CN102776555A - Polycrystalline silicon ingot and preparation method thereof as well as polycrystalline silicon wafer - Google Patents
Polycrystalline silicon ingot and preparation method thereof as well as polycrystalline silicon wafer Download PDFInfo
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- CN102776555A CN102776555A CN2012100962322A CN201210096232A CN102776555A CN 102776555 A CN102776555 A CN 102776555A CN 2012100962322 A CN2012100962322 A CN 2012100962322A CN 201210096232 A CN201210096232 A CN 201210096232A CN 102776555 A CN102776555 A CN 102776555A
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 142
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 142
- 239000010703 silicon Substances 0.000 claims abstract description 142
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 18
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000011049 filling Methods 0.000 claims abstract 2
- 239000002210 silicon-based material Substances 0.000 claims description 58
- 229920005591 polysilicon Polymers 0.000 claims description 31
- 239000011856 silicon-based particle Substances 0.000 claims description 21
- 230000004927 fusion Effects 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 15
- 239000004484 Briquette Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 229910021419 crystalline silicon Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 abstract description 5
- 230000006911 nucleation Effects 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 3
- 238000013459 approach Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 4
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000010453 quartz Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 230000009466 transformation Effects 0.000 description 10
- 238000001514 detection method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000009395 breeding Methods 0.000 description 2
- 230000001488 breeding effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- TVZRAEYQIKYCPH-UHFFFAOYSA-N 3-(trimethylsilyl)propane-1-sulfonic acid Chemical compound C[Si](C)(C)CCCS(O)(=O)=O TVZRAEYQIKYCPH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
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Abstract
The invention discloses a preparation method of a polycrystalline silicon ingot, comprising the following steps of: filling a silicon mixture in a crucible from bottom to top after coating a silicon nitride layer on the inner wall of the crucible; heating the crucible so that the silicon mixture in the crucible is melted to form a silicon melt, and when a solid-liquid interface formed by the silicon melt and an unmelted silicon mixture approaches to the bottom surface of the crucible, regulating a thermal field to form a supercooled state, so that the silicon melt carries out crystal growth on the basis of the silicon mixture which is not completely melted; and after crystallization of all the silicon melt, annealing and cooling to obtain the polycrystalline silicon ingot. With the adoption of the preparation method, the polycrystalline silicon ingot can have good initial nucleation, and dislocation propagation of the polycrystalline silicon ingot in the growth process is lowered. The invention also discloses the polycrystalline silicon ingot acquired through the preparation method and a polycrystalline silicon wafer prepared with the polycrystalline silicon ingot as a raw material.
Description
Technical field
The present invention relates to field of semiconductor manufacture, relate in particular to a kind of polycrystal silicon ingot and preparation method thereof and polysilicon chip.
Background technology
In recent years, sun power has become the focus of people's R and D as a kind of emerging renewable green energy resource.Be accompanied by the fast development of solar cell industry, the low and polysilicon that be suitable for large-scale production of cost becomes one of topmost photovoltaic material in the industry, and progressively replaces the dominant position of traditional pulling of silicon single crystal in solar cell material market.
At present, the preparation method of polycrystal silicon ingot is mainly directional freeze systems approach (being called for short DSS) the stove crystal technique that adopts GT Solar to be provided, and this method generally includes heating, melts, solidifies steps such as long crystalline substance, annealing and cooling.In solidifying long brilliant process, be accompanied by the lasting cooling of crucible bottom, the spontaneous formation of silicon material of molten state at random forming core and at random forming core grow gradually.But because that initial forming core does not have is controlled, be easy to generate dislocation in the nucleation process, cause the crystal orientation mixed and disorderly, crystal grain is inhomogeneous, and the polycrystal silicon ingot quality that therefore prepares through this method is lower.Utilize the photoelectric transformation efficiency of the solar cell that this polycrystal silicon ingot makes low.Therefore, in order to make the high quality polycrystal silicon ingot that dislocation desity is low, defective is few, a kind of polycrystal silicon ingot castmethod that can effectively obtain good initial forming core becomes very important.
Summary of the invention
In order to solve the problems of the technologies described above, the present invention aims to provide a kind of preparation method of polycrystal silicon ingot, and this preparation method can make polycrystal silicon ingot obtain good initial forming core, reduces the dislocation breeding of polycrystal silicon ingot in process of growth, obtains the high quality polycrystal silicon ingot.The present invention provides the high-quality polycrystal silicon ingot that obtains through this preparation method simultaneously, and with said polycrystal silicon ingot is the polysilicon chip that raw material makes.
