingot, the method inwall of normally the silicon material being packed into is sprayed with in the quartz crucible of silicon nitride coating, after melting fully, reduces gradually in the silicon material temperature of crucible bottom, so that silicon melt is from crucible bottom continuous crystallization from bottom to top until solidify fully, the polycrystal silicon ingot of the method manufacturing causes the crystal mass that will be lower than the silicon ingot central zone by the crystal mass in crucible zone owing to be subject to the pollution of quartz crucible and silicon nitride coating.
In the existing above-mentioned polycrystalline cast ingot process, polycrystalline comprises following shortcoming at the capable nuclear of sidewall of quartz crucible: 1) in the fusing of silicon material and directional freeze process, crucible wall is because higher near heater temperature, the impurity such as the oxynitride that crucible wall and inwall silicon nitride coating generation chemical reaction generate under the high temperature and Si oxide melt easily and enter easily in the crystal in crystal growth phase, easily form inclusion, the electric leakage probability of induced defects and battery; 2) crucible sidepiece crystal is with the crystal grain in the certain crystal orientation of dendrite mode row karyogenesis, and crystal grain is larger, and crystal boundary is less, and the diffusion length of impurity in crystal grain is longer, thereby has reduced the crystal mass in close sidewall of crucible zone.
Summary of the invention
For addressing the above problem, the present invention aims to provide the preparation method of polycrystal silicon ingot, and this preparation method can prepare the much higher crystal silicon ingot of quality, and simple and convenient, and easy handling is suitable for scale operation.The present invention provides the high-quality polycrystal silicon ingot that obtains by this preparation method simultaneously, and the polysilicon chip and the crucible used for polycrystalline silicon ingot casting that utilize described polycrystal silicon ingot to prepare.The crystal grain by the sidewall of crucible zone of the polycrystal silicon ingot that this preparation method makes is less, even, regular, dislocation desity is low and impurity is few.
First aspect the invention provides the preparation method of polycrystal silicon ingot, may further comprise the steps:
Before or after crucible inner-wall spraying silicon nitride layer, inside sidewalls at described crucible arranges barrier layer, described barrier layer is silica flour coating or silica powder coating or silica flour and silica powder mixed coating, and the purity of described silica flour and described silica powder is more than 99.99%;
Then the silicon material of molten state is set in described crucible;
Control temperature in the described crucible along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually, make the silicon material of described molten state begin crystallization;
After whole crystallizations are complete, obtain polycrystal silicon ingot through the annealing cooling.
Preferably, the thickness of described barrier layer is 1～5mm.
More preferably, the thickness of described barrier layer is 2～3mm.
Wherein, the preparation method of barrier layer is not limit.Preferably, described barrier layer adopts the mode that applies or spray to prepare.
Preferably, the grain diameter of described silica flour is 1～8 μ m, and the grain diameter of described silica powder is 1～20 μ m.
More preferably, the grain diameter of described silica flour is 1～5 μ m, and the grain diameter of described silica powder is 1～5 μ m.
Crucible of the present invention refers to the container of accommodating polycrystal silicon ingot growth, and its shape and kind are not limit.
Preferably, the described silicon material that molten state is set is: load the solid silicon material in described crucible, described crucible is heated so that the melting of described silicon material.
Also preferably, the described silicon material that molten state is set is: heat solid silicon material in the another one crucible, make the silicon material of molten state, and the silicon material of described molten state is poured in the described crucible that is provided with barrier layer.
The thermal field of control in the crucible be for the silicon material to molten state cools off, and solidifies from bottom to top after making it reach supercooled state.At this moment, the molten silicon material near crucible wall carries out a large amount of nucleation and crystallizations at the barrier layer of sidewall.The barrier layer that utilizes high-purity silicon powder and/or silica powder to make, apply or be sprayed on four inside sidewalls of crucible, the silica flour coating can separate silicon nitride coating or crucible inwall with silicon melt or silicon crystal, thereby reduce silicon nitride in fusion stage and crystallisation stage, Si oxide enters silicon solution or silicon crystal, reduced nitrogen, the impurity such as oxygen are to the pollution of silicon crystal, crystallisation stage can form little crystal grain by a large amount of forming cores on the remaining silica flour of sidewall, barrier layer can increase the nucleation rate of crucible wall, increase at the capable check figure order of crystallisation stage crucible wall like this, number of dies significantly increases, form a large amount of crystal boundaries, impurity in the quartz crucible spreads in crystal boundary comparatively fast, simultaneously because the crystal boundary in close sidewall of crucible zone tends to be parallel to sidewall of crucible, a large amount of like this crystal boundaries has reduced the transverse diffusion distance of the diffusion of impurity, thereby has improved the few sub-carrier lifetime of the silicon chip of close sidewall of crucible part.
