CN103243392A - Polycrystalline silicon ingot furnace and method for preparing polycrystalline silicon ingot with even and fine crystalline grains - Google Patents
Polycrystalline silicon ingot furnace and method for preparing polycrystalline silicon ingot with even and fine crystalline grains Download PDFInfo
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Abstract
The invention provides a polycrystalline silicon ingot furnace and a method for preparing a polycrystalline silicon ingot with even and fine crystalline grains. The polycrystalline silicon ingot furnace comprises a heat insulating cage lifting mechanism, an upper furnace body, a heat insulating cage, a crucible assembly, a directional coagulantion enhancement block, a lower furnace body, a support pillar and an ultrasonic generator, wherein the ultrasonic generator is arranged at the bottom of the outer wall of the lower furnace body, or on the side surface of the outer wall of the upper furnace body. The polycrystalline silicon ingot furnace and the method are characterized in that in the process of producing the polycrystalline silicon ingot, the ultrasonic generator is opened when the polycrystalline melt is in critical nucleation state, and the ultrasonic generator is closed in 1-20 min, and mechanical oscillation is introduced in initial stage of polycrystalline nucleation, so that the polycrystalline silicon ingot with even and fine in crystalline grains can be formed.
Description
Technical field
The present invention relates to technical field of solar batteries, relate in particular to polycrystalline silicon ingot or purifying furnace and the method for preparing even small grains polycrystalline silicon ingot casting.
Background technology
Solar cell is one of industry with fastest developing speed in recent years, grows at top speed with the speed above 50%.In various types of solar cells, crystal silicon solar energy battery is because the turnover ratio height, technology maturation and holding the lead.The complete industrial chain of crystal silicon solar photovoltaic module comprises ingot casting, section, battery and assembly four parts, and the casting polycrystalline silicon ingot is first step of producing the polycrystalline silicon solar photovoltaic module.
The casting polycrystalline silicon ingot generally adopts polycrystalline silicon ingot or purifying furnace at present, and Fig. 1 is the structural representation of polycrystalline silicon ingot or purifying furnace, and as shown in Figure 1, polycrystalline silicon ingot or purifying furnace comprises heat-insulation cage lifting mechanism 1, upper furnace body 2, heat-insulation cage 3, crucible assembly 4, orientation helps grumeleuse 5, lower furnace body 6, pillar stiffener 7; Described upper furnace body 2 and described lower furnace body 6 are connected by hydraulic pressure, described upper furnace body 2 can separate with described lower furnace body 6 or be closed, described heat-insulation cage 3 is arranged in the body of heater of upper furnace body 2 and lower furnace body 6 formations, described orientation helps grumeleuse 5 to be arranged in the heat-insulation cage 3 by pillar stiffener 7, the orientation that is positioned over described crucible assembly 4 helps on grumeleuse 5 platforms, described heat-insulation cage lifting mechanism 1 is connected with heat-insulation cage 3, upper furnace body 2, and described heat-insulation cage 3 is realized the lifting of heat-insulation cage 3 by heat-insulation cage lifting mechanism 1.
Silicon chip and battery cost continue to reduce at present, and the cost proportion in the Application of Solar Energy industrial chain is more and more lower.The cost of assembly, I﹠M etc. has become first factor, and expensive part becomes the developing direction of solar cell in the reduction polysilicon solar cell industrial chain.Battery efficiency promotes will improve battery cost, but reduce total cost, so high-efficiency battery becomes the direction of future development.Be key factor and the basic premise that improves battery conversion efficiency and cast high-quality polycrystal silicon ingot.The tiny polysilicon of preparation uniform crystal particles can guarantee the quality of polycrystalline silicon ingot casting.
The method of the even little crystal grain of preparation mainly relies on the cooling rate of long brilliant elementary increasing ingot furnace bottom at present, to obtain bigger condensate depression, reaches the purpose of crystal grain thinning.The concrete operations scheme is after the fusing of silicon material is finished, and promotes heat-insulation cage rapidly, makes ingot furnace bottom heat dissipation capacity strengthen, the forming core amount increases, after crucible bottom forms the more tiny parent phase of crystal grain, suitably reduce the aperture of heat-insulation cage, under suitable temperature, continue to finish the brilliant process of remaining length.
Increase long ingot furnace bottom radiating rate of brilliant initial stage with the method that adds big supercooling degree can realize the growing purpose of little crystal grain, but there is following shortcoming in this production method: one, increase rate of temperature change suddenly crucible and coating are exerted an influence, if there is defective in crucible coating layer, then be easy to take place industrial accidents such as sticking crucible even leakage; Two, the cooling velocity of variation that increases suddenly can to the back normally long brilliant process impact, cause the long brilliant rate fluctuation of silicon ingot bigger, cause polycrystal silicon ingot defective, dislocation to increase; Three, ingot furnace mainly relies on and promotes the purpose that heat-insulation cage realizes reducing bottom temp at present, but simple lifting heat-insulation cage, orientation helps the rate of heat release on grumeleuse four limits to be higher than the rate of heat release of central authorities, this cooling pattern can form the thermograde on the horizontal direction, finally can influence the verticality of silicon ingot crystal grain.Therefore, the invention provides a kind of method for preparing the tiny and uniform polycrystalline silicon ingot casting of crystal grain.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of method for preparing the polycrystalline silicon ingot casting of even small grains.
In view of this, the invention provides a kind of polycrystalline silicon ingot or purifying furnace, comprise: heat-insulation cage lifting mechanism, upper furnace body, heat-insulation cage, crucible assembly, orientation help grumeleuse, lower furnace body and pillar stiffener, described polycrystalline silicon ingot or purifying furnace also comprises ultrasonic generator, described ultrasonic generator is arranged at the bottom of described lower furnace body outer wall, or described ultrasonic generator is arranged at the side of described upper furnace body outer wall.
The present invention also provides a kind of method of utilizing described polycrystalline silicon ingot or purifying furnace to prepare even small grains polycrystalline silicon ingot casting, comprising:
Polycrystalline silicon material is loaded in the crucible, places orientation to help on the grumeleuse in described crucible;
Close down furnace chamber and vacuumize, heat described polycrystalline silicon material then, make described polycrystalline silicon material fusing;
Open ultrasonic generator when utilizing the heat-insulation cage lifting mechanism to make the polycrystalline silicon material cooling of fusing, the polycrystalline silicon material of described fusing reach critical forming core state;
Described ultrasonic generator cuts out after opening 1min～20min, obtains polycrystalline silicon ingot casting successively after long crystalline substance, annealing and cooling.
Preferably, described crucible is that inwall scribbles Si
3N
4Quartz crucible.
Preferably, the power the during unlatching of described ultrasonic generator is 500w～1200w, and frequency is 20 ± 2khz.
The invention provides a kind of polycrystalline silicon ingot or purifying furnace and utilize described polycrystalline silicon ingot or purifying furnace to prepare the method for polycrystalline silicon ingot casting.The application's polycrystalline silicon ingot or purifying furnace is provided with ultrasonic generator in the bottom of lower furnace body outer wall or the side of upper furnace body outer wall.Utilize polycrystalline silicon ingot or purifying furnace provided by the invention, in the process of preparation polycrystalline silicon ingot casting, after silicon material in the crucible melts fully, at critical forming core state ultrasonic generator is opened 1min～20min, during the ultrasonication silicon melt, fluid molecule is subjected to the periodically influence of alternation sound field, under suction function, produced cavitation bubble by drawing crack, under the positive effect of sound wave, the cavitation bubble that produces is with high speed closure or avalanche, thereby the part produces instantaneous pressure, high temperature and strong shockwave in melt.The continuous shock coagulation of the formed localized heat pulse of cavitation bubble forward position, and make the local corrosion in interface, the high temperature that cavitation bubble produces makes dendrite fusing, has also increased forming core quantity, thereby has reached the effect of crystal grain thinning.Therefore, become more tiny more even through the crystal grain under the acting in conjunction of sound cavitation effect and acoustic streaming effect of the melt after the ultrasonication, crucible bottom has formed the tiny parent phase of one deck uniform crystal particles after stopping ultrasonic generator, crystal can be grown on the basis of this parent phase from bottom to top gradually since then, finally obtains the complete tiny polycrystalline silicon ingot casting of inside even grain size.
Description of drawings
Fig. 1 is the structural representation of prior art polycrystalline silicon ingot or purifying furnace;
Fig. 2 is the structural representation of polycrystalline silicon ingot or purifying furnace of the present invention;
Fig. 3 is the structural representation of polycrystalline silicon ingot or purifying furnace of the present invention;
Fig. 4 is the interior tissue photo of the polycrystalline silicon ingot casting of the embodiment of the invention 2 preparations;
Fig. 5 is the interior tissue photo of the polycrystalline silicon ingot casting of Comparative Examples preparation.
Embodiment
In order further to understand the present invention, be described below in conjunction with the preferred embodiment of the invention of embodiment, but should be appreciated that these describe just to further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
The embodiment of the invention discloses a kind of polycrystalline silicon ingot or purifying furnace, as shown in Figure 2, Fig. 2 is the structural representation of polycrystalline silicon ingot or purifying furnace.Described polycrystalline silicon ingot or purifying furnace comprises: heat-insulation cage lifting mechanism 1, upper furnace body 2, heat-insulation cage 3, crucible assembly 4, orientation help grumeleuse 5, lower furnace body 6 and pillar stiffener 7, described polycrystalline silicon ingot or purifying furnace also comprises ultrasonic generator 8, described ultrasonic generator 8 is arranged at the bottom of described lower furnace body 6 outer walls, or as shown in Figure 3, described ultrasonic generator 8 is arranged at the side of described upper furnace body 2 outer walls.
According to the present invention, the effect of described ultrasonic generator is to convert civil power (380v or 220v) to be complementary with ultrasonic transducer high frequency ac signal, thereby the ultrasonic wave of certain frequency takes place.It is that 0w～1200w is adjustable continuously that the specifications and models of described ultrasonic generator can be selected power, and ultrasonic frequency is the ultrasonic generator of 20 ± 2khz, also can select the ultrasonic generator of other specifications and models, and the present invention has no particular limits.According to the present invention, more evenly tiny for the inner grain-size of the polycrystalline silicon ingot casting that makes formation, described ultrasonic generator is preferably disposed on the bottom of polycrystalline silicon ingot or purifying furnace lower furnace body outer wall.
The present invention also provides a kind of method of utilizing described polycrystalline silicon ingot or purifying furnace to prepare even small grains polycrystalline silicon ingot casting, may further comprise the steps:
Polycrystalline silicon material is loaded in the crucible, places orientation to help on the grumeleuse in described crucible;
Close down furnace chamber and vacuumize, heat described polycrystalline silicon material then, make described polycrystalline silicon material fusing;
Open ultrasonic generator when utilizing the heat-insulation cage lifting mechanism to make the polycrystalline silicon material cooling of fusing, the polycrystalline silicon material of described fusing reach critical forming core state;
Close behind described ultrasonic generator 1min～20min, after long crystalline substance, annealing and cooling, obtain polycrystalline silicon ingot casting successively.
The present invention adopts ultrasonic generator at the long brilliant initial stage of polycrystalline silicon material ultrasonic wave to take place, begin to stop ultrasonic wave immediately after the growth when measuring silicon ingot, according to technology of the prior art crystal grain is finished until process of growth along the direction growth of thermograde then.
According to the present invention, in the polycrystalline silicon ingot casting preparation process, at first polycrystalline silicon material is loaded in the crucible, and the crucible that polycrystalline silicon material will be housed places orientation to help on the grumeleuse, described crucible is preferably inwall and scribbles Si
3N
4Quartz crucible.It is the hollow graphite piece that described orientation helps grumeleuse, and thermal conductivity is very strong.
Close lower chambers then and carry out vacuum pumping, enter heating process after the operation of preferably polycrystalline silicon ingot or purifying furnace being hunted leak.Around the described crucible and top is equipped with well heater, namely the silicon material is heated behind the connection power supply, and heating and continuous 12～24h melts fully until the silicon material.Utilize the heat-insulation cage lifting mechanism then, make on the heat-insulation cage position to rise, accelerate heat and help grumeleuse to the speed of external diffusion by orientation, the polycrystalline silicon material that melts is cooled off, and take away the heat of crucible, the final vertical temperature gradient that in melted silicon, forms from bottom to top indirectly; Under the effect of described vertical gradient, the molten silicon material begins to solidify from crucible bottom, and namely long brilliant process is to carry out to the top order from the liquation bottom.
When the long brilliant initial stage, namely molten silicon reached critical forming core state, open ultrasonic generator.When open ultrasonic generator for very crucial to the polycrystalline silicon ingot casting forming core, the ultrasonic generator time opening is too early, influence the normal forming core of polysilicon liquation, opening time crosses late inoperative to forming even small grains, therefore, need carry out strictness control to the opening time, thus the application to open ultrasonic generator be criticality at the beginning forming core.The present invention measures the weight break point that the silicon material is melted to the beginning forming core fully as follows:
Select a quartz pushrod, quartz pushrod is extend in the liquid silicon of fusion, the position that touches the crucible bottom surface is made as basic point, at the long brilliant initial stage quartz pushrod is repeated to stretch into from the ingot furnace top, measured once in per 10 minutes, by measuring the position that glass stick stretches into, determine whether silicon crystal begins growth, and the difference of observed value and basic point is the growing height of crystal.Measure and begin to open ultrasonic wave immediately after the growth, finally when growing brilliant height measurements and reach 3mm～10mm, close ultrasonic wave.Certainly, the method for this measurement is more loaded down with trivial details, can be on based measurement, by ingot furnace bottom warm area temperature is judged the time that this key point of beginning forming core takes place.
In the ultrasonic generator open stage, during the ultrasonication silicon melt, fluid molecule is subjected to the periodically effect of alternation sound field, under suction function, produced cavitation bubble by drawing crack, under the positive effect of sound wave, the cavitation bubble that produces is with high speed closure or avalanche, cavitation bubble forms the process of growing up will be from absorbing heat on every side, this causes cavitation bubble surf zone silicon melt temperature to reduce, produce local overcooling, but in cavitation bubble avalanche process, the crystal that the intense impact ripple of generation can smash primary crystal and grow up makes it to become broken crystal particle.The continuous shock coagulation of the formed localized heat pulse of cavitation forward position, and make the local corrosion in interface, the high temperature that cavitation produces makes dendrite fusing, has also increased forming core quantity, thereby has reached the effect of crystal grain thinning.High pressure through ultrasonication produces can make liquid-state silicon change to solid state si, thereby promote the formation of nucleus, and therefore, the melt after the ultrasonication makes crystal grain become more tiny more even under the acting in conjunction of sound cavitation effect and acoustic streaming effect.The energy waste that takes place during the ultrasonication melt can be absorbed heat energy by entire body, the more big heat effect of power input is more obvious, so when hyperacoustic power is excessive, can make the cooling rate of melt slack-off, can make the crystal alligatoring on the contrary, so need to guarantee that the power of ultrasonic generator is in reasonable range.According to the present invention, the opening time of described ultrasonic generator is 1min～20min, is preferably 10min～20min.Power when described ultrasonic generator is opened is preferably 500w～1200w.
Mechanical oscillation by ultrasonic generator, crucible bottom forms a fairly large number of new nucleus, treat namely to stop ultra-sonic oscillation after nucleus produces, this moment, crucible bottom formed the tiny parent phase of one deck uniform crystal particles, after this crystal can be grown on the basis of this parent phase from bottom to top gradually, finally grow into complete polycrystalline silicon ingot casting, silicon ingot annealed and the cooling after just finished the whole production cycle.
Utilize polycrystalline silicon ingot or purifying furnace of the present invention, can make the polycrystalline silicon ingot casting grain refining that obtains, simultaneously compared to prior art remarkable advantages is arranged: do not change the variation of temperature rate, do not change the thermograde direction yet, thereby a stable external environment is provided for the crystal stage of growing up after forming core, guarantee not introduce unnecessary dislocation, defective, do not influence the verticality of silicon crystal grain simultaneously; Can not introduce thermal shocking, protect the quality stability of crucible, coating; Better crystal grain consistence is arranged, and the internal stress of process of growth is little, causes the good uniformity of ingot casting, helps to improve open circuit voltage and current characteristics, improves the photoelectric transformation efficiency of polycrystal silicon cell sheet.
In order further to understand the present invention, to polycrystalline silicon ingot or purifying furnace provided by the invention and utilize polycrystalline silicon ingot or purifying furnace to prepare the process of polycrystalline silicon ingot casting, protection scope of the present invention is not limited by the following examples below in conjunction with embodiment.
As shown in Figure 2, Fig. 2 is the structural representation of polycrystalline silicon ingot or purifying furnace, described polycrystalline silicon ingot or purifying furnace comprises: heat-insulation cage lifting mechanism 1, upper furnace body 2, heat-insulation cage 3, crucible assembly 4, orientation helps grumeleuse 5, lower furnace body 6, pillar stiffener 7, ultrasonic generator 8, described ultrasonic generator 8 is arranged at the bottom of lower furnace body 6 outer walls.
Polycrystalline silicon material is loaded into inwall scribbles Si
3N
4Quartz crucible in, and crucible is positioned over the hollow graphite piece, namely orientation helps on the grumeleuse (DS piece); Subsequently, close down furnace chamber and carry out vacuum pumping, system heats after finishing the leak detection operation; Around the crucible and top is equipped with well heater, after connecting power supply the silicon material is heated, heat-processed continues to melt fully until the silicon material in 15 hours, then utilize the heat-insulation cage lifting mechanism, make on the heat-insulation cage position to rise, accelerate heat and help grumeleuse to the speed of external diffusion by orientation, it is cooled off, thereby take away the heat in the crucible indirectly, finally in silicon solution formation vertical temperature gradient from bottom to top; Under the effect of this thermograde, the silicon material begins to solidify from crucible bottom, and namely long brilliant process is to carry out to the top order from the solution bottom; When molten silicon reaches critical forming core state, open ultrasonic generator, long brilliant height measurements reaches 3mm～10mm, stop ultrasonic wave, this moment, crucible bottom formed the tiny parent phase of one deck uniform crystal particles, next crystal can be from bottom to top growth gradually on the basis of this parent phase, finally grow into complete efficient polycrystal silicon ingot, just finished the whole production cycle after the annealed and cooling of silicon ingot.
Choose the silicon ingot bottom position and take pictures, as shown in Figure 4, Fig. 4 is the interior tissue photo of the polycrystalline silicon ingot casting of present embodiment production.
Comparative Examples
Polycrystalline silicon material is loaded into inwall scribbles Si
3N
4Quartz crucible in, and crucible is positioned over the hollow graphite piece, namely orientation helps on the grumeleuse (DS piece); Subsequently, close down furnace chamber and carry out vacuum pumping, system heats after finishing the leak detection operation; Around the crucible and top is equipped with well heater, after connecting power supply the silicon material is heated, heat-processed continues to melt fully until the silicon material in 15 hours, then utilize the heat-insulation cage lifting mechanism, make on the heat-insulation cage position to rise, accelerate heat and help grumeleuse to the speed of external diffusion by orientation, it is cooled off, thereby take away the heat in the crucible indirectly, finally in silicon solution formation vertical temperature gradient from bottom to top; Under the effect of this thermograde, the silicon material begins to solidify from crucible bottom, and namely long brilliant process is to carry out to the top order from the solution bottom, finally grows into complete polycrystal silicon ingot, has just finished the whole production cycle after the annealed and cooling of silicon ingot.
Choose with embodiment 2 ingot casting same positions and take pictures, as shown in Figure 5, Fig. 5 is the interior tissue photo of the polycrystalline silicon ingot casting of Comparative Examples production.
By Fig. 4 and 5 as can be seen, the crystallographic grain that Comparative Examples 1 is produced is thick, the lack of homogeneity of crystal grain, and dendritic structure is more; And the sample of process ultrasonication, grain refining is obvious, and the uniformization effect of crystal is good.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.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 carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments herein.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the wideest scope consistent with principle disclosed herein and features of novelty.
Claims (4)
1. polycrystalline silicon ingot or purifying furnace, comprise: heat-insulation cage lifting mechanism, upper furnace body, heat-insulation cage, crucible assembly, orientation help grumeleuse, lower furnace body and pillar stiffener, it is characterized in that, described polycrystalline silicon ingot or purifying furnace also comprises ultrasonic generator, described ultrasonic generator is arranged at the bottom of described lower furnace body outer wall, or described ultrasonic generator is arranged at the side of described upper furnace body outer wall.
2. method of utilizing the described polycrystalline silicon ingot or purifying furnace of claim 1 to prepare even small grains polycrystalline silicon ingot casting comprises:
Polycrystalline silicon material is loaded in the crucible, places orientation to help on the grumeleuse in described crucible;
Close down furnace chamber and vacuumize, heat described polycrystalline silicon material then, make described polycrystalline silicon material fusing;
Open ultrasonic generator when utilizing the heat-insulation cage lifting mechanism to make the polycrystalline silicon material cooling of fusing, the polycrystalline silicon material of described fusing reach critical forming core state;
Described ultrasonic generator cuts out after opening 1min～20min, obtains polycrystalline silicon ingot casting successively after long crystalline substance, annealing and cooling.
3. method according to claim 2 is characterized in that, described crucible is that inwall scribbles Si
3N
4Quartz crucible.
4. method according to claim 2 is characterized in that, the power the during unlatching of described ultrasonic generator is 500w～1200w, and frequency is 20 ± 2khz.
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| CN105506731A (en) * | 2015-12-09 | 2016-04-20 | 上海超硅半导体有限公司 | Monocrystalline silicon growth oxygen content control technology |
| DE102015216734A1 (en) | 2015-09-02 | 2017-03-02 | Alzchem Ag | Crucible for the production of silicon ingots, process for its production and silicon ingots |
| CN106637397A (en) * | 2016-12-30 | 2017-05-10 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method of polycrystalline silicon ingot and polycrystalline silicon ingot furnace |
| CN110512283A (en) * | 2019-09-23 | 2019-11-29 | 新余学院 | A method for preparing solar-grade polysilicon based on axial magnetic field and ultrasonic treatment |
| CN111809233A (en) * | 2020-05-14 | 2020-10-23 | 江苏高照新能源发展有限公司 | Dislocation-reducing full-melting efficient casting polycrystalline production process |
| CN113463198A (en) * | 2021-06-17 | 2021-10-01 | 江苏富乐德半导体科技有限公司 | Preparation method of silicon nitride ceramic |
| CN113755945A (en) * | 2021-09-09 | 2021-12-07 | 扬州晶樱光电科技有限公司 | Polycrystalline ingot furnace body for oversized silicon ingot |
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