CN101812726A - Method for preparing gallium-doped p-type crystalline silicon - Google Patents
Method for preparing gallium-doped p-type crystalline silicon Download PDFInfo
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Abstract
The invention discloses a method for preparing Ga-doped p-type crystalline silicon. The method is characterized in that a DC electric field parallel to a crystal growth direction is applied to molten silicon liquid during the crystal growth of polycrystalline silicon ingots or monocrystalline silicon rods so as to allow Ga dopant in liquid phase to migrate to a liquid-solid interface; under the dual action of the electric field and solidification segregation, a Ga high-concentration area is formed in the liquid phase of a crystal growth apex so as to improve the doping concentration of subsequently growing crystals, weaken the influence of solidification segregation and obtain p-type polycrystalline ingots or p-type monocrystalline rods of which the Ga content is uniformly distributed in the crystal growth direction; the deviation range of resistivity is reduced; the yield of materials is improved, so that the production cost of silicon chips is reduced and the industrial application of Ga-doped p-type silicon chips has cost feasibility. Meanwhile, the method also applies to the p-type doping with small segregation coefficient of Al, In and the like.
Description
Technical field
The present invention relates to the growth method of crystalline silicon, specifically be meant the preparation method of a kind of gallium (Ga) doped p-type crystalline 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 long brilliant process, usually doped with II I family element obtains p type silicon in the crystalline silicon process of growth, the doping V group element obtains n type silicon, 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.Adulterated energy level has determined the characteristic of semiconductor of material, and solid solubility is too little can only be used when the preparation high-resistance semi-conductor, and the Modulatory character and the stability of spread coefficient and vapour pressure and crystal growth are closely related.
Choose adulterated another important indicator and be its equilibrium segregation coefficient (k in silicon
0), from the angle of crystal growth, adulterated equilibrium segregation coefficient approaches 1 more, and its segregation in crystal growing process is more little, and then the doping content distribution is even more on the 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, because the equilibrium segregation coefficient maximum of B in all elements, other III family element beyond the boron is as aluminium (Al, k
0=0.002), gallium (Ga, k
0=0.008), indium (In, k
0=0.0004), all too little because of segregation coefficient, segregation is serious, the finished product rate is too low and use hardly.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.Therefore wish that substituting B with Ga prepares p type silicon chip, avoid the efficiency of conversion of light to relaxation phenomenon, raising battery.But the segregation coefficient of Ga is little more a lot of than B, if adopt existing polycrystalline casting ingot process or monocrystalline growing process, this serious Ga segregation phenomena will occur, must reduce yield rate, the increase production cost of product.
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 is to a certain degree suppressing the concentration distribution inequality that the doping segregation causes, the silicon single crystal rod specification that the MCZ method is produced is less, cost is high, is not suitable for 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
Based on the problem that above-mentioned prior art exists, the purpose of this invention is to provide the preparation method of the uniform Ga doped p-type crystalline silicon of a kind of doping content and resistivity distribution.
Technical scheme
Technical scheme of the present invention is in the crystal growing process of making polycrystal silicon ingot or silicon single crystal rod, a DC electric field that is parallel to crystal growth direction is put on molten silicon liquid, Ga 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 the area with high mercury of a Ga, improved subsequent growth crystalline Ga content, weakened the influence of solidifying segregation, acquisition is Ga content equally distributed p type polycrystalline ingot or p type single crystal rod on crystal growth direction, and reduced the deviation range of resistivity, improved the yield rate of material, thereby reduce the production cost of silicon chip, make the industry of Ga doped p type silicon chip be applied in and have feasibility on the cost.
The preparation method of a kind of Ga doped p-type crystalline 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 the Ga uniform doping distributes on crystal growth direction p N-type waferN silicon ingot or p type silicon single crystal rod.
Described crystal growth mainly 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, its direction of an electric field is opposite with crystal growth direction; Its voltage of 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 control of described temperature field and electric field synergistic 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 compares difference and is with traditional crystal growth:
Do not having under the situation of electric field, Ga is entrained in crystal to begin to be the chaotic distribution state before the growth in silicon liquid, along with crystal begins growth, the solidifying segregation effect makes Ga enrichment gradually in the liquid phase of 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 of Ga in crystal growth tip liquid phase raises gradually, makes the also corresponding rising of crystalline doping content, the crystal that obtains doping content of Ga on the direction of growth present the regularity of distribution shown in Figure 2.
When applying DC electric field, because Ga is entrained in the silicon liquid and presents cationic characteristic, so when direction of an electric field is opposite with crystal growth direction, Ga will move 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 the Ga in the liquid phase be entrained in the enrichment of solid-liquid interface place, to such an extent as to be lower than starting point concentration C away from Ga concentration 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 the enrichment degree of Ga 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, the enrichment degree of keeping Ga in the crystal growth tip liquid phase can obtain the equally distributed p N-type waferN of Ga content silicon on crystal growth direction, as shown in Figure 2 in same level.
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) method of the present invention is mixed suitable too not only for the production of Ga doped p N-type waferN silicon provides feasibility to the little p type of fractional condensation coefficients such as Al, In.
3) crystalline silicon that adopts the inventive method to grow, as shown in Figure 2, except that the sub-fraction that crystal growth begins and finishes, Ga content uniform distribution on crystal growth direction, and doping content maintains the ideal level, 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 Ga doped p type silicon chip on cost, have feasibility.