Preferably, in the forming core crystallisation process control condensate depression be-1K～-30K.High condensate depression is conducive to form in a large number take (110), (112) and is main crystal orientation, wrong row distinguishes because crystal boundary is atom, a large amount of crystal boundaries can stop the motion propagation of dislocation, so that the whole dislocation minimizing of silicon ingot, thereby the efficiency of conversion of raising crystalline silicon.
Second aspect the invention provides polycrystal silicon ingot, and described polycrystal silicon ingot makes according to the preparation method of aforementioned polycrystal silicon ingot.The dislocation desity of described polycrystal silicon ingot≤4 * 10
5Individual/cm
2
The third aspect the invention provides polysilicon chip, and described polysilicon chip is for to carry out making after evolution-section-cleaning take aforementioned polycrystal silicon ingot as raw material.
Fourth aspect, the invention provides a kind of crucible used for polycrystalline silicon ingot casting, described crucible comprises body, silicon nitride layer and barrier layer, described body comprises that base reaches by the upwardly extending sidewall of base, described base and described sidewall surround a receiving space jointly, described silicon nitride layer is attached to described body base and the sidewall surfaces towards described receiving space, described barrier layer is arranged on the silicon nitride layer of described sidewall or is arranged between the silicon nitride layer of described sidewall and described sidewall, described barrier layer is the silica flour coating, or silica powder coating, or silica flour and silica powder mixed coating, the purity of described silica flour and described silica powder is more than 99.99%.
Preferably, the thickness of described barrier layer is 1～5mm.
More preferably, the thickness of described barrier layer is 2～3mm.
Crucible used for polycrystalline silicon ingot casting provided by the invention, by the barrier layer of being made by high-purity silicon powder and/or silica powder particle in the inside sidewalls setting, so that the silicon material of melting can be not in process of setting with high temperature under the impurity of non-silicon class contact the greatly pollution of impurity reduction; Simultaneously, in the process of setting, easily form less crystal grain on the barrier layer of crucible wall, crystal boundary density is high, but impurity reduction in the horizontal rate of diffusion in sidewall of crucible zone, thereby improve silicon crystal quality near the sidewall of crucible part.
Polycrystal silicon ingot provided by the invention and preparation method thereof, polysilicon chip and crucible used for polycrystalline silicon ingot casting have following beneficial effect:
(1) polycrystal silicon ingot provided by the invention is low and impurity is few near homogeneous grain size, rule, the dislocation desity of sidewall of crucible;
(2) preparation method of polycrystal silicon ingot provided by the invention is simple and convenient, and easy handling is suitable for scale operation;
(3) polysilicon chip provided by the invention is applicable to prepare solar cell, and the conversion efficiency of solar cell that makes is high;
(4) crucible used for polycrystalline silicon ingot casting provided by the invention has barrier layer, but its barrier layer impurity reduction improves the silicon ingot quality to the pollution of silicon ingot.
Description of drawings
Fig. 1 is the synoptic diagram of the crucible used for polycrystalline silicon ingot casting of preparation in the embodiment of the invention one;
Fig. 2 is the synoptic diagram of the embodiment of the invention one preparation process;
Fig. 3 is the minority carrier life time figure of the polycrystal silicon ingot that makes of embodiment one;
Fig. 4 is the minority carrier life time figure of the polycrystal silicon ingot that makes of embodiment two;
The minority carrier life time figure of the polycrystal silicon ingot that Fig. 5 makes for the comparative example.
Embodiment
The following stated is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Embodiment one
The preparation method of polycrystal silicon ingot may further comprise the steps:
(1) after the crucible inwall is coated silicon nitride layer, be 99.99% silica flour again in the silicon nitride layer spraying purity of the inside sidewalls of crucible, make the barrier layer that thickness is 3mm; The particle diameter of silica flour is 1～8 μ m;
Fig. 1 is the synoptic diagram of the crucible used for polycrystalline silicon ingot casting of embodiment of the invention preparation.Wherein, 1 is the crucible body, and 2 is silicon nitride layer, and 3 is the barrier layer that arranges on the crucible wall.
(2) then the silicon material of molten state is set in crucible;
Wherein, the silicon material that molten state is set is: load solid silicon material 530kg in crucible, crucible is heated to 1560 ℃ so that the melting of solid silicon material.
Fig. 2 is the synoptic diagram of the embodiment of the invention one preparation process.Wherein, 1 is the crucible body, and 2 is silicon nitride layer, and 3 is the silica flour barrier layer that arranges on the crucible wall, and 4 is the solid silicon material.
(3) temperature of control in the described crucible makes the silicon material of described molten state begin crystallization along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually; After whole crystallizations are complete, obtain polycrystal silicon ingot through the annealing cooling;
Wherein, open heat-insulation cage, the control bottom temp is 1380 ℃, so that silicon melt reaches the supercooled state crystallization and freezing, obtains polycrystal silicon ingot.
