CN101812728A - Preparation method of n-type crystalline silicon - Google Patents
Preparation method of n-type crystalline silicon Download PDFInfo
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- CN101812728A CN101812728A CN 201010148437 CN201010148437A CN101812728A CN 101812728 A CN101812728 A CN 101812728A CN 201010148437 CN201010148437 CN 201010148437 CN 201010148437 A CN201010148437 A CN 201010148437A CN 101812728 A CN101812728 A CN 101812728A
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Abstract
The invention discloses a preparation method of n-type crystalline silicon, which is characterized in that during the manufacturing process of a polycrystalline silicon ingot or the crystal growth process of a single crystal silicon rod, a DC electric field which is parallel with the crystal growth direction is applied on molten silicon liquid, so that doping in liquid phase are shifted to the solid-liquid interface direction; under the double action of the electric field and solidification segregation, a high-concentration area is formed in the liquid phase of a crystal growth tip, thereby improving the doping content of the follow-up grown crystal, weakening the impact of solidification segregation, obtaining the n-type polycrystalline silicon ingot or the n-type single crystal silicon rod which is uniformly doped in the crystal growth direction, reducing the deviation range of resistivity, improving the product pass rate, so as to reduce the manufacturing cost of an n-type silicon chip. The method is particularly applicable in manufacturing P-, As- or Sb-doped n-type polycrystalline silicon ingots or n-type single crystal silicon rods.
Description
Technical field
The present invention relates to the growth method of crystalline silicon, specifically be meant a kind of method of n N-type waferN silicon.
Background technology
Crystal-silicon solar cell (comprising monocrystalline and polycrystalline) is the main product of photovoltaic generation, the silicon chip of producing battery is to obtain from polycrystal silicon ingot or silicon single crystal rod section, so the electric property that silicon chip requires must be finished in the production process of polycrystalline ingot casting or single crystal rod, usually doped with II I family element obtains the p N-type semiconductorN in the crystalline silicon process of growth, the doping V group element obtains the n N-type semiconductorN, and makes the resistivity of silicon chip be controlled at the requirement of satisfying the preparation solar cell between 0.5～3 Ω cm by regulating doping content.Doping as silicon must form a shallow energy level in the band gap of silicon, and has the advantages that solid solubility is big, spread coefficient is little and steam forces down.The energy level of doping agent has determined the characteristic of semiconductor of material, and solid solubility is too little can only be used when the preparation high ohmic semiconductor, and the Modulatory character and the stability of spread coefficient and vapour pressure and crystal growth are closely related.
Another important indicator of choosing doping agent is its equilibrium segregation coefficient (k in silicon
0), from the angle of crystal growth, the equilibrium segregation coefficient of doping agent approaches 1 more, and its segregation in crystal growing process is more little, and then the doping content distribution is even more on crystal growth direction, thus the yield rate that satisfies the electric property requirement is also just high more.Under the prerequisite that improves yield rate and reduce production costs, that solar cell uses at present nearly all is boron (B, k
0=0.8) doped p type silicon chip is because the equilibrium segregation coefficient maximum of B in all elements.But oxygen (O) residual in B and the crystal forms the B-O complex body easily under illumination condition, form B-Fe with impurity iron (Fe) and combine, and makes battery light occur to relaxation phenomenon, has reduced the efficiency of conversion of battery.
N N-type waferN silion cell has longer minority carrier life time than p type battery, and battery making temperature is low simultaneously, meets low cost, high yield, high efficiency demand for development, therefore is subjected to the generally attention of countries in the world.The technology of preparing of n N-type waferN silicon solar cell has obtained developing rapidly in recent years, adopts the battery conversion efficiency of the high resistant n type wafer production of some contact technique to reach 20.1%, 156cm
2The n type polycrystal silicon cell efficiency of conversion of specification reaches 16.4%.
N N-type waferN silicon is mixed by V group element usually and obtains, and that the most frequently used is phosphorus (P, k
0=0.35) mixes the V group element beyond the phosphorus, nitrogen (N, k
0=0.0007), arsenic (As, k
0=0.3), antimony (Sb, k
0=0.023) and bismuth (Bi, k
0=0.0007) among, N exists with molecularity in crystal, makes crystal present thundering electrology characteristic, is not used to usually mix; Bi is not used because of its metallic character and less equilibrium segregation coefficient yet.But the equilibrium segregation coefficient of P, As and Sb is all little than B, so their the segregation degree when crystal growth is more serious than B, if adopt existing polycrystalline ingot casting and monocrystalline growing process, the yield rate of product must descend, and increases production cost.
Magnetic field crystal pulling (MCZ) technology is adopted in Chinese patent application number 85100591 propositions, outside crystal growing apparatus, apply a transverse magnetic field, make conductive melt velocity component cutting magnetic line perpendicular to field direction in flow process produce induced current, under the acting in conjunction of induced current and externally-applied magnetic field, produce the lorentz's force opposite with conductive melt direction of motion, increase the magnetic viscous force of melt, weaken flowing of melt, reduce melt temperature and rise and fall and liquid fluctuating, thus the content and the distribution of impurity in the control crystal.Although the MCZ method has improved the homogeneity that doping content distributes to a certain extent, the silicon single crystal rod specification of producing is less, can not satisfy the requirement of solar cell low cost production.
United States Patent (USP) 2008002919 and Japanese Patent 2002128591 have proposed a kind of resistivity compensation method respectively, in crystal growing process, an amount of transoid doping is added in the silicon liquid with main the doping, utilize transoid to be entrained in the main little characteristics of mixing of segregation coefficient ratio in the silicon crystal, the main resistivity decreased that causes because of solidifying segregation of mixing is compensated, the product percent of pass that satisfies the resistivity index is increased.Although this compensative material satisfies the requirement of cell preparation aspect resistivity, reduced the comprehensive electric property of silicon chip.
Summary of the invention
Problem based on above-mentioned prior art existence, the preparation method who the purpose of this invention is to provide the uniform n N-type waferN of a kind of doping content and resistivity distribution silicon, this method are particularly useful for making the preparation with P, As or Sb doped n type polycrystal silicon ingot or n type silicon single crystal rod.
Technical scheme of the present invention is in crystal growing process, a DC electric field that is parallel to crystal growth direction is put on molten silicon liquid, doping in the liquid phase is moved to the solid-liquid interface direction, under the dual function of electric field and solidifying segregation, in the liquid phase of crystal growth tip, form an area with high mercury of doping enrichment, improved subsequent growth crystalline doping content, weakened the influence of solidifying segregation, acquisition is even doped n type polycrystalline ingot or n type single crystal rod on crystal growth direction, and reduced the deviation range of resistivity, improve product percent of pass, thereby reduced the manufacturing cost of n type silicon chip.
The preparation method of a kind of n N-type waferN silicon of the present invention, it is characterized in that: in crystal growing process, molten silicon liquid is applied a DC electric field that is parallel to crystal growth direction, under the Collaborative Control of temperature field and electric field, finish crystal growth, obtain to be entrained in crystal growth direction equally distributed n type polycrystal silicon ingot or n type silicon single crystal rod.
Described n N-type waferN silicon is meant with one or more the n N-type waferN silicon that mix and form among P, As and the Sb.
Described crystal growth is meant the polycrystalline silicon ingot casting that adopts directional freeze or adopts CZ (Czochralski) method pulling monocrystal or adopt FZ (Float-Zone) method growing single-crystal.
The described DC electric field that is parallel to crystal growth direction is meant that direction of an electric field is identical with crystal growth direction; The voltage of its electric field is that 0.1～10V or current density are 0.1～10A/cm
2Used power supply can be current stabilization direct current, voltage stabilizing direct current or other direct current form.
The Collaborative Control of described temperature field and electric field is to be the main control crystalline speed of growth with the temperature field, and DC electric field intensity does not influence the temperature field with the joule heating of its generation and is advisable.
The present invention distinguishes with traditional n N-type waferN growth phase ratio and is:
Do not having under the situation of electric field, being entrained in crystal begins to be the chaotic distribution state before the growth in silicon liquid, along with crystal begins growth, the solidifying segregation effect makes enrichment gradually in the liquid phase be entrained in the crystal growth tip, under motivating force effects such as concentration gradient and convection current, in whole liquid phase, spread gradually simultaneously, finally reach a dynamic equilibrium state, referring to Fig. 1.Along with the carrying out of crystal growth, the enrichment degree that is entrained in the crystal growth tip liquid phase raises gradually, makes the also corresponding rising of crystalline doping content, the doping content of the crystal that obtains on the direction of growth present the regularity of distribution shown in Figure 2.
When applying DC electric field, because being entrained in, n types such as P, As and Sb present anion characteristic in the silicon liquid, so when direction of an electric field is identical with crystal growth direction, doping will be moved to the solid-liquid interface direction of crystal growth.By regulating the size of strength of electric field, not only can weaken the influence of concentration gradient and convection current, can also make to be entrained in the enrichment of solid-liquid interface place in the liquid phase, to such an extent as to be lower than starting point concentration C away from doping content in the liquid phase of solid-liquid interface
0, referring to Fig. 1.Under the dual function of solidifying segregation and electrical forces, to exceed a lot when adulterated enrichment degree ratio does not have electric field action in the liquid phase of crystal growth tip, make subsequent growth crystalline doping content improve, therefore begin to reach soon ideal doping content C in crystal growth
0, keep that adulterated enrichment degree can obtain the equally distributed n N-type waferN of doping content silicon on crystal growth direction, as shown in Figure 2 in same level in the crystal growth tip liquid phase.
Method of the present invention has the following advantages:
1) method of the present invention is applicable to existing crystal growth technique, comprises directional freeze polycrystalline silicon casting ingot process, CZ farad monocrystalline technology and FZ method monocrystalline growing process, but not only is confined to these crystal growth patterns.
2) have stronger handiness, can be entrained in size and electronegative strong and weak suitable DC electric field intensity of selecting of equilibrium segregation coefficient in the silicon, can improve these and be entrained in homogeneity on the crystal growth direction according to selected n type.
3) the sub-fraction that begins and finish except that crystal growth, uniform doping distributes on crystal growth direction, and deviation is very little, compare the yield rate that this method of the brilliant technology of existing length has greatly improved material, reduce the production cost of silicon chip, thereby make the production application of n type silicon chip on cost, have feasibility.
Description of drawings
Fig. 1 is the distribution schematic diagram of doping content at the solid-liquid interface place;
Fig. 2 be in the crystal doping content with the distribution schematic diagram of growing height;
Fig. 3 is that the electric field of polysilicon directional freezing ingot casting is provided with synoptic diagram;
Fig. 4 adopts the electric field of CZ method pulling monocrystal that synoptic diagram is set;
Fig. 5 adopts the electric field of FZ method growing single-crystal that synoptic diagram is set.
Each label is among the figure: 1 is crucible; 2 is silicon liquid; 3 is growing crystal; 4 are the doping of n type; 5 is crystal fusion; 11 is direct supply; 12 is lead; 13 is negative electrode; 14 is anode; 20 is induction coil.
Embodiment
Below in conjunction with drawings and Examples the specific embodiment of the present invention is described in further detail:
Under the DC electric field effect, adopt directional solidification processes to prepare n type polycrystal silicon ingot,, adopt following steps to realize referring to Fig. 3:
1) requires to calculate the required doping content of corresponding silicon material according to the silicon chip electric property, the preparation doping agent.
2) in crucible 1 bottom anode 14 is set, silicon material and doping agent are put into crucible according to a certain percentage, negative electrode 13 is set above the silicon material then, with lead 12 positive pole of anode 14 with direct supply 11 linked to each other, negative electrode 13 links to each other with negative pole.Note making direction of an electric field parallel with the crystalline direction of growth during arrangement of electrodes, anode 14 and negative electrode 13 adopt high purity graphite to make, and lead 12 adopts high-purity molybdenum filament.
3) the attemperation Controlling System is adjusted the position of negative electrode 13 with silicon material heat fused, makes the negative electrode 13 and the liquid level of silicon liquid 2 keep good Ohmic contact.Keep the molten state of silicon liquid 2, begin to apply DC electric field, interelectrode voltage is that 0.1～10V or current density are 0.1～10A/cm
2Arbitrary value in interval makes the direction migration of 4 anode 14 of mixing of n type, and keeps static more than 1 hour, allows be entrained in the abundant enrichment of anode region.
4) regulate temperature control system, carry out crystal growth, in crystal growth, keep DC electric field, make that adulterated enrichment degree maintains same level in the solid-liquid interface place liquid phase, solidify fully up to silicon liquid 2 with the speed of 5～50mm/h.
5) processing mode of steps such as remaining thermal treatment, cooling is the same with traditional directional freeze casting ingot process.Part excision silicon ingot bottom doping content is on the low side and the top doping content is higher, and the edge section that contacts with crucible 1 of excision can obtain than the more uniform n type of traditional directional freeze dopant profiles polycrystal silicon ingot.
Directional freeze mode under the DC electric field effect, the electric field setting also not only is confined to illustrational a kind of form, also can adopt the container of high purity graphite crucible as carrying silicon liquid, coats insulation layer at the crucible periphery, crucible bottom is used as anode, or adopts other similar mode.
Under the DC electric field effect, adopt CZ farad system n type silicon single crystal rod,, adopt following steps to realize referring to Fig. 4:
1) requires to calculate the required doping content of corresponding silicon material according to the silicon chip electric property, the preparation doping agent.
2) crucible made from high purity graphite 1 is a negative electrode, is connected to lead 12 on the negative pole of power supply 11; Silicon material and doping agent are put into crucible 1 according to a certain percentage, and heating makes silicon material fusing, adjusts temperature control system and begins to lift, and grows into isodiametric growth after the stage finishing necking down and shouldering, is that anode is connected on the positive pole of power supply 11 with growing crystal 3.
3) begin silicon liquid 2 is applied DC electric field, interelectrode voltage is that 0.1～10V or current density are 0.1～10A/cm
2Arbitrary value in interval makes n type doping 4 liquid phase region domain migration, enrichments to the crystal growth tip.
4) carry out crystal growth with the speed of 5～50mm/h, in crystal growth, keep DC electric field, make that adulterated enrichment degree maintains same level in the solid-liquid interface place liquid phase, stop to apply electric field after entering the afterbody growth phase.
5) subsequent processing steps is identical with the technology of existing CZ method pulling monocrystal.With the head and the afterbody excision of silicon single crystal rod, can obtain then than the more uniform n type of traditional C Z method dopant profiles silicon single crystal rod.
CZ farad crystal type under the DC electric field effect, the electric field setting not only is confined to illustrational a kind of form, also can adopt quartz crucible as silicon liquid carrying container, in crucible bottom and side electrode is set, or adopts other similar mode.
Under the DC electric field effect, adopt FZ manufactured n type silicon single crystal rod,, adopt following steps to realize referring to Fig. 5:
1) require to calculate the required doping content of corresponding silicon material according to the silicon chip electric property, doping agent can be added in advance in the silicon rod 5 fusion or in the molten process in district and add.
2) supposition induction coil 20 moves from bottom to top, with growing crystal 3 as anode, crystal 5 fusion as negative electrode, be connected respectively to lead 12 on the positive pole and negative pole of power supply 11.
3) strengthen the part heating and melting of the power of induction coil 20 with silicon rod 5 fusion, begin then silicon liquid 2 is applied DC electric field, interelectrode voltage is that 0.1～10V or current density are 0.1～10A/cm
2Arbitrary value in interval makes n type doping 4 liquid phase region domain migration, enrichments to the crystal growth tip.
4) carry out crystal growth with the speed of 5～50mm/h, in crystal growth, keep DC electric field, make that adulterated enrichment degree maintains same level in the solid-liquid interface place liquid phase, stop to apply electric field after entering the afterbody growth phase.
5) other treatment step is identical with the long brilliant technology of existing FZ method.With the head and the afterbody excision of silicon single crystal rod, can obtain then than the more uniform n type of traditional F Z method dopant profiles silicon single crystal rod.
Claims (5)
1. the preparation method of a n N-type waferN silicon, it is characterized in that: in crystal growing process, molten silicon liquid is applied a DC electric field that is parallel to crystal growth direction, under the Collaborative Control of temperature field and electric field, finish crystal growth, obtain even doped n type polycrystal silicon ingot or n type silicon single crystal rod on crystal growth direction.
