CN105063750A - Ga-Ge-B co-doped monocrystalline silicon and preparation method thereof - Google Patents
Ga-Ge-B co-doped monocrystalline silicon and preparation method thereof Download PDFInfo
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- CN105063750A CN105063750A CN201510492138.2A CN201510492138A CN105063750A CN 105063750 A CN105063750 A CN 105063750A CN 201510492138 A CN201510492138 A CN 201510492138A CN 105063750 A CN105063750 A CN 105063750A
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Abstract
The invention relates to Ga-Ge-B co-doped monocrystalline silicon and belongs to the technical field of production of semiconductor materials. The monocrystalline silicon is characterized in that the monocrystalline silicon is doped with three elements, namely, Ga, Ge and B, and the final atomic volume concentration of the three elements in the monocrystalline silicon is as follows: Ga: 1.02*10<15>-1.02*10<17> atoms/cm<3>, Ge: 1*10<15>-1*10<17> atoms/cm<3> and B: 1*10<16>-2*10<19> atoms/cm<3> respectively. Meanwhile, the invention further discloses a preparation method of the Ga-Ge-B co-doped monocrystalline silicon. According to the Ga-Ge-B co-doped monocrystalline silicon, B-O compounds are greatly reduced or avoided, and light degradation of batteries is reduced; in addition, the mechanical strength of cells is enhanced; the preparation method of the Ga-Ge-B co-doped monocrystalline silicon is simple, easy to operate, low in cost and capable of realizing mass production.
Description
Technical field
The present invention relates generally to a kind of gallium germanium boron and mixes silicon single crystal and preparation method thereof altogether, belongs to semi-conducting material manufacturing technical field.
Background technology
Current solar cell is raw materials used based on crystalline silicon, and wherein, the silicon single crystal prepared by vertical pulling method has the high advantage of cell conversion rate, but its complicated operation and high expensive.In addition, the oxygen mixed in straight pulling process makes the photo attenuation of monocrystalline silicon battery obvious.Polycrystalline silicon ingot casting has easy and simple to handle, lower-cost advantage, but its battery conversion efficiency is low.Quasi-monocrystalline silicon between silicon single crystal and polysilicon is emerging silicon materials, it has the advantage of silicon single crystal and polysilicon concurrently, but, not yet find the defect about how reducing in its production, improve the technology of wafer physical strength, its application industrially and popularization are restricted.
Therefore, optimize Si wafer quality by doping techniques, overcoming Defect is current comparatively effective solution.For this reason, people have carried out various trial and improvement, design the technical scheme that the doping of various silicon chip is optimized.
As being ZL200610154949.2 in the patent No., disclosing a kind of directional solidification casting polycrystalline silicon mixing germanium in the Chinese invention patent that name is called " a kind of directional solidification casting polycrystalline silicon of doped germanium ", is 1*10 containing concentration
15-1*10
17atoms/cm
3boron or phosphorus, and also containing concentration be 1*10
16-1*10
19atoms/cm
3germanium; The polysilicon of this doped germanium improves the physical strength of finished product polysilicon chip effectively, but, polysilicon area of solar cell application all the time limit to by the low speciality of its photoelectric conversion rate.
Be 200910099991.2 at application number, disclose the preparation scheme of the directionally solidified casting monocrystalline silicon that boron or gallium and germanium are mixed altogether in the Chinese invention patent application file that name is called " directionally solidified casting monocrystalline silicon mixing germanium and preparation method thereof ", containing 1*10
15-1*10
17atoms/cm
3boron or gallium or phosphorus, and 1*10
18-5*10
20atoms/cm
3germanium, solve the problem that monocrystalline silicon piece physical strength is low.But there is the high problem of optical attenuation in the single doping of boron, and the single doping of gallium makes the more difficult control of the resistivity of cell piece.
Be 201310140670.9 at application number, disclose the preparation scheme of the silicon single crystal that boron gallium is mixed altogether in the Chinese invention patent application file that name is called " boron gallium mixes monocrystalline silicon piece and preparation method thereof and solar cell altogether ", containing 10
14-10
16atoms/cm
3boron, 10
13-6*10
16atoms/cm
3gallium element, reduce the boron oxygen complex body concentration that independent boron-doping causes, reduce photo attenuation rate, but not to improve cell piece physical strength propose solution.