First aspect the invention provides a kind of preparation method of polycrystal silicon ingot, comprising:
After the crucible inwall is coated silicon nitride layer, in said crucible, load the silicon material from bottom to up;
Heating makes silicon material fusing formation silicon melt in the said crucible; When said silicon melt and the formed solid-liquid interface of unfused said silicon material during near the crucible bottom surface; Regulate thermal field and form supercooled state, it is long brilliant that said silicon melt is begun on the silicon material basis of not exclusively fusing;
After treating that whole silicon melt crystallizations are intact, obtain polycrystal silicon ingot through the annealing cooling.
Wherein, the setting of silicon nitride layer on the crucible inwall can prevent effectively that the impurity of crucible inwall from getting in the crystal, and prevents that polycrystal silicon ingot from sticking pot phenomenon taking place, thereby improves the quality and the operation easier that reduces casting ingot process of polycrystal silicon ingot.
The forming core of silicon melt on silicon solid aspect belongs to homogeneity forming core mode; The needed motivating force of homogeneity forming core mode will be much smaller than the heterogeneous forming core mode on the crucible of materials such as quartz or pottery; On silicon solid aspect, can form a plurality of equally distributed forming cores source; Thereby make polycrystal silicon ingot obtain good initial forming core, and then grow crystal with advantage crystal orientation.In addition, solid silicon has good heat conductivility, obtains bigger motivating force when making the silicon melt forming core, thereby promotes the control of initial forming core, grows the crystal grain with advantage crystal orientation.
Preferably, when loading the silicon material, lay one deck silicon particle in crucible bottom earlier.
Preferably, the silicon particle is one or more in silicon single crystal particle, polysilicon particle and the non-crystalline silicon particle.
Preferably, when silicon melt and the formed solid-liquid interface of unfused silicon material just are in silicon particle layer, regulate thermal field and form supercooled state, it is long brilliant that silicon melt is begun on the silicon material basis of not exclusively fusing.
Preferably, when silicon melt and the formed solid-liquid interface of unfused silicon material are goed deep into silicon particle layer, regulate thermal field and form supercooled state, it is long brilliant that silicon melt is begun on the silicon material basis of not exclusively fusing.
Silicon particle place mat is a lack of alignment in crucible bottom, and the particle layer forms a supporting structure, and this supporting structure has countless holes; In the silicon material fusion stage, the silicon melt that the fusing of silicon material forms will be filled in the hole, in the initial forming core stage; Under supercooled state; On silicon particle aspect, form a plurality of equally distributed forming cores source, thereby make polycrystal silicon ingot obtain good initial forming core, and then grow crystal with advantage crystal orientation.Particularly; Controlled temperature makes silicon melt that is in silicon melt and the formed solid-liquid interface of unfused silicon material and the silicon melt that is filled in the hole reach supercooled state earlier; Preferential forming core crystallization, move to the direction away from crucible bottom at the silicon melt interface subsequently, the silicon melt crystallization and freezing.The initial forming core of polycrystal silicon ingot is well controlled, thereby grows the prevailing crystal in useful crystal orientation, therefore can prevent a large amount of propagation of dislocation, obtains the high quality polycrystal silicon ingot.
Preferably, the size of silicon particle is 0.1 μ m～10cm; More preferably, the size of silicon particle is 0.1cm～10cm.
Wherein, size is that the silicon particle of 0.1 μ m～10 μ m is a micro mist.
Preferably, silicon particle laying depth is 0.5cm～5cm.
The thickness of silicon particle is too thin, is not easy to carry out lay-up operation, is difficult to control, and in addition, the thickness of silicon particle is too thin, is unfavorable for forming complete supporting structure, thereby is unfavorable for follow-up forming core crystallisation process.
Preferably, place mat one deck heat-conducting block between the bottom of silicon material and said crucible.
Preferably, heat-conducting block is silico briquette or graphite block.
Preferably, said silico briquette is one or more in monocrystalline silico briquette, polysilicon block and the noncrystal silico briquette.
Preferably, the laying depth of heat-conducting block is 1cm～2cm.
Silico briquette and graphite block all have good heat conductivility, when the silicon melt forming core, will make forming core obtain bigger motivating force, thereby promote to produce in the nucleation process crystal grain with advantage crystal orientation.
Preferably, every in the fusion stage of silicon material at a distance from 0.2～1h, survey the position of once said silicon melt and the formed solid-liquid interface of unfused said silicon material.