Description of drawings
Fig. 1 is the concentration distribution synoptic diagram of Ga at the solid-liquid interface place;
Fig. 2 be in the crystal Ga 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 Ga doping; 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 Ga doped p type polycrystal silicon ingot,, adopt following steps to realize referring to Fig. 3:
1) requires to calculate the required Ga doping content of corresponding silicon material according to the silicon chip electric property, the preparation doping agent.
2) in crucible 1 bottom negative electrode 13 is set, silicon material and doping agent are put into crucible 1 according to a certain percentage, anode 14 is set above the silicon material then, with lead 12 negative pole of negative electrode 13 with direct supply 11 linked to each other, anode 14 links to each other with positive 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 the high purity graphite material to make, and lead 12 adopts high-purity molybdenum filament.
3) charged crucible 1 is placed the furnace chamber well heater, vacuumize in the stove or protective atmosphere.The attemperation Controlling System with silicon material heat fused, is adjusted the position of anode 14, makes it keep good ohmic to contact with the liquid level of silicon liquid 2, begins silicon liquid is applied electric field, and interelectrode voltage is that 0.1～10V or current density are 0.1～10A/cm
2Arbitrary value in interval makes Ga mix 4 to the migration of negative electrode 13 directions, and keeps static more than 1 hour, allows Ga mix 4 in negative electrode 13 fully enrichments of zone.
4) regulate temperature control system, carry out crystal growth, in crystal growth, keep DC electric field, make the enrichment degree of Ga in the solid-liquid interface place liquid phase maintain same level, 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.The edge section that contacts with crucible is excised in part excision then that silicon ingot bottom doping content is on the low side and the top doping content is higher again, can obtain the uniform p type of Ga content distribution polycrystal silicon ingot on crystal growth direction.
Directional freeze mode under the DC electric field effect, the electric field setting 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 negative electrode, or adopts other similar mode.
Under the DC electric field effect, adopt CZ farad system Ga doped p 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 an anode, is connected to lead 12 on the positive 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 negative electrode is connected on the negative 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 Ga 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 the enrichment degree of Ga in the solid-liquid interface place liquid phase maintain same level, stop to apply electric field after entering the afterbody growth phase.
5) other treatment step 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 the uniform p type of Ga concentration distribution silicon single crystal rod on crystal growth direction then.
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 method growth Ga doped p 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, preparation doping agent, 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, and as negative electrode, crystal 5 fusion is connected respectively to lead 12 on the negative pole and positive pole of power supply 11 as anode with growing crystal 3.
3) strengthen the part thawing of the power of induction coil 20 with silicon rod 5 fusion, begin silicon liquid 2 is applied electric field, interelectrode voltage is that 0.1～10V or current density are 0.1～10A/cm
2Arbitrary value in interval makes Ga doping 4 liquid phase 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 the enrichment degree of Ga in the solid-liquid interface place liquid phase maintain same level, 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 the uniform p type of Ga concentration distribution silicon single crystal rod on crystal growth direction then.
Claims (4)
1. the preparation method of a Ga doped p-type crystalline 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 the Ga uniform doping distributes on crystal growth direction p type crystal silicon ingot or p type silicon single crystal rod.
2. according to the preparation method of a kind of Ga doped p-type crystalline 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.
3. according to the preparation method of a kind of Ga doped p-type crystalline silicon of claim 1, it is characterized in that: the described DC electric field that is parallel to crystal growth direction, its direction of an electric field is opposite 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.
4. according to the preparation method of a kind of Ga doped p-type crystalline silicon of claim 1, it is characterized in that: the control of described temperature field and electric field synergistic 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 (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102162122A (en) * | 2010-11-26 | 2011-08-24 | 亚洲硅业（青海）有限公司 | Preparation method of P-type medium-low-resistance silicon core carrier |
| CN102181926A (en) * | 2011-04-08 | 2011-09-14 | 光为绿色新能源有限公司 | Polycrystalline silicon ingot doping method and ingot casting equipment for implementing method |
| WO2014093087A1 (en) * | 2012-12-11 | 2014-06-19 | Hemlock Semiconductor Corporation | Methods of forming and analyzing doped silicon |
| CN103966665A (en) * | 2014-05-15 | 2014-08-06 | 阿特斯光伏电力(洛阳)有限公司 | Gallium-doped polycrystalline silicon ingot 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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| US20090255456A1 (en) * | 2008-04-10 | 2009-10-15 | Shunji Kuragaki | Method for evaluating metal contamination of silicon single crystal |
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| JPS5490086A (en) * | 1977-12-28 | 1979-07-17 | Toshiba Corp | Method of producing single crystal |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102162122A (en) * | 2010-11-26 | 2011-08-24 | 亚洲硅业（青海）有限公司 | Preparation method of P-type medium-low-resistance silicon core carrier |
| CN102181926A (en) * | 2011-04-08 | 2011-09-14 | 光为绿色新能源有限公司 | Polycrystalline silicon ingot doping method and ingot casting equipment for implementing method |
| WO2014093087A1 (en) * | 2012-12-11 | 2014-06-19 | Hemlock Semiconductor Corporation | Methods of forming and analyzing doped silicon |
| CN103966665A (en) * | 2014-05-15 | 2014-08-06 | 阿特斯光伏电力(洛阳)有限公司 | Gallium-doped polycrystalline silicon ingot and preparation method thereof |
| WO2015172556A1 (en) * | 2014-05-15 | 2015-11-19 | 苏州阿特斯阳光电力科技有限公司 | Gallium-doped polycrystalline silicon ingot and preparation method therefor |
| CN103966665B (en) * | 2014-05-15 | 2016-06-29 | 阿特斯光伏电力(洛阳)有限公司 | One mixes gallium polycrystal silicon ingot 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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