Be 201110173386.2 at application number, disclose the preparation scheme of the silicon single crystal that a kind of gallium indium is mixed altogether in the Chinese invention patent application file that name is called " a kind of preparation method of gallium doped monocrystaline silicon used for solar batteries ", containing 10
16-10
18atoms/cm
3gallium metal and 10
14-10
16atoms/cm
3indium metal, avoid the problem that photo attenuation rate that boron oxygen defect that boron-doping produces causes is high.But there is the high problem of cost in the electromagnetism daraf(reciprocal of farad) that this patent uses.
Summary of the invention
The present invention is directed in prior art and improve by doping the above-mentioned technical problem existed in Si wafer quality, B-Ge-codoped silicon single crystal of a kind of gallium and preparation method thereof is provided, reduce solar cell photo attenuation.
For this reason, the present invention is by the following technical solutions:
The B-Ge-codoped silicon single crystal of a kind of gallium, is characterized in that: doped with gallium, boron, germanium three kinds of elements in silicon single crystal, and the atomic volume concentration final in silicon single crystal of these three kinds of elements is respectively: gallium element 1.02*10
15-1.02*10
17atoms/cm
3, boron 1*10
15-1*10
17atoms/cm
3, element Ge 1*10
16-2*10
19atoms/cm
3.
Meanwhile, the invention also discloses a kind of method preparing the B-Ge-codoped silicon single crystal of above-mentioned gallium, comprise the steps:
S1: be placed in quartz crucible by by polycrystalline silicon material, boracic material, the raw material that jointly forms containing gallium material and germanic material;
S2: the crucible that above-mentioned raw materials is housed is placed in ingot furnace, heat after vacuumizing process, temperature-gradient method is all melted completely to above-mentioned raw materials, after mixing, regulates temperature in furnace, slowly puts into seed crystal;
S3: the seed crystal in body of heater through seeding, necking down, shouldering, isodiametric growth, finishing phase completes crystal growing process, makes monocrystalline crystal bar;
S4: the monocrystalline crystal bar made in step S3 is processed into boron gallium germanium through subsequent disposal and mixes monocrystalline silicon piece altogether, mixes monocrystaline silicon solar cell altogether for making boron gallium germanium.
Further, in step sl, the high purity elemental that described boracic material is selected the high purity elemental of more than 5N purity, selected the high purity elemental of more than 6N purity containing gallium material, more than 4N purity selected by germanic material, or the High Purity compound containing above-mentioned simple substance; Boracic material, to take according to the atom number in every cubic centimetre of finished product single crystal silicon material containing the consumption of gallium material and germanic material, i.e. gallium element 1.02*10
15-1.02*10
17atoms/cm
3, boron 1*10
15-1*10
17atoms/cm
3, element Ge 1*10
16-2*10
19atoms/cm
3.
Further, described High Purity compound is gallium silicon alloy, borosilicate alloy, germanium-silicon alloy, gallium boron alloy, gallium germanium alloy, germanium gallium alloy, gallium boron germanium alloy or gallium boron germanium-silicon alloy.
Further, in step s 2, temperature-gradient method is to 1450-1480 DEG C, make silicon raw material, boracic material, all melt containing gallium material and germanic material, meanwhile, adjustment crucible bottom temperature rise rate keeps crucible bottom temperature to be 1420-1450 DEG C, slowly put into seed crystal, described seed crystal is silicon single crystal.
Further, seed crystal in step S3 is through seeding, necking down, shouldering, isodiametric growth, finishing phase completes crystal growing process, controlling crystal rotation in whole process is 4-20rpm, and quartz crucible rotating speed is 4-20rpm, shouldering, isodiametric growth, finishing phase crystal average growth rate 30-150mm/h.
Further, vertical pulling method is adopted in step S3 by the seed crystal in body of heater through seeding, necking down, shouldering, isodiametric growth, finishing phase completes crystal growing process, make monocrystalline crystal bar, and in S3 in crystal growing process single crystal growing direction be <100> direction.
Further, described in step S4, subsequent disposal comprises evolution, tail of decaptitating, grinding, chamfering, section and matting.
Further, the photo attenuation degree that the boron gallium germanium made in step S4 mixes monocrystaline silicon solar cell is altogether 0.5%-2.5%.