Particularly, adopt quartz pushrod to survey the position of said silicon melt and the formed solid-liquid interface of unfused said silicon material.
Preferably, every in early stage fusion stage of silicon material at a distance from 0.5～1h, survey the position of once said silicon melt and the formed solid-liquid interface of unfused said silicon material.
Preferably, every in later stage fusion stage of silicon material at a distance from 0.2～0.5h, survey the position of once said silicon melt and the formed solid-liquid interface of unfused said silicon material.
When the position that detects said silicon melt and the formed solid-liquid interface of unfused said silicon material just is in or gos deep into silicon particle layer, begin to regulate thermal field and reach supercooled state, it is long brilliant that silicon melt is begun on the silicon material basis of not exclusively fusing.
Preferably, regulate being operating as of thermal field and regulate the heating power cooling, the amplitude of cooling is 2～500K/min.
Particularly, reduce the heating power of heating unit or directly close heating unit, or open the heat heat abstractor, make the thermal field of silicon ingot growth reach supercooled state, forming core is long brilliant under this supercooled state.
Second aspect the invention provides a kind of polycrystal silicon ingot, and said polycrystal silicon ingot makes according to the preparation method of aforementioned polycrystal silicon ingot.Said polycrystal silicon ingot dislocation desity is less than 10
5Individual/cm
2
The third aspect the invention provides a kind of polysilicon chip, and said polysilicon chip is that raw material makes through evolution-section-cleaning with aforementioned polycrystal silicon ingot.
Embodiment of the present invention embodiment has following beneficial effect:
(1) preparation method of the present invention can make polycrystal silicon ingot obtain good initial forming core, has reduced the dislocation breeding of polycrystal silicon ingot in process of growth, has obtained high-quality polycrystal silicon ingot;
(2) preparation method of the present invention is simple to operate, is easy to the industrial production of mass-producing;
(3) polysilicon chip dislocation desity provided by the invention is little, is applicable to and manufactures solar cell;
(4) photoelectric transformation efficiency of the solar cell of the present invention's making is improved.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art; To do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below; Obviously, the accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills; Under the prerequisite of not paying creative work property, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is a synoptic diagram after the charging of the embodiment of the invention 1;
Fig. 2 is the silicon ingot minority carrier life time detection figure of the embodiment of the invention 1;
Fig. 3 is the silicon ingot bottom dislocation detected result figure of the embodiment of the invention 1;
Fig. 4 is the silicon ingot head dislocation detected result figure of the embodiment of the invention 1.
Embodiment
To combine the accompanying drawing in the embodiment of the invention below, the technical scheme in the embodiment of the invention is carried out clear, intactly description, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills are not making the every other embodiment that is obtained under the creative work prerequisite, all belong to the scope of the present invention's protection.
Embodiment 1
A kind of preparation method of polycrystal silicon ingot comprises:
Getting quartz crucible, behind this crucible inner-wall spraying one deck silicon nitride coating, is 1～5cm in crucible bottom place mat one deck size, and thickness is the polysilicon particle of 1cm.After place mat is intact, on the polysilicon particle, load various blocky silicon material, intact up to whole dresses, Fig. 1 is present embodiment charging back synoptic diagram, and wherein 1 is crucible, and 2 is the polysilicon particle, and 3 is the silicon material.
The above-mentioned crucible that the silicon material is housed is packed in the ingot furnace, start the ingot casting program, vacuumize, be heated to the silicon melting temperature then, the silicon material is slowly melted.In the fusion stage, adopt quartz pushrod detection silicon melt and the formed solid-liquid interface of unfused silicon material position, in early stage fusion stage, every separated 1h once surveys, and in later stage fusion stage, every separated 0.5h once surveys.
When the position that detects silicon melt and the formed solid-liquid interface of unfused silicon material just is in polysilicon particle layer; Heat-insulation cage and cooling are slowly opened in beginning; The temperature of silicon melt is reduced; Temperature reduction amplitude is approximately 10k/min, forms certain condensate depression, and silicon melt begins the long crystalline substance of beginning forming core on the silicon material basis of not exclusively fusing.
After treating that whole silicon melt crystallizations are intact, obtain polycrystal silicon ingot through the annealing cooling.
After the above-mentioned polycrystal silicon ingot cooling that makes, carry out evolution and obtain polysilicon block, obtain polysilicon chip after the section-cleaning, be that raw material adopts silk-screen printing technique to be made into solar cell with this polysilicon chip.