2. according to the preparation method of a kind of n N-type waferN silicon of claim 1, it is characterized in that: described n N-type waferN silicon is meant to be mixed by among P, As and the Sb one or more and forms.
3. according to the preparation method of a kind of n N-type waferN silicon of claim 1, it is characterized in that: described crystal growth is meant polycrystalline silicon ingot casting or CZ method pulling monocrystal or the FZ method growing single-crystal that adopts directional freeze.
4. according to the preparation method of a kind of n N-type waferN silicon of claim 1, it is characterized in that: the described DC electric field that is parallel to crystal growth direction is meant that direction of an electric field is identical with crystal growth direction; The voltage of its electric field is that 0.1～10V or current density are 0.1～10A/cm
2Used power supply is current stabilization direct current or voltage stabilizing direct current.
5. according to the preparation method of a kind of n N-type waferN silicon of claim 1, it is characterized in that: the Collaborative Control of described temperature field and electric field is to be the main control crystalline speed of growth with the temperature field, and DC electric field intensity does not influence the temperature field with the joule heating of its generation and is advisable.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021650A (en) * | 2010-12-31 | 2011-04-20 | 常州天合光能有限公司 | Production method of large polycrystalline ingot |
| CN102732960A (en) * | 2011-04-14 | 2012-10-17 | 浙江昱辉阳光能源有限公司 | Method and system for testing crystalline silicon growth rate |
| CN104846435A (en) * | 2015-06-02 | 2015-08-19 | 江苏协鑫硅材料科技发展有限公司 | P type gallium-doped crystalline silicon and preparation method thereof |
| CN107164802A (en) * | 2017-04-12 | 2017-09-15 | 济南大学 | A kind of method that electrostatic field aids in polycrystalline silicon ingot casting |
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| JPS5490086A (en) * | 1977-12-28 | 1979-07-17 | Toshiba Corp | Method of producing single crystal |
| JPH08259382A (en) * | 1995-03-24 | 1996-10-08 | Res Dev Corp Of Japan | Growing method for si single crystal by controlling melt convection current |
| CN101319364A (en) * | 2008-06-03 | 2008-12-10 | 天津市环欧半导体材料技术有限公司 | Process for preparing gallium doped elementarysubstance solar energy single crystal |
| US20090255456A1 (en) * | 2008-04-10 | 2009-10-15 | Shunji Kuragaki | Method for evaluating metal contamination of silicon single crystal |
| WO2009136464A1 (en) * | 2008-05-08 | 2009-11-12 | 信越半導体株式会社 | Method for growing single crystal and apparatus for pulling up single crystal |
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2010
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5490086A (en) * | 1977-12-28 | 1979-07-17 | Toshiba Corp | Method of producing single crystal |
| JPH08259382A (en) * | 1995-03-24 | 1996-10-08 | Res Dev Corp Of Japan | Growing method for si single crystal by controlling melt convection current |
| US20090255456A1 (en) * | 2008-04-10 | 2009-10-15 | Shunji Kuragaki | Method for evaluating metal contamination of silicon single crystal |
| WO2009136464A1 (en) * | 2008-05-08 | 2009-11-12 | 信越半導体株式会社 | Method for growing single crystal and apparatus for pulling up single crystal |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021650A (en) * | 2010-12-31 | 2011-04-20 | 常州天合光能有限公司 | Production method of large polycrystalline ingot |
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| CN102732960A (en) * | 2011-04-14 | 2012-10-17 | 浙江昱辉阳光能源有限公司 | Method and system for testing crystalline silicon growth rate |
| CN102732960B (en) * | 2011-04-14 | 2015-07-08 | 浙江昱辉阳光能源有限公司 | Method and system for testing crystalline silicon growth rate |
| CN104846435A (en) * | 2015-06-02 | 2015-08-19 | 江苏协鑫硅材料科技发展有限公司 | P type gallium-doped crystalline silicon and preparation method thereof |
| CN107164802A (en) * | 2017-04-12 | 2017-09-15 | 济南大学 | A kind of method that electrostatic field aids in polycrystalline silicon ingot casting |
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Open date: 20100825 |