Compared with prior art, the present invention has following beneficial effect:
Gallium germanium boron in the present invention mixes silicon single crystal altogether, due to the effect that boron gallium in silicon crystal is mixed altogether, greatly reduces or avoids the generation of boron oxygen complex body, reduce the photo attenuation of battery; Germanium metal mix the physical strength significantly improving cell piece, be the ideal material of high efficiency solar cell; Meanwhile, the preparation method that gallium germanium boron provided by the invention mixes silicon single crystal is altogether easy, easy to operate, and cost is low to be produced on a large scale.
Embodiment
In order to make those skilled in the art person better understand the present invention program, below in conjunction with specific embodiment, clear, complete description is carried out to technical scheme of the present invention.
The B-Ge-codoped silicon single crystal of gallium of the present invention, is characterized in that: doped with gallium, boron, germanium three kinds of elements in silicon single crystal, and the atomic volume concentration final in silicon single crystal of these three kinds of elements is respectively: gallium element 1.02*10
15-1.02*10
17atoms/cm
3, boron 1*10
15-1*10
17atoms/cm
3, element Ge 1*10
16-2*10
19atoms/cm
3.
Another aspect of the present invention, provide a kind of method preparing the B-Ge-codoped silicon single crystal of above-mentioned gallium, specific embodiment is as follows:
Embodiment 1:
The raw material be jointly made up of polycrystalline silicon material, borosilicate alloy, gallium silicon alloy and germanium metal is placed in quartz crucible, wherein, the consumption of borosilicate alloy, gallium silicon alloy and germanium metal takes according to the atom number in every cubic centimetre of finished product single crystal silicon material, gallium element 1.02*10
15atoms/cm
3, boron 1*10
15atoms/cm
3, element Ge 1*10
16atoms/cm
3, surplus is polycrystalline silicon material, the crucible that above-mentioned raw materials is housed is placed in czochralski crystal growing furnace, system vacuumizes heating, control in-furnace temperature and be progressively elevated to 1450 DEG C, make melting sources, after abundant mixing, stablize melt temperature at 1420 DEG C, slowly put into seed crystal, thermograde in regulating stove is constant, through seeding, necking down, shouldering, isodiametric growth, finishing phase, in whole process, control crystal rotation is 8rpm, crucible rotation is 6rpm, after necking down, crystalline growth velocity is reduced to 50mm/h by 70mm/h, boule diameter reaches requirement and completes a turn shoulder, and then raising crystalline growth velocity continues isodiametric growth to 60mm/h, last finishing phase improves crystalline growth velocity to 150mm/h, complete crystal growth, whole process crystal grows along <100> crystal orientation.
After cooling, in crystal, the concentration of boron is 9.2*10
15-9*10
16atoms/cm
3, the concentration of gallium is 1.02*10
15atoms/cm
3, the concentration of germanium is 1*10
16-1*10
17atoms/cm
3.Through making herbs into wool, diffusion, etching, plated film, printing and sintering process are made as boron gallium germanium and mix monocrystaline silicon solar cell altogether.Be 60kWh/m in irradiation
2under, recording photo attenuation rate is 0.9%.
embodiment 2:
The raw material be jointly made up of polycrystalline silicon material, borosilicate alloy, gallium germanium alloy and germanium metal is placed in quartz crucible, wherein, the consumption of borosilicate alloy, gallium germanium alloy and germanium metal takes according to the atom number in every cubic centimetre of finished product single crystal silicon material, gallium element 5*10
16atoms/cm
3, boron 1*10
16atoms/cm
3, element Ge 1*10
18atoms/cm
3, surplus is polycrystalline silicon material, the crucible that above-mentioned raw materials is housed is placed in czochralski crystal growing furnace, system vacuumizes heating, control in-furnace temperature and be progressively elevated to 1450 DEG C, make melting sources, after abundant mixing, stablize melt temperature at 1420 DEG C, slowly put into seed crystal, thermograde in regulating stove is constant, through seeding, necking down, shouldering, isodiametric growth, finishing phase, in whole process, control crystal rotation is 5rpm, crucible rotation is 5rpm, after necking down, crystalline growth velocity has 70mm/h to be reduced to 40mm/h, boule diameter reaches requirement and completes a turn shoulder, and then raising crystalline growth velocity continues isodiametric growth to 50mm/h, last finishing phase improves crystalline growth velocity to 150mm/h, complete crystal growth, whole process crystal grows along <100> crystal orientation.
After cooling, obtain the B-Ge-codoped silicon single crystal of gallium containing gallium, boron, germanium three kinds of elements, through making herbs into wool, diffusion, etching, plated film, printing and sintering process are made as boron gallium germanium and mix monocrystaline silicon solar cell altogether.Be 60kWh/m in irradiation
2under, recording photo attenuation rate is 0.8%.
embodiment 3:
The raw material be jointly made up of polycrystalline silicon material, borosilicate alloy, gallium boron alloy and germanium metal is placed in quartz crucible, wherein, the consumption of borosilicate alloy, gallium boron alloy and germanium metal takes according to the atom number in every cubic centimetre of finished product single crystal silicon material, gallium element 2*10
16atoms/cm
3, boron 4*10
16atoms/cm
3, element Ge 1*10
17atoms/cm
3, surplus is polycrystalline silicon material, the crucible that above-mentioned materials is housed is placed in czochralski crystal growing furnace, system vacuumizes heating, control in-furnace temperature and be progressively elevated to 1460 DEG C, it is melting sources, abundant mixing stablizes melt temperature afterwards at 1430 DEG C, slowly put into seed crystal, thermograde in regulating stove is constant, through seeding, necking down, shouldering, isodiametric growth, finishing phase, in whole process, control crystal rotation is 10rpm, crucible rotation is 10rpm, after necking down, crystalline growth velocity has 60mm/h to be reduced to 38mm/h, boule diameter reaches requirement and completes a turn shoulder, and then raising crystalline growth velocity continues isodiametric growth to 48mm/h, last finishing phase improves crystalline growth velocity to 130mm/h, complete crystal growth, whole process crystal grows along <100> crystal orientation.
After cooling, obtain the B-Ge-codoped silicon single crystal of gallium containing gallium, boron, germanium three kinds of elements, through making herbs into wool, diffusion, etching, plated film, printing and sintering process are made as boron gallium germanium and mix monocrystaline silicon solar cell altogether.Be 60kWh/m in irradiation
2under, recording photo attenuation rate is 0.7%.
Embodiment 4:
The raw material be jointly made up of polycrystalline silicon material, borosilicate alloy, gallium silicon alloy and germanium-silicon alloy is placed in quartz crucible, wherein, the consumption of borosilicate alloy, gallium silicon alloy and germanium-silicon alloy takes according to the atom number in every cubic centimetre of finished product single crystal silicon material, gallium element 1*10
17atoms/cm
3, boron 1*10
17atoms/cm
3, element Ge 1*10
19atoms/cm
3, surplus is polycrystalline silicon material, the crucible that above-mentioned raw materials is housed is placed in czochralski crystal growing furnace, system vacuumizes heating, control in-furnace temperature and be progressively elevated to 1450 DEG C, make melting sources, after abundant mixing, stablize melt temperature at 1420 DEG C, slowly put into seed crystal, thermograde in regulating stove is constant, through seeding, necking down, shouldering, isodiametric growth, finishing phase, in whole process, control crystal rotation is 12rpm, crucible rotation is 8rpm, after necking down, crystalline growth velocity has 80mm/h to be reduced to 70mm/h, boule diameter reaches requirement and completes a turn shoulder, and then raising crystalline growth velocity continues isodiametric growth to 70mm/h, last finishing phase improves crystalline growth velocity to 120mm/h, complete crystal growth, whole process crystal grows along <100> crystal orientation.
After cooling, obtain the B-Ge-codoped silicon single crystal of gallium containing gallium, boron, germanium three kinds of elements, through making herbs into wool, diffusion, etching, plated film, printing and sintering process are made as boron gallium germanium and mix monocrystaline silicon solar cell altogether.Be 60kWh/m in irradiation
2under, recording photo attenuation is 2%.
Obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, should belong to the scope of protection of the invention.
Claims (9)
1. the B-Ge-codoped silicon single crystal of gallium, is characterized in that: doped with gallium, boron, germanium three kinds of elements in silicon single crystal, and the atomic volume concentration final in silicon single crystal of these three kinds of elements is respectively: gallium element 1.02*10
13-1.02*10
17atoms/cm
3, boron 1*10
15-1*10
17atoms/cm
3, element Ge 1*10
16-2*10
19atoms/cm
3.