Adopt WT2000 to detect the minority carrier life time of gained polycrystal silicon ingot, detected result is as shown in Figure 2, and as can be seen from Figure 2, (right side) distributes very evenly to the minority carrier life time of head (left side) this polycrystal silicon ingot from the bottom, and low minority carrier life time region area is little, silicon ingot quality height.
To the gained polycrystal silicon ingot, adopt opticmicroscope (amplifying 200 times) to carry out dislocation observation, its detected result is: the average dislocation density of silicon ingot bottom is 2.96 * 10
4(individual/cm
2), be silicon ingot bottom dislocation detected result figure like Fig. 3; The average dislocation density of silicon ingot head is 3.41 * 10
4(individual/cm
2), Fig. 4 is silicon ingot head dislocation detected result figure.
To the gained solar cell, adopt German halm company battery sheet detecting instrument to measure its photoelectric transformation efficiency.The mensuration result is 17.3% for the photoelectric transformation efficiency of solar cell.
Embodiment 2
A kind of preparation method of polycrystal silicon ingot comprises:
Get quartz crucible, behind this crucible inner-wall spraying one deck silicon nitride coating.Be the polysilicon block of 1cm at crucible bottom place mat one layer thickness earlier, and then place mat one deck size is 1～5cm in the above, thickness is the polycrystalline particle of 2cm.After place mat is intact, on the polycrystalline particle, load various blocky silicon material, intact up to whole dresses.
The above-mentioned crucible that the silicon material is housed is packed in the ingot furnace, start the ingot casting program, vacuumize, be heated to the silicon melting temperature then, the silicon material is slowly melted.In the fusion stage, adopt quartz pushrod detection silicon melt and the formed solid-liquid interface of unfused silicon material position, in early stage fusion stage, every separated 1h once surveys, and in later stage fusion stage, every separated 0.5h once surveys.
When polysilicon particle layer 0.5cm goed deep in the position that detects silicon melt and the formed solid-liquid interface of unfused silicon material; Heat-insulation cage and cooling are slowly opened in beginning; The temperature of silicon melt is reduced; Temperature reduction amplitude is approximately 20k/min, forms certain condensate depression, and silicon melt begins the long crystalline substance of beginning forming core on the silicon material basis of not exclusively fusing.
After treating that whole silicon melt crystallizations are intact, obtain polycrystal silicon ingot through the annealing cooling.
After the above-mentioned polycrystal silicon ingot cooling that makes, carry out evolution and obtain polysilicon block, obtain polysilicon chip after the section-cleaning, be that raw material adopts silk-screen printing technique to be made into solar cell with this polysilicon chip.
To the gained polycrystal silicon ingot, adopt opticmicroscope (amplifying 200 times) to carry out dislocation observation, its detected result is: the average dislocation density of silicon ingot bottom is 2.8 * 10
4(individual/cm
2); The average dislocation density of silicon ingot head is 3.40 * 10
4(individual/cm
2).
To the gained solar cell, adopt German halm company battery sheet detecting instrument to measure its photoelectric transformation efficiency.The mensuration result is 17.46% for the photoelectric transformation efficiency of solar cell.
Embodiment 3
A kind of preparation method of polycrystal silicon ingot comprises:
Get quartz crucible, behind this crucible inner-wall spraying one deck silicon nitride coating.Be the graphite cake of 1cm at crucible bottom place mat one layer thickness earlier, graphite material is three high graphite, and then place mat one deck size is 1～5cm in the above, and thickness is the polycrystalline particle of 0.5cm.After place mat is intact, on the polycrystalline particle, load various blocky silicon material, intact up to whole dresses.
The above-mentioned crucible that the silicon material is housed is packed in the ingot furnace, start the ingot casting program, vacuumize, be heated to the silicon melting temperature then, the silicon material is slowly melted.In the fusion stage, adopt quartz pushrod detection silicon melt and the formed solid-liquid interface of unfused silicon material position, in early stage fusion stage, every separated 1h once surveys, and in later stage fusion stage, every separated 0.5h once surveys.
When polysilicon particle layer 0.2cm goed deep in the position that detects silicon melt and the formed solid-liquid interface of unfused silicon material; Heat-insulation cage and cooling are slowly opened in beginning; The temperature of silicon melt is reduced; Temperature reduction amplitude is approximately 15k/min, forms certain condensate depression, and silicon melt begins the long crystalline substance of beginning forming core on the silicon material basis of not exclusively fusing.