The prepared polycrystal silicon ingot average dislocation density of present embodiment is less than 2 * 10
5Individual/cm
2, the sidepiece silico briquette is removed end to end the bad rear average minority carrier lifetime of impurity greater than 5 microseconds (us).
The polysilicon chip that the polycrystal silicon ingot that utilizes present embodiment to make makes is applicable to prepare solar cell, and the average efficiency of conversion of solar cell that makes by the silicon chip in sidewall of crucible zone is 17.4～17.5%.
Embodiment two
The preparation method of polycrystal silicon ingot may further comprise the steps:
(1) after the crucible inwall is coated silicon nitride layer, be 99.9999% silica powder again in the silicon nitride layer spraying purity of the inside sidewalls of crucible, make the barrier layer that thickness is 2mm; The particle diameter of silica powder is 1～20 μ m;
(2) then the silicon material of molten state is set in crucible;
Wherein, the silicon material that molten state is set is: load solid silicon material 530kg in crucible, crucible is heated to 1560 ℃ so that the melting of solid silicon material.
(3) temperature of control in the described crucible makes the silicon material of described molten state begin crystallization along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually; After whole crystallizations are complete, obtain polycrystal silicon ingot through the annealing cooling;
Wherein, open heat-insulation cage, the control bottom temp is 1300 ℃, so that silicon melt reaches the supercooled state crystallization and freezing, obtains polycrystal silicon ingot.
The prepared polycrystal silicon ingot dislocation desity of present embodiment is less than 3 * 10
5Individual/cm
2, the sidepiece silico briquette is removed end to end the bad rear average minority carrier lifetime of impurity greater than 5 microseconds (us).
The polysilicon chip that the polycrystal silicon ingot that utilizes present embodiment to make makes is applicable to prepare solar cell, and the average efficiency of conversion of solar cell that makes by the silicon chip in sidewall of crucible zone is 17.3～17.5%.
Embodiment three
The preparation method of polycrystal silicon ingot may further comprise the steps:
(1) the spraying purity in crucible inwall inboard is 99.9999% silica powder, makes the barrier layer that thickness is 5mm; The particle diameter of silica powder is 1～5 μ m, afterwards spraying silicon nitride coating on the silica powder barrier layer;
(2) then the silicon material of molten state is set in crucible;
Wherein, the silicon material that molten state is set is: heat solid silicon material is 530 kilograms in the another one crucible, is heated to 1560 ℃, makes the silicon material of molten state, the silicon material of molten state is poured into step (1) is provided with in the crucible of barrier layer;
(3) temperature of control in the described crucible makes the silicon material of described molten state begin crystallization along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually; After whole crystallizations are complete, obtain polycrystal silicon ingot through the annealing cooling;
Wherein, open heat-insulation cage, the control bottom temp is 1350 ℃, so that silicon melt reaches the supercooled state crystallization and freezing, obtains polycrystal silicon ingot.
The prepared polycrystal silicon ingot average dislocation density of present embodiment is less than 4 * 10
5Individual/cm
2, the sidepiece silico briquette is removed end to end the bad rear average minority carrier lifetime of impurity greater than 5 microseconds (us).
The polysilicon chip that the polycrystal silicon ingot that utilizes present embodiment to make makes is applicable to prepare solar cell, and the average efficiency of conversion of solar cell that makes by the silicon chip in sidewall of crucible zone is 17.3～17.4%.
Embodiment four
The preparation method of polycrystal silicon ingot may further comprise the steps:
(1) after the crucible inwall is coated silicon nitride layer, be 99.9999% silica flour and silica powder again in the silicon nitride layer spraying purity of the inside sidewalls of crucible, make the barrier layer that thickness is 3mm; The particle diameter of silica flour is 1～8 μ m, and the particle diameter of silica powder is 1～20 μ m;
(2) then the silicon material of molten state is set in crucible;
Wherein, the silicon material that molten state is set is: heat solid silicon material is 530 kilograms in the another one crucible, is heated to 1560 ℃, makes the silicon material of molten state, the silicon material of molten state is poured into step (1) is provided with in the crucible of barrier layer;
(3) temperature of control in the described crucible makes the silicon material of described molten state begin crystallization along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually; After whole crystallizations are complete, obtain polycrystal silicon ingot through the annealing cooling;
Wherein, open heat-insulation cage, the control bottom temp is 1350 ℃, so that silicon melt reaches the supercooled state crystallization and freezing, obtains polycrystal silicon ingot.
The dislocation desity of the prepared polycrystal silicon ingot sidepiece of present embodiment silico briquette is less than 3 * 10
5Individual/cm
2, the sidepiece silico briquette is removed end to end the bad rear average minority carrier lifetime of impurity greater than 5 microseconds (us).
The polysilicon chip that the polycrystal silicon ingot that utilizes present embodiment to make makes is applicable to prepare solar cell, and the average efficiency of conversion of solar cell that makes by the silicon chip in sidewall of crucible zone is 17.3～17.5%.
Effect embodiment
For providing powerful support for beneficial effect of the present invention, the spy provides following comparative example:
The comparative example: the silicon material of in the crucible of the good silicon nitride coating of inner-wall spraying, packing into, be heated to 1560 ℃ of meltings, open afterwards heat-insulation cage, so that the bottom begins to cool down.After finishing, long crystalline substance enters the annealing cooling stages.Obtain polycrystal silicon ingot after the cooling fully.
The embodiment of the invention 1～4 and comparative example's gained polycrystal silicon ingot are carried out quality examination, and the detected result contrast is as follows:
Table 1. embodiment 1～4 and comparative example's contrast
The gained measured value is the mean value of measuring 20 sample gained in the table 1.
The bad ratio of minority carrier life time of the polycrystal silicon ingot that makes of embodiment of the invention preparation method all significantly is lower than the comparative example as can be seen from Table 1.
Fig. 3 is the minority carrier life time figure of the polycrystal silicon ingot that makes of embodiment 1; Fig. 4 is the minority carrier life time figure of the polycrystal silicon ingot that makes of embodiment 2.The minority carrier life time figure of the polycrystal silicon ingot that Fig. 5 makes for the comparative example.The bad width of minority carrier life time that can find out the polycrystal silicon ingot silico briquette side that employing embodiment of the invention preparation method makes from Fig. 3, Fig. 4 and Fig. 5 has had remarkable minimizing.This explanation, the barrier layer that the embodiment of the invention is made by high-purity silicon powder and/or silica powder particle in the inside sidewalls setting so that the silicon material of melting can be not in process of setting with high temperature under the impurity of non-silicon class contact the greatly pollution of impurity reduction; Simultaneously, in the process of setting, easily form less crystal grain on the barrier layer of crucible wall, crystal boundary density is high, but impurity reduction in the horizontal rate of diffusion in sidewall of crucible zone, thereby improve silicon crystal quality near the sidewall of crucible part.
Claims (10)
1. the preparation method of a polycrystal silicon ingot is characterized in that, comprising:
Before or after crucible inner-wall spraying silicon nitride layer, inside sidewalls at described crucible arranges barrier layer, described barrier layer is silica flour coating or silica powder coating or silica flour and silica powder mixed coating, and the purity of described silica flour and described silica powder is more than 99.99%;
Then the silicon material of molten state is set in described crucible;
Control temperature in the described crucible along the vertical direction that makes progress with the described crucible bottom formation temperature gradient that rises gradually, make the silicon material of described molten state begin crystallization;
After whole crystallizations are complete, obtain polycrystal silicon ingot through the annealing cooling.
2. the preparation method of polycrystal silicon ingot as claimed in claim 1 is characterized in that, the thickness of described barrier layer is 1～5mm.
3. the preparation method of polycrystal silicon ingot as claimed in claim 1 is characterized in that, described barrier layer adopts the mode that applies or spray to prepare.
4. the preparation method of polycrystal silicon ingot as claimed in claim 1 is characterized in that, the grain diameter of described silica flour is 1～8 μ m, and the grain diameter of described silica powder is 1～20 μ m.
5. the preparation method of polycrystal silicon ingot as claimed in claim 1 is characterized in that, the described silicon material that molten state is set is: load the solid silicon material in described crucible, described crucible is heated so that the melting of described silicon material.
6. the preparation method of polycrystal silicon ingot as claimed in claim 1, it is characterized in that, the described silicon material that molten state is set is: heat solid silicon material in the another one crucible, make the silicon material of molten state, and the silicon material of described molten state is poured in the described crucible that is provided with barrier layer.
7. polycrystal silicon ingot is characterized in that, according to making such as the described preparation method of arbitrary claim in the claim 1～6.
8. polysilicon chip is characterized in that, described polysilicon chip is for to carry out making after evolution-section-cleaning take polycrystal silicon ingot as claimed in claim 7 as raw material.
9. crucible used for polycrystalline silicon ingot casting, it is characterized in that, described crucible comprises body, silicon nitride layer and barrier layer, described body comprises that base reaches by the upwardly extending sidewall of base, described base and described sidewall surround a receiving space jointly, described silicon nitride layer is attached to described body base and the sidewall surfaces towards described receiving space, described barrier layer is arranged on the silicon nitride layer of described sidewall or is arranged between the silicon nitride layer of described sidewall and described sidewall, described barrier layer is the silica flour coating, or silica powder coating, or silica flour and silica powder mixed coating, the purity of described silica flour and described silica powder is more than 99.99%.
10. crucible as claimed in claim 9 is characterized in that, the thickness of described barrier layer is 1～5mm.
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