2. prepare a method for the B-Ge-codoped silicon single crystal of gallium according to claim 1, comprise the steps:
S1: be placed in quartz crucible by by polycrystalline silicon material, boracic material, the raw material that jointly forms containing gallium material and germanic material;
S2: the crucible that above-mentioned raw materials is housed is placed in ingot furnace, heat after vacuumizing process, temperature-gradient method is all melted completely to above-mentioned raw materials, after mixing, regulates temperature in furnace, slowly puts into seed crystal;
S3: the seed crystal in body of heater through seeding, necking down, shouldering, isodiametric growth, finishing phase completes crystal growing process, makes monocrystalline crystal bar;
S4: the monocrystalline crystal bar made in step S3 is processed into boron gallium germanium through subsequent disposal and mixes monocrystalline silicon piece altogether, mixes monocrystaline silicon solar cell altogether for making boron gallium germanium.
3. prepare the method for the B-Ge-codoped silicon single crystal of gallium according to claim 2, it is characterized in that: in step sl, the high purity elemental that described boracic material is selected the high purity elemental of more than 5N purity, selected the high purity elemental of more than 6N purity containing gallium material, more than 4N purity selected by germanic material, or the High Purity compound containing above-mentioned simple substance; Described boracic material, to take according to the atom number in every cubic centimetre of finished product single crystal silicon material containing the consumption of gallium material and germanic material, i.e. gallium element 1.02*10
15-1.02*10
17atoms/cm
3, boron 1*10
15-1*10
17atoms/cm
3, element Ge 1*10
16-2*10
19atoms/cm
3.
4. prepare the method for the B-Ge-codoped silicon single crystal of gallium according to claim 3, it is characterized in that: described High Purity compound is gallium silicon alloy, borosilicate alloy, germanium-silicon alloy, gallium boron alloy, gallium germanium alloy, germanium gallium alloy, gallium boron germanium alloy or gallium boron germanium-silicon alloy.
5. prepare the method for the B-Ge-codoped silicon single crystal of gallium according to claim 2, it is characterized in that: in step s 2, temperature-gradient method is to 1450-1480 DEG C, make silicon raw material, boracic material, all melt containing gallium material and germanic material, simultaneously, adjustment crucible bottom temperature rise rate keeps crucible bottom temperature to be 1420-1450 DEG C, and slowly put into seed crystal, described seed crystal is silicon single crystal.
6. prepare the method for the B-Ge-codoped silicon single crystal of gallium according to claim 2, it is characterized in that: the seed crystal in step S3 is through seeding, necking down, shouldering, isodiametric growth, finishing phase completes crystal growing process, controlling crystal rotation in whole process is 4-20rpm, and quartz crucible rotating speed is 4-20rpm, shouldering, isodiametric growth, finishing phase crystal average growth rate 30-150mm/h.
7. prepare the method for the B-Ge-codoped silicon single crystal of gallium according to claim 2, it is characterized in that: adopt vertical pulling method in step S3 by the seed crystal in body of heater through seeding, necking down, shouldering, isodiametric growth, finishing phase completes crystal growing process, makes monocrystalline crystal bar, and in S3 in crystal growing process single crystal growing direction be <100> direction.
8. prepare the method for the B-Ge-codoped silicon single crystal of gallium according to claim 2, it is characterized in that: described in step S4, subsequent disposal comprises evolution, tail of decaptitating, grinding, chamfering, section and matting.
9. prepare the method for the B-Ge-codoped silicon single crystal of gallium according to claim 2, it is characterized in that: the photo attenuation degree that the boron gallium germanium made in step S4 mixes monocrystaline silicon solar cell is altogether 0.5%-2.5%.
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| CN110202419A (en) * | 2019-05-31 | 2019-09-06 | 北京通美晶体技术有限公司 | Single germanium wafer, its preparation method, the purposes of the preparation method of crystal bar and single-chip |
| CN111910248A (en) * | 2020-07-14 | 2020-11-10 | 江苏协鑫硅材料科技发展有限公司 | Ingot casting single crystal seed crystal, cast single crystal silicon ingot and preparation method thereof, cast single crystal silicon slice and preparation method thereof |
| CN111910248B (en) * | 2020-07-14 | 2022-02-18 | 江苏协鑫硅材料科技发展有限公司 | Ingot casting single crystal seed crystal, cast single crystal silicon ingot and preparation method thereof, cast single crystal silicon slice and preparation method thereof |
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