After treating that whole silicon melt crystallizations are intact, obtain polycrystal silicon ingot through the annealing cooling.
After the above-mentioned polycrystal silicon ingot cooling that makes, carry out evolution and obtain polysilicon block, obtain polysilicon chip after the section-cleaning, be that raw material adopts silk-screen printing technique to be made into solar cell with this polysilicon chip.
To the gained polycrystal silicon ingot, adopt opticmicroscope (amplifying 200 times) to carry out dislocation observation, its detected result is: the average dislocation density of silicon ingot bottom is 3.1 * 10
4(individual/cm
2); The average dislocation density of silicon ingot head is 3.56 * 10
4(individual/cm
2).
To the gained solar cell, adopt German halm company battery sheet detecting instrument to measure its photoelectric transformation efficiency.The mensuration result is 17.53% for the photoelectric transformation efficiency of solar cell.
Embodiment 4
A kind of preparation method of polycrystal silicon ingot comprises:
Get quartz crucible, behind this crucible inner-wall spraying one deck silicon nitride coating.In crucible, load earlier various blocky silicon material from bottom to up, intact up to whole dresses.
The above-mentioned crucible that the silicon material is housed is packed in the ingot furnace, start the ingot casting program, vacuumize, be heated to the silicon melting temperature then, the silicon material is slowly melted.In the fusion stage, adopt quartz pushrod detection silicon melt and the formed solid-liquid interface of unfused silicon material position, in early stage fusion stage, every separated 1h once surveys, and in later stage fusion stage, every separated 0.5h once surveys.
When the distance when the position that detects silicon melt and the formed solid-liquid interface of unfused silicon material from the crucible bottom surface is 0.2cm; Heat-insulation cage and cooling are slowly opened in beginning; The temperature of silicon melt is reduced; Temperature reduction amplitude is approximately 15k/min, forms certain condensate depression, and silicon melt begins the long crystalline substance of beginning forming core on the silicon material basis of not exclusively fusing.
After treating that whole silicon melt crystallizations are intact, obtain polycrystal silicon ingot through the annealing cooling.
After the above-mentioned polycrystal silicon ingot cooling that makes, carry out evolution and obtain polysilicon block, obtain polysilicon chip after the section-cleaning, be that raw material adopts silk-screen printing technique to be made into solar cell with this polysilicon chip.
To the gained polycrystal silicon ingot, adopt opticmicroscope (amplifying 200 times) to carry out dislocation observation, its detected result is: the average dislocation density of silicon ingot bottom is 3.12 * 10
4(individual/cm
2); The average dislocation density of silicon ingot head is 3.58 * 10
4(individual/cm
2).
To the gained solar cell, adopt German halm company battery sheet detecting instrument to measure its photoelectric transformation efficiency.The mensuration result is 17.48% for the photoelectric transformation efficiency of solar cell.
The above is a 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 improvement and retouching, these improvement and retouching also are regarded as protection scope of the present invention.
Claims (10)
1. the preparation method of a polycrystal silicon ingot is characterized in that, comprising:
After the crucible inwall is coated silicon nitride layer, in said crucible, load the silicon material from bottom to up;
Heating makes silicon material fusing formation silicon melt in the said crucible; When said silicon melt and the formed solid-liquid interface of unfused said silicon material during near the crucible bottom surface; Regulate thermal field and form supercooled state, it is long brilliant that said silicon melt is begun on the silicon material basis of not exclusively fusing;
After treating that whole silicon melt crystallizations are intact, 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, during said filling silicon material, lays one deck silicon particle in said crucible bottom earlier, and said silicon particle is one or more in silicon single crystal particle, polysilicon particle and the non-crystalline silicon particle.
3. the preparation method of polycrystal silicon ingot as claimed in claim 2; It is characterized in that; When said silicon melt and the formed solid-liquid interface of unfused said silicon material just are in silicon particle layer or go deep into silicon particle layer; Regulate thermal field and form supercooled state, it is long brilliant that said silicon melt is begun on the silicon material basis of not exclusively fusing.
4. the preparation method of polycrystal silicon ingot as claimed in claim 2 is characterized in that, the size of said silicon particle is 0.1 μ m～10cm, and said silicon particle laying depth is 0.5cm～5cm.
5. the preparation method of polycrystal silicon ingot as claimed in claim 1 is characterized in that, place mat one deck heat-conducting block between the bottom of said silicon material and said crucible.
6. the preparation method of polycrystal silicon ingot as claimed in claim 5 is characterized in that, said heat-conducting block is silico briquette or graphite block.
7. the preparation method of polycrystal silicon ingot as claimed in claim 5 is characterized in that, the laying depth of said heat-conducting block is 1cm～2cm.
8. the preparation method of polycrystal silicon ingot as claimed in claim 1 is characterized in that, and is every at a distance from 0.2～1h in the fusion stage of said silicon material, surveys the position of once said silicon melt and the formed solid-liquid interface of unfused said silicon material.
9. a polycrystal silicon ingot is characterized in that, said polycrystal silicon ingot is according to making like each described preparation method of claim 1～8.
10. a polysilicon chip is characterized in that, said polysilicon chip is that raw material prepares through evolution-section-cleaning with the described polycrystal silicon ingot of claim 9.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210096232.2A CN102776555B (en) | 2012-04-01 | 2012-04-01 | A kind of polycrystal silicon ingot and preparation method thereof and polysilicon chip |
| KR1020147030926A KR101656596B1 (en) | 2012-04-01 | 2013-03-28 | Polycrystalline silicon ingot, preparation method thereof, and polycrystalline silicon wafer |
| US14/389,452 US9562304B2 (en) | 2012-04-01 | 2013-03-28 | Polycrystalline silicon ingot, preparation method thereof, and polycrystalline silicon wafer |
| PCT/CN2013/073364 WO2013149560A1 (en) | 2012-04-01 | 2013-03-28 | Polycrystalline silicon ingot, preparation method thereof, and polycrystalline silicon wafer |
| US15/357,707 US10227711B2 (en) | 2012-04-01 | 2016-11-21 | Method for preparing polycrystalline silicon ingot |
| US15/360,472 US10253430B2 (en) | 2012-04-01 | 2016-11-23 | Method for preparing polycrystalline silicon ingot |
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| CN201210096232.2A CN102776555B (en) | 2012-04-01 | 2012-04-01 | A kind of polycrystal silicon ingot and preparation method thereof and polysilicon chip |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014833A (en) * | 2012-12-26 | 2013-04-03 | 阿特斯(中国)投资有限公司 | Preparation method of silicon ingot |
| CN103074669A (en) * | 2013-01-29 | 2013-05-01 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method thereof and polycrystalline silicon chip |
| WO2013149560A1 (en) * | 2012-04-01 | 2013-10-10 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method thereof, and polycrystalline silicon wafer |
| CN103397378A (en) * | 2013-07-29 | 2013-11-20 | 山东大海新能源发展有限公司 | Preparation method of polycrystalline silicon ingot |
| CN103866381A (en) * | 2012-12-13 | 2014-06-18 | 阿特斯(中国)投资有限公司 | Novel directional solidification method for preparing silicon ingots with low dislocation density |
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| CN103866381A (en) * | 2012-12-13 | 2014-06-18 | 阿特斯(中国)投资有限公司 | Novel directional solidification method for preparing silicon ingots with low dislocation density |
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| CN104562193A (en) * | 2015-01-30 | 2015-04-29 | 扬州荣德新能源科技有限公司 | Casting method for polycrystalline silicon ingot |
| CN107208308A (en) * | 2015-02-05 | 2017-09-26 | 瓦克化学股份公司 | The method for preparing polysilicon |
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| CN106245113A (en) * | 2016-09-18 | 2016-12-21 | 江西赛维Ldk太阳能高科技有限公司 | A kind of polycrystal silicon ingot and preparation method thereof and polysilicon chip |
| CN107723792A (en) * | 2017-11-20 | 2018-02-23 | 江苏高照新能源发展有限公司 | A kind of preparation method of the efficient silicon ingots of the G8 of low-dislocation-density |
| CN109989108A (en) * | 2019-03-08 | 2019-07-09 | 赛维Ldk太阳能高科技(新余)有限公司 | The preparation method and polycrystal silicon ingot of a kind of seed crystal laying method, polycrystal silicon ingot |
| CN109881076A (en) * | 2019-03-12 | 2019-06-14 | 西北工业大学 | A kind of wear-resistant amorphous-dendritic composite material and preparation method thereof |
| CN109881076B (en) * | 2019-03-12 | 2021-06-08 | 西北工业大学 | A kind of wear-resistant amorphous-dendritic composite material and preparation method thereof |
| CN109811408A (en) * | 2019-03-26 | 2019-05-28 | 西安华晶电子技术股份有限公司 | Application of the silicon powder in polycrystalline silicon ingot casting preparation |
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