CN102719883A - Semiconductor monocrystal silicon production process - Google Patents
Semiconductor monocrystal silicon production process Download PDFInfo
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- CN102719883A CN102719883A CN2012102357546A CN201210235754A CN102719883A CN 102719883 A CN102719883 A CN 102719883A CN 2012102357546 A CN2012102357546 A CN 2012102357546A CN 201210235754 A CN201210235754 A CN 201210235754A CN 102719883 A CN102719883 A CN 102719883A
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Abstract
The invention discloses a semiconductor monocrystal silicon production process, which includes the following steps: laying a transverse magnetic field with the intensity ranging from 1200 to 1400 G; preparing silicon raw materials and doping agent; loading materials; melting materials; shoulder leading and shouldering; shoulder rotating at the pull speed ranging from 2.7 to 3.3 mm/min after the shouldering; isodiametric growing for 45 to 55 mm at the pull speed ranging from 1.5 to 1.7 mm/min after the shoulder rotating; and completing the follow-up isodiametric growing process of the to-be-made semiconductor monocrystal silicon according to the ordinary isodiametric growing method of the straight-pulled monocrystal silicon. The semiconductor monocrystal silicon production process has reasonable design, simple method steps and excellent use effect, is convenient to realize and easy to master, can ensure the quality of the produced semiconductor monocrystal silicon, and enables the produced semiconductor monocrystal silicon to be highly uniform in the resistivity of the cross section and free from all sorts of microdefects as vortex formation.
Description
Patented claim of the present invention the dividing an application that be on 07 15th, 2011 applying date, application number 201110199182.6 and invention and created name for the application for a patent for invention of " a kind of semiconductor grade monocrystalline silicon production technology ".
Technical field
The invention belongs to the monocrystalline silicon production technical field, especially relate to a kind of semiconductor grade monocrystalline silicon production technology.
Background technology
Silicon single crystal is claimed silicon single crystal again, is a kind of semiconductor material.In recent years, along with the fast development of photovoltaic industry, silicon single crystal was used to manufacturing solar cells again, demonstrated the situation that supply falls short of demand.Along with high-tech development; Produce and be close to perfect high quality monocrystalline silicon; Be the common aspiration of each material producer, device producer, this silicon single crystal has the good characteristics that section resistivity evenness, high life, carbon content are few, microdefect density is little, oxygen level can be controlled.
At present, the method for manufacture order crystal silicon has vertical pulling method, zone melting method, pedestal pulling method, lamellar growth method, vapor growth method, epitaxy etc., and wherein pedestal pulling method, lamellar growth method, vapor growth method and epitaxy all fail generally to be promoted because of deficiency separately; And vertical pulling method and zone melting method are relatively, are main machining method with the vertical pulling method, and its charging capacity single crystal diameters many, that produce are big, and automation degree of equipment is high, and technology is fairly simple, and production efficiency is high.The silicon single crystal that vertical pulling method is produced accounts for more than 70% of world's silicon single crystal total amount.Single crystal growing furnace is a kind of in inert gas environment, with graphite heater with polycrystalline materials such as polysilicon fusings, and with the equipment of Grown by CZ Method dislocation-free monocrystalline.Vertical pulling method is called Czochralski method again, is called for short the CZ method.The characteristics of CZ method are in the hot system of a straight barrel type, with the graphite resistance heating, with the unmelted polycrystalline silicon that is contained in the high-purity silica pot; Then seed crystal is inserted bath surface and carry out welding; Rotate seed crystal simultaneously, backward rotation crucible again, seed crystal slowly upwards promote; Through seeding, amplification, commentaries on classics shoulder, isodiametric growth, epilog, a silicon single crystal has just grown.
Semiconductor grade silicon single crystal is one type and has semiconducting behavior; And be used for making the silicon materials of semiconducter device; Along with the continuous development of electronic product, the market demand of semiconductor grade silicon single crystal is increasing, and the quality to semiconductor grade silicon single crystal also requires increasingly high simultaneously.But, the semiconductor grade silicon single crystal that is occurred in the market all exist to some extent the section resistivity evenness relatively poor, be prone to number of drawbacks and deficiencies such as the difficult control of swirl defect, quality product.
Summary of the invention
Technical problem to be solved by this invention is to above-mentioned deficiency of the prior art; A kind of semiconductor grade monocrystalline silicon production technology is provided; It is reasonable in design, method steps is simple, realization is convenient and be easy to grasp, result of use is good; Can effectively guarantee the quality of the semiconductor grade silicon single crystal of producing, the semiconductor grade silicon single crystal section resistivity evenness produced is high and do not have a whirlpool.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of semiconductor grade monocrystalline silicon production technology is characterized in that this technology may further comprise the steps:
Step 1, transverse magnetic field are laid: a transverse magnetic field is laid in the outside in the middle part of producing the single crystal growing furnace master furnace chamber that needs making semiconductor grade silicon single crystal, and the magneticstrength of said transverse magnetic field is 1300 Gausses ± 100 Gausses;
Step 2, silicon raw material and doping agent are prepared: according to the conventional preparation method of single crystal growing furnace with the silicon raw material, prepare the silicon raw material that the growth pulling of silicon single crystal is used, and press the conventional cleaning method of single crystal growing furnace with the silicon raw material, the silicon raw material of preparing is carried out clean; Simultaneously,, need to confirm the kind and the doping of interpolation doping agent, and the doping agent that the growth pulling of silicon single crystal is used is prepared according to model and the resistivity that need are made semiconductor grade silicon single crystal;
Step 3, charging:, ready silicon raw material and doping agent in the step 1 are put into respectively in the quartz crucible that has been in place according to the conventional loading method of single crystal growing furnace; Simultaneously, the previously prepd seed crystal is installed on the seed chuck in the said single crystal growing furnace;
Step 4, melt: the conventional melt method according to single crystal growing furnace, melt silicon raw material and doping agent in the said quartz crucible of packing in the step 2, until said silicon raw material and whole fusings of doping agent and acquisition silicon melt;
Step 5, draw shoulder and shouldering: after melt is accomplished, adopt single crystal growing furnace and draw shoulder and shouldering method according to the routine of pulling of silicon single crystal, accomplish need to make semiconductor grade silicon single crystal draw shoulder and shouldering process;
Step 6, change shoulder: when changeing shoulder after shouldering finishes, change shoulder with the pulling rate of 3mm/min ± 0.3mm/min;
Step 7, isodiametric growth: after changeing the shoulder end, with pulling rate isodiametric growth 50mm ± 5mm of 1.6mm/min ± 0.1mm/min; Afterwards, press the conventional isodiametric growth method of pulling of silicon single crystal again, accomplish the follow-up isodiametric growth process that needs to make semiconductor grade silicon single crystal.
Above-mentioned a kind of semiconductor grade monocrystalline silicon production technology is characterized in that: the magneticstrength of transverse magnetic field described in the step 1 is 1300 Gausses ± 20 Gausses.
Above-mentioned a kind of semiconductor grade monocrystalline silicon production technology is characterized in that: when step 5 was drawn shoulder and shouldering, said single crystal growing furnace was controlled the pulling rate that draws in shoulder and the shouldering process according to predefined pulling rate control curve automatically; Change when shoulder in the step 6,, control said single crystal growing furnace and change shoulder with the pulling rate of 3mm/min ± 0.3mm/min artificially through the electric control box of said single crystal growing furnace; After step 7 transfer shoulder finishes, artificial again through the electric control box of said single crystal growing furnace, control the pulling rate isodiametric growth 50mm ± 5mm of said single crystal growing furnace with 1.6mm/min ± 0.1mm/min; Afterwards, said single crystal growing furnace is accomplished the follow-up isodiametric growth process that needs to make semiconductor grade silicon single crystal according to predefined pulling rate control curve.
Above-mentioned a kind of semiconductor grade monocrystalline silicon production technology is characterized in that: change when shoulder in the step 6, change shoulder with the pulling rate of 3mm/min; After step 7 transfer shoulder finishes, with the pulling rate isodiametric growth 50mm of 1.6mm/min; Afterwards, again by conventional isodiametric growth method, accomplish the follow-up isodiametric growth process that needs to make semiconductor grade silicon single crystal.
Above-mentioned a kind of semiconductor grade monocrystalline silicon production technology is characterized in that: the transverse magnetic field described in the step 1 is made up of two blocks of PMs that are laid in the left and right sides, single crystal growing furnace master furnace chamber middle part respectively, and two blocks of said PMs are symmetry and lay.
Above-mentioned a kind of semiconductor grade monocrystalline silicon production technology; It is characterized in that: after accomplishing the follow-up isodiametric growth process of semiconductor grade silicon single crystal in the step 7; Press the routine ending of pulling of silicon single crystal again and accomplish the subsequent production process that needs to make semiconductor grade silicon single crystal, perhaps adopt the treatment process that does not finish up to accomplish the subsequent production process that needs to make semiconductor grade silicon single crystal with stopping process; And when adopting the treatment process completion that does not finish up to need to make the subsequent production process of semiconductor grade silicon single crystal, its treatment process may further comprise the steps:
ⅰ, close the graphite thermal field system of single crystal growing furnace: carry out in the isodiametric growth process in the step 7; When the single crystal silicon length of isodiametric growth reaches the preseting length that needs making semiconductor grade silicon single crystal; Close the graphite thermal field system of single crystal growing furnace; And the heating power of said single crystal growing furnace reduced to zero, remaining silicon melt surface temperature reduces gradually in the said afterwards quartz crucible, begins crystallization until the surface of said silicon melt;
ⅱ, crystallization and crystal are lifted from fusion silicon liquid level: after the beginning crystallization of said silicon melt surface; Crystalline polamer to said silicon melt surface carries out simultaneous observation; When being 1mm～5mm when the crystallisate on said silicon melt surface and the gap between the current institute growing single-crystal silicon crystal; Through seed crystal rotary lifting mechanism set on the said single crystal growing furnace current single crystal silicon of growing is upwards promoted, and make the liquid level of current single crystal silicon of growing and said molten silicon body be separated;
ⅲ, crystal promote and get crystalline substance: through said seed crystal rotary lifting mechanism current single crystal silicon of growing is promoted in the secondary furnace chamber of single crystal growing furnace; Afterwards, close the segregaion valve between secondary furnace chamber of single crystal growing furnace and the single crystal growing furnace master furnace chamber, single crystal growing furnace master furnace chamber and the secondary furnace chamber of single crystal growing furnace are isolated; Subsequently, get crystal method, in the secondary furnace chamber of single crystal growing furnace, take out single crystal silicon, just accomplish the production process of silicon single crystal according to the routine of single crystal growing furnace.
Above-mentioned a kind of semiconductor grade monocrystalline silicon production technology is characterized in that: after melt is accomplished in the step 4 and carry out before the seeding, also need carry out carrying slag behind the melt, it is following that it puies forward the slag process:
I, decrease temperature crystalline: reduce the heating power of single crystal growing furnace, and make the surface temperature of said silicon melt reduce gradually, begin crystallization until the surface of said silicon melt;
II, progressively heat up and keep crystallisation process and carry out continuously; Insolubles until the silicon melt surface flotation is all condensed by crystallisate: after the beginning crystallization of said silicon melt surface, and the surface temperature of the heating power of the single crystal growing furnace that raises again and the said silicon melt that raises gradually; In the surface temperature of said silicon melt gradually in the elevation process; Crystalline polamer to said silicon melt surface carries out simultaneous observation; When the insolubles that observes said silicon melt surface flotation is all condensed by the crystallisate on said silicon melt surface; Through seed crystal rotary lifting mechanism set on the said single crystal growing furnace said seed crystal is dropped to said crystallisate and to contact; And after treating said seed crystal and said crystallisate welding, will condense through said seed crystal rotary lifting mechanism has the crystallisate of insolubles to be promoted in the secondary furnace chamber of single crystal growing furnace; Afterwards, close said segregaion valve, single crystal growing furnace master furnace chamber and the secondary furnace chamber of single crystal growing furnace are isolated;
III, scarfing cinder: the routine according to single crystal growing furnace is got crystal method, in the secondary furnace chamber of single crystal growing furnace, takes out seed crystal, and removes the crystallisate of seed crystal bottom institute welding, then accomplishes the slag process of putting forward behind the melt; Afterwards, close single crystal growing furnace bell and open said segregaion valve.
Above-mentioned a kind of semiconductor grade monocrystalline silicon production technology is characterized in that: accomplish in the step III behind the melt put forward the slag process after, also need change to the seed crystal that in the secondary furnace chamber of single crystal growing furnace, takes out in the step III; And after having changed seed crystal, the bell of the single crystal growing furnace that closes is again also opened said segregaion valve.
The present invention compared with prior art has the following advantages:
1, reasonable in design and treatment process steps is simple, be easy to grasp.
2, the low and realization convenience of input cost.
The semiconductor grade silicon single crystal quality of 3, being produced is good; It draws shoulder and the shouldering process is all undertaken by common process; And only be that the pulling rate with 3mm/min ± 0.3mm/min changes shoulder in changeing the shoulder process; Like this when improve changeing shoulder process process, accelerating monocrystalline silicon production efficient, change the crystalline growth velocity when takeing on through improving crystal, can effectively improve the section resistivity evenness of semiconductor grade silicon single crystal.After changeing the shoulder end simultaneously, with pulling rate isodiametric growth 50mm ± 5mm of 1.6mm/min ± 0.1mm/min, can effectively control crystalline growth quality under the unsteady state again; And can guarantee effectively that current single crystal silicon of being grown carries out steady state by unsteady state behind the pulling rate isodiametric growth 50mm ± 5mm with 1.6mm/min ± 0.1mm/min; Spend the transitory stage between unsteady state to the steady state in high quality, thereby can further improve the section resistivity evenness of semiconductor grade silicon single crystal.In addition, actually control very easyly, realize convenient and be easy to grasping, practical effect is very good.The section center resistivity that employing the present invention produces semiconductor grade silicon single crystal is almost consistent with the section edge resistivity, has improved the section resistivity evenness of semiconductor grade silicon single crystal significantly, can effectively eliminate various microdefects such as whirlpool simultaneously.
4, selecting the specific magnetising moment for use is 1300 Gausses' horizontal externally-applied magnetic field, and in the magnetic field of this intensity, the natural convection of silicon melt receives good inhibition effect, has improved the crystalline homogeneity that draws greatly; Simultaneously, the present invention chooses permanent magnetic field, thereby need not consume additional electric energy, has reduced production cost.
5, adopt the treatment process that do not finish up; When the length of single crystal silicon growth reaches ending length; The method that does not finish up but take to close the graphite thermal field system of single crystal growing furnace is cooled off the silicon melt in the quartz crucible fast; And when the crystallization on silicon melt surface is about to touch silicon crystal, upwards promotes single crystal silicon rapidly and make crystal break away from silicon melt level.Thereby, compare with existing technology, omitted the epilog in the single crystal silicon pulling process, practiced thrift the PT, and the corresponding production efficiency that improves silicon single crystal, the while can effectively guarantee the quality of the semiconductor grade silicon single crystal of producing.
6, to carry the slag process operation behind the melt that adopts simple; Workable, and put forward the slag process and be easy to control, can be simple, convenient and a large amount of contaminant removals of after melt is accomplished, containing in the silicon material apace; Thereby bonding crystal silicon production process is carried out safely and fast; Can effectively avoid simultaneously because of not proposing the industrial accident that slag causes, thereby practice thrift a large amount of stopping production servicing time, improve the production efficiency of manufacturer.In addition; After proposing the slag end, also need change to seed crystal; Be that whole monocrystalline silicon production process adopts two seed crystals, wherein put forward the slag process of putting forward after the slag seed crystal is used for melt, finish the pulling process that seed crystal after the back is changed is used for follow-up single crystal silicon and carry slag; Incidental seed crystal breakage problem when adopting two seed crystals can effectively avoid only using a seed crystal to propose slag and crystal drawing; Improved the security of producing largely, reduced the probability of occurrence that leaks the silicon accident, the silicon material is purified to produce to be significant; And also correspondingly guaranteed the monocrystalline silicon production process fast, effectively carry out; When reducing accident rate; The also corresponding production efficiency that improves silicon single crystal makes because accident causes the temporary transient probability that stops production or keep in repair to reduce, and has not only practiced thrift production and maintenance cost; Save the servicing time after a large amount of accidents, made the monocrystalline silicon production efficient of whole producer be greatly improved.
In sum; The present invention is reasonable in design, method steps is simple, realization is convenient and be easy to grasp, result of use is good; Can effectively guarantee the quality of the semiconductor grade silicon single crystal of producing, the semiconductor grade silicon single crystal section resistivity evenness produced is high and do not have various microdefects such as whirlpool.
Through accompanying drawing and embodiment, technical scheme of the present invention is done further detailed description below.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
A kind of semiconductor grade monocrystalline silicon production technology as shown in Figure 1 may further comprise the steps:
Step 1, transverse magnetic field are laid: outside producing single crystal growing furnace master furnace chamber 1 middle part that needs making semiconductor grade silicon single crystal, lay a transverse magnetic field, and the magneticstrength of said transverse magnetic field is 1300 Gausses ± 100 Gausses.Wherein, 1 Gauss=1 oersted.We can say that also the magneticstrength of said transverse magnetic field is 1300 oersteds ± 100 oersteds.
Actual when laying said transverse magnetic field, the magneticstrength of said transverse magnetic field is 1300 Gausses ± 20 Gausses.In the present embodiment, the magneticstrength of said transverse magnetic field is 1300 Gausses, in the actual use, can be according to actual needs, and the magneticstrength of said transverse magnetic field is adjusted accordingly.
In the present embodiment, said transverse magnetic field is made up of two blocks of PMs that are laid in the left and right sides, single crystal growing furnace master furnace chamber middle part respectively, and two blocks of said PMs are symmetry and lay.That is to say; Two said PM symmetries are laid in the left and right sides, middle part of single crystal growing furnace master furnace chamber; And two blocks of said PMs are over against laying, and said transverse magnetic field structure is all identical with distribution method with existing single crystal growing furnace transverse magnetic field structure with distribution method.
Step 2, silicon raw material and doping agent are prepared: according to the conventional preparation method of single crystal growing furnace with the silicon raw material, prepare the silicon raw material that the growth pulling of silicon single crystal is used, and press the conventional cleaning method of single crystal growing furnace with the silicon raw material, the silicon raw material of preparing is carried out clean; Simultaneously,, need to confirm the kind and the doping of interpolation doping agent, and the doping agent that the growth pulling of silicon single crystal is used is prepared according to model and the resistivity that need are made semiconductor grade silicon single crystal.
In the present embodiment; Identical with routine preparation growth pulling of silicon single crystal with the method for silicon raw material; Elder generation is according to the specification and the size of need making semiconductor grade silicon single crystal, and the model of institute's employing single crystal growing furnace and respective performances parameter, need use the amount of silicon raw material when confirming to make silicon single crystal.The prepared silicon raw material that goes out refers to the raw material that carries out crystal-pulling in the quartz crucible of preparing to pack into, comprises that polysilicon that reduction method produces, polysilicon, zone melting single-crystal that silane thermal decomposition process is produced are expected end to end, flaw-piece material, pot bottom material, silicon chip reclaimed materials etc.Wherein, the polysilicon that reduction method is produced is for being raw material and the raw material that obtains through processing and preparing with the industrial silicon, and purity can reach more than nine " 9 ", is called high-purity polycrystalline silicon again, its phosphorus content ﹤ 1.5 * 10
13Individual atom/cm
3(corresponding N type resistivity>=300 Ω cm); Boron content≤4.5 * 10
12Individual atom/cm
3(corresponding P type resistivity>=3000 Ω cm).
Simultaneously, when the common metal material contained a spot of impurity, change in resistance was little, but after purified semiconductor material mixed small amount of impurities, change in resistance was huge, and this is an essential characteristic of semiconductor material.Therefore for guaranteeing the quality of institute's manufacture order crystal silicon, the used polycrystalline silicon material of pulling monocrystal silicon must carry out clean.Wherein, polysilicon, mother alloy (being doping agent) and seed crystal generally with nitric acid and the corrosion of hydrofluoric acid mixing acid, also can be used caustic corrosion.But no matter with acid corrosion or caustic corrosion, it is high that the purity of bronsted lowry acids and bases bronsted lowry is wanted, and needs to adopt the acid or the alkali of the above grade of analytical pure to corrode.
When preparation growth pulling of silicon single crystal is with the silicon raw material, also need prepare to the doping agent that the growth pulling of silicon single crystal is used.In the present embodiment, adopt mother alloy as doping agent.When reality is prepared adulterant, make the model and the resistivity of semiconductor grade monocrystalline silicon earlier based on need, and confirm to add the kind and the doping of adulterant according to conventional method.
Step 3, charging:, ready silicon raw material and doping agent in the step 1 are put into respectively in the quartz crucible that has been in place according to the conventional loading method of single crystal growing furnace; Simultaneously, the previously prepd seed crystal is installed on the seed chuck in the said single crystal growing furnace;
Step 4, melt: the conventional melt method according to single crystal growing furnace, melt silicon raw material and doping agent in the said quartz crucible of packing in the step 2, until said silicon raw material and whole fusings of doping agent and acquisition silicon melt.
Step 5, draw shoulder and shouldering: after melt is accomplished, adopt single crystal growing furnace and draw shoulder and shouldering method according to the routine of pulling of silicon single crystal, accomplish need to make semiconductor grade silicon single crystal draw shoulder and shouldering process.
Step 6, change shoulder: when changeing shoulder after shouldering finishes, change shoulder with the pulling rate of 3mm/min ± 0.3mm/min.
Step 7, isodiametric growth: after changeing the shoulder end, with pulling rate isodiametric growth 50mm ± 5mm of 1.6mm/min ± 0.1mm/min; Afterwards, press the conventional isodiametric growth method of pulling of silicon single crystal again, accomplish the follow-up isodiametric growth process that needs to make semiconductor grade silicon single crystal.
In the present embodiment, the semiconductor grade silicon single crystal of being produced is the silicon single crystal of 4 cun or 6 cun.
In the actual production process; Before in step 3, feeding; Also need tear stove earlier open; The purpose of tearing stove open is in order to have drawn the single crystal silicon of moulding before taking out, the volatile matter in the clearing furnace, foreign material such as the dirt settling on the graphite piece such as removing Graphite Electrodes, well heater, insulation cover, adaptation fragment, graphite granule, graphite carbon felt dust.Tear open and will note mending to such an extent that bring new foreign material in the stove process.Tearing open and inflate earlier before the stove, specifically is to write down vacuum tightness in the stove of tearing the stokehold open earlier, the argon gas loading line in the open auxiliary furnace chamber afterwards, and close when being inflated to furnace pressure for barometric point.Actual when getting crystalline substance, through body of heater up-down opener secondary furnace chamber (perhaps with secondary furnace chamber together with bell together) is raised to upper limit position earlier after, slow revolute furnace chamber is got crystalline substance afterwards again till taking out single crystal silicon.When reality is torn stove open to main furnace chamber, take out guide shell, quartz crucible (its outside is set with plumbago crucible), pot holder, pressure pin and graphite thermal field system from top to bottom successively; And the above-mentioned internals that split out are cleaned, the purpose of cleaning is that volatile matter that produces in crystal pulling or the calcination process and dust is clean with the cleaning of methods such as polishing, wiping or absorption.After having cleaned, again each internals that splits out are assembled one by one.
Simultaneously, before the melt, closed fire door earlier,, just can hunt leak, and confirmed that the voltage rise rate power cabinet that just can start single crystal growing furnace that meets the requirements heats until being extracted into pressure drop to 3Pa to vacuumizing in the burner hearth.Before the starting power cabinet heats, charge into earlier and calm the anger to 1300Pa and keep furnace pressure.Afterwards; Begin heating, divide to be heated to for 3～4 times high temperature and each about 1.5 hours of heat-up time, heating power is 70KW～80KW; About 4～5 hours of whole fusing time; If should in time handle when the polycrystalline piece is attached on the quartz crucible limit in the melting process, just should lower the temperature gradually when having polycrystalline piece about 20% also not melt when surplus, and through raise the gradually position of quartz crucible of crucible driving mechanism.Subsequently, utilize the thermal inertia of graphite thermal field system to make remaining polycrystalline piece material continue fusing, treat just to drop to the seeding temperature after polycrystalline has melted.After the silicon material has melted, quartz crucible is increased to the seeding position, rotates seed shaft and be adjusted to the seeding temperature, the beginning seeding through seed crystal rotation and lifting mechanism.To confirm before the seeding that brilliant commentaries on classics, crucible change and seeding crucible position, treat that temperature begins seeding when suitable.At first to judge suitable seeding temperature during seeding, when seed crystal when melted silicon face in the quartz crucible contacts, observe seed crystal and the aperture situation after the melted silicon face contacts: during the seeding temperature drift; Seed crystal one contact fusion silicon liquid level aperture occurs, very bright, very black and very dazzling at once; Seed crystal seamed edge place wedge angle; Close circle and shake, even fusing, the pulling rate necking down can't be improved; When the seeding temperature was on the low side, seed crystal aperture do not occur with after the melted silicon face contacts, and seed crystal is not fused, and occurs the phenomenon that crystallization is outwards grown up on the contrary; Have only when the seeding temperature is suitable, seed crystal aperture slowly occurs, but does not have wedge angle with after fusion silicon liquid level contacts, and aperture is soft mellow and full, neither can grow up, and also can not dwindle and fuses.After welding was good, cooling just can begin to have carried out necking down slightly, and the purpose of necking down is in order to eliminate dislocation.After seeding is accomplished, pulling rate is reduced to 0.4mm/min, begin to amplify, reduce power simultaneously, the pulling rate size of the big I of the range of decrease during according to necking down, the thin speed that contracts decides, and adjusts power in real time.
After seeding is accomplished, just carry out shouldering, and can the phenomenon when observing shouldering judge the shouldering quality in the shouldering process.When the shouldering quality is good, can occur: the shoulder crest line is symmetrical, clear, tall and straight and continuous; The plane symmetry that occurs is smooth, bright, does not have cut channel; The shouldering angle is suitable, and surface smoothing, mellow and full does not have cut channel.And when shouldering is of poor quality: the shoulder crest line do not endure, intermittently, and cut channel is arranged, and explained that dislocation produces; The planar Flatness is poor, light inadequately, the time cut channel is arranged, dislocation generation be described; The shouldering angle is too big, has surpassed 180 °.In addition, the shouldering diameter will in time be measured, and has little time to change shoulder and makes crystal diameter bigger than normal in order to avoid mistake.
In the shouldering process, because amplification speed is very fast, the size of the diameter of monitoring shouldering in time is as the poor approximately 10mm of diameter during near target value; Can improve pulling rate to 2.5mm/min～4mm/min, getting into changes the shoulder operation, can see that the aperture that was positioned at the shoulder rear originally forwards surrounds quickly this moment; Last closed, can not dwindle in order to change shoulder back crystal diameter, a temperature can be fallen in advance; Takeed on Deng commentaries on classics, temperature head is seldom reacted, and diameter just can not dwindle.Aperture changes the shoulder process exactly by reaching closed process, and in this process, single crystal silicon is still being grown up, and just speed is more and more slower, no longer grows up at last, changes shoulder and has just accomplished.If this commentaries on classics shoulder speed control amount is just right, the diameter that just can let changes after takeing on just in time meets the requirements, and at this moment, falls pulling rate to the setting pulling rate, and catches up with the crucible liter in proportion, drops into automatic control diameter state, promptly carries out isometrical operation.If equipment operation is normal, the Rational Parameters of setting cooperates finely during man-machine handing-over, can normally proceed to afterbody during the crystalline isodiametric growth.
In the present embodiment; When reality is produced semiconductor grade silicon single crystal; Draw shoulder and shouldering process and all undertaken, and only be that the pulling rate with 3mm/min ± 0.3mm/min changes shoulder in changeing the shoulder process, like this when improving the shoulder process process of changeing, quickening monocrystalline silicon production efficient by common process; Crystalline growth velocity when changeing shoulder through improving crystal can effectively improve the section resistivity evenness of semiconductor grade silicon single crystal.The semiconductor grade silicon single crystal section central point resistivity and the section marginal point resistivity value that adopt common process to draw moulding differ bigger; Particularly obvious especially for the crystal of crystal head resistivity >=more than the 3 Ω cm, and can significantly improve the section resistivity evenness after adopting the present invention that the pulling rate that changes the shoulder process is limited.Simultaneously; After changeing the shoulder end; With pulling rate isodiametric growth 50mm ± 5mm of 1.6mm/min ± 0.1mm/min, owing to the growth conditions of the distribution of the thermal field in the single crystal growing furnace in this process and institute's produce single crystal silicon crystal is also all unstable, crystal production plays pendulum again; Thereby after pulling rate is limited to 1.6mm/min ± 0.1mm/min and isodiametric growth 50mm ± 5mm, can effectively control crystalline growth quality under the unsteady state; Simultaneously; Can guarantee effectively that current single crystal silicon of being grown carries out steady state by unsteady state behind pulling rate isodiametric growth 50mm ± 5mm with 1.6mm/min ± 0.1mm/min; Spend the transitory stage between unsteady state to the steady state in high quality, thereby can further improve the section resistivity evenness of semiconductor grade silicon single crystal.
In the actual production process; Under 1300 Gausses' athwartships magnetisation intensity effect; The natural convection of silicon melt receives this technical characterstic of good inhibition behind the melt; In changeing the shoulder process, remaining on simultaneously a very high crystalline growth velocity during with crystal growth (specifically is 3mm/min ± 0.3mm/min), can effectively eliminate the local melt back phenomenon at the semiconductor grade single crystal silicon crystallization position that produces like this, thereby has eliminated the swirl defect of the semiconductor grade single crystal silicon that draws.Simultaneously, the present invention can also improve the section resistivity evenness of semiconductor grade single crystal silicon, thereby can avoid the generation of " evil mind sheet " when eliminating semiconductor grade single crystal silicon swirl defect.
In the actual mechanical process, for single crystal growing furnace, its system inside all stores and the corresponding pulling rate control of the single crystal silicon curve that needs to produce any specification and model.Thereby in the actual mechanical process, when step 5 was drawn shoulder and shouldering, said single crystal growing furnace was controlled the pulling rate that draws in shoulder and the shouldering process according to predefined pulling rate control curve automatically; Change when shoulder in the step 6,, control said single crystal growing furnace and change shoulder with the pulling rate of 3mm/min ± 0.3mm/min artificially through the electric control box of said single crystal growing furnace; After step 7 transfer shoulder finishes, artificial again through the electric control box of said single crystal growing furnace, control the pulling rate isodiametric growth 50mm ± 5mm of said single crystal growing furnace with 1.6mm/min ± 0.1mm/min; Afterwards, said single crystal growing furnace is accomplished the follow-up isodiametric growth process that needs to make semiconductor grade silicon single crystal according to predefined pulling rate control curve.Thereby, actually control very easyly, realize convenient and be easy to grasping, practical effect is very good.
In the present embodiment, change when shoulder in the step 6, change shoulder with the pulling rate of 3mm/min; After step 7 transfer shoulder finishes, with the pulling rate isodiametric growth 50mm of 1.6mm/min; Afterwards, again by conventional isodiametric growth method, accomplish the follow-up isodiametric growth process that needs to make semiconductor grade silicon single crystal.In the actual use, can adjust accordingly above-mentioned pulling rate and isodiametric growth speed according to actual needs.
In the actual production process; After accomplishing the follow-up isodiametric growth process of semiconductor grade silicon single crystal in the step 7; Press the routine ending of pulling of silicon single crystal again and accomplish the subsequent production process that needs to make semiconductor grade silicon single crystal, perhaps adopt the treatment process that does not finish up to accomplish the subsequent production process that needs to make semiconductor grade silicon single crystal with stopping process.And when adopting the treatment process completion that does not finish up to need to make the subsequent production process of semiconductor grade silicon single crystal, its treatment process may further comprise the steps:
ⅰ, close the graphite thermal field system of single crystal growing furnace: carry out in the isodiametric growth process in the step 7; When the single crystal silicon length of isodiametric growth reaches the preseting length that needs making semiconductor grade silicon single crystal; Close the graphite thermal field system of single crystal growing furnace; And the heating power of said single crystal growing furnace reduced to zero, remaining silicon melt surface temperature reduces gradually in the said afterwards quartz crucible, begins crystallization until the surface of said silicon melt.
ⅱ, crystallization and crystal are lifted from fusion silicon liquid level: after the beginning crystallization of said silicon melt surface; Crystalline polamer to said silicon melt surface carries out simultaneous observation; When being 1mm～5mm when the crystallisate on said silicon melt surface and the gap between the current institute growing single-crystal silicon crystal; Through seed crystal rotary lifting mechanism set on the said single crystal growing furnace current single crystal silicon of growing is upwards promoted, and make the liquid level of current single crystal silicon of growing and said molten silicon body be separated.
ⅲ, crystal promote and get crystalline substance: through said seed crystal rotary lifting mechanism current single crystal silicon of growing is promoted in the secondary furnace chamber of single crystal growing furnace; Afterwards, close the segregaion valve between secondary furnace chamber of single crystal growing furnace and the single crystal growing furnace master furnace chamber, single crystal growing furnace master furnace chamber and the secondary furnace chamber of single crystal growing furnace are isolated; Subsequently, get crystal method, in the secondary furnace chamber of single crystal growing furnace, take out single crystal silicon, just accomplish the production process of silicon single crystal according to the routine of single crystal growing furnace.
In the prior art field, in the isodiametric growth process, treat the single crystal silicon isodiametric growth, remain under the few situation of material and will carry out tailing in work that the length that generally finishes up equals the diameter of institute's pulling monocrystal silicon crystal to afterbody.After ending is accomplished, stop that crucible changes, the brilliant commentaries on classics at once, stop crucible shaft, seed shaft moves up and down, and heating power drops to zero, cool off after 4～5 hours whole crystal pulling Production Flow Chart end.
In the actual production process; The purpose that isodiametric growth finishes up behind the afterbody mainly is; Ending can reduce the diameter of single crystal silicon, makes the useful area of the suffered thermal stresses effect of crystal afterbody reduce, like this when single crystal silicon is lifted from molten silicon body fluid face; The action effect of thermal stresses is reduced to minimum, thereby prevents the generation of dislocation to greatest extent.Under the normal circumstances; Atom in the silicon single crystal all is according in good order being arranged in together of the mode of diamond lattice structure; Dislocation then is that entanglement appears in the arrangement of Siliciumatom in the local area, belongs to the L&S line defect in the silicon single crystal, thereby will avoid as far as possible; The reason that produces dislocation is a lot; Wherein be that the viscous deformation that thermal stresses causes causes the generation of dislocation, if can effectively eliminate or reduce the generation that viscous deformation that thermal stresses causes can effectively prevent dislocation, the main purpose that finishes up in the existing technology is to prevent that dislocation from taking place.
But among the present invention; When the length of single crystal silicon growth reaches ending length; Be that single crystal silicon is during to afterbody; The method that does not finish up but take to close the graphite thermal field system of single crystal growing furnace is cooled off the silicon melt in the quartz crucible fast, and when the crystallization on silicon melt surface is about to touch silicon crystal, upwards promotes single crystal silicon rapidly and make crystal disengaging silicon melt level.Thereby the present invention compares with existing technology, has omitted the epilog in the single crystal silicon pulling process, has practiced thrift the PT, and the corresponding production efficiency that improves silicon single crystal.
Simultaneously; When the length of single crystal silicon growth reaches ending length; The present invention adopts the graphite thermal field system close single crystal growing furnace, and the heating power of said single crystal growing furnace is reduced to zero method, makes that remaining silicon melt surface temperature reduces and begin crystallization gradually in the quartz crucible; And when the crystallisate on silicon melt surface and the gap between the current institute growing single-crystal silicon crystal are 1mm～5mm, upwards promote single crystal silicon rapidly and make crystal disengaging silicon melt level.Thereby actually operating is very easy and be easy to control, and it is convenient to realize.In addition; Because the present invention reduces to beginning crystallization and crystallisation process in the silicon melt surface temperature to proceed to and lift from rapidly when gap between crystallisate and the crystal is 1mm～5mm fast; And the useful area of the suffered thermal stresses effect of single crystal silicon afterbody this moment is very little; When single crystal silicon was lifted from molten silicon body fluid face, the action effect of thermal stresses was reduced to minimum, thereby adopts the present invention can prevent the generation of dislocation to greatest extent like this; Reach the technique effect identical, can effectively guarantee the quality of institute's produce single crystal silicon crystal with tailing-in technique.
In the present embodiment, when the length of single crystal silicon growth reached ending length, the pot bottom material in the quartz crucible approximately remained 2kg; Make zero heating power moment this moment; Make silicon melt level generation crystallization, when crystallization is about to touch crystal, rapidly crystal and silicon melt level are broken away from.
Simultaneously, after melt described in the step 4 is accomplished and carry out before the seeding, also need carry out carrying slag behind the melt, it is following that it puies forward the slag process:
I, decrease temperature crystalline: reduce the heating power of single crystal growing furnace, and make the surface temperature of said silicon melt reduce gradually, begin crystallization until the surface of said silicon melt.
In the actual mechanical process, reduce heating power after melt is accomplished, make the silicon melt surface cooling, the temperature surperficial along with silicon melt descends gradually, and silicon melt level just begins to take place crystalline polamer.
II, progressively heat up and keep crystallisation process and carry out continuously; Insolubles until the silicon melt surface flotation is all condensed by crystallisate: after the beginning crystallization of said silicon melt surface, and the surface temperature of the heating power of the single crystal growing furnace that raises again and the said silicon melt that raises gradually; In the surface temperature of said silicon melt gradually in the elevation process; Crystalline polamer to said silicon melt surface carries out simultaneous observation; When the insolubles that observes said silicon melt surface flotation is all condensed by the crystallisate on said silicon melt surface; Through seed crystal rotary lifting mechanism set on the said single crystal growing furnace said seed crystal is dropped to said crystallisate and to contact; And after treating said seed crystal and said crystallisate welding, will condense through said seed crystal rotary lifting mechanism has the crystallisate of insolubles to be promoted in the secondary furnace chamber of single crystal growing furnace; Afterwards, close said segregaion valve, single crystal growing furnace master furnace chamber and the secondary furnace chamber of single crystal growing furnace are isolated.
During actually operating; After the silicon melt level crystallization took place, the heating power that raises immediately heated up, owing to heat up a process was arranged; Thereby in temperature-rise period; The crystallization of silicon melt level still can be carried out, and does like this to prevent the whole crystallisation problems of the silicon melt level that causes owing to crystallization velocity is too fast, to prevent causing the phenomenon that cracks to take place to quartz crucible after the whole crystallizations of silicon melt level.Thereby, when keeping crystallisation process and continuing to carry out,, too fast to prevent crystallization velocity through reducing temperature gradually.
Thereby; In the step II in the surface temperature of said silicon melt gradually in the elevation process; And before the insolubles of said silicon melt surface flotation is all condensed by the crystallisate on said silicon melt surface, the crystallisation process on said silicon melt surface is observed, when observation finds that the crystallisation process on said silicon melt surface is about to stop; Reduce the heating power of single crystal growing furnace immediately, and make the crystallisation process on said silicon melt surface continue to carry out; And after reducing the heating power of single crystal growing furnace, when the crystallization velocity on said silicon melt surface accelerate to the step I in crystallization velocity during beginning crystallization when consistent, the heating power of the single crystal growing furnace that raises again.To sum up; In the actual mechanical process,, and the heating power of single crystal growing furnace is carried out lift adjustment according to observed result through the crystallisation process on the said silicon melt of simultaneous observation surface; And through adjusting the heating power of single crystal growing furnace; The silicon melt level temperature is carried out lift adjustment, thereby when guaranteeing that crystallisation process continues to carry out, also can effectively prevent the whole crystallisation problems of the too fast silicon melt level that causes of crystallization velocity.Thereby actually operating is very easy, and is workable, and crystallisation process is safe and reliable.
III, scarfing cinder: the routine according to single crystal growing furnace is got crystal method, in the secondary furnace chamber of single crystal growing furnace, takes out seed crystal, and removes the crystallisate of seed crystal bottom institute welding, then accomplishes the slag process of putting forward behind the melt;
IV, replacing seed crystal: the seed crystal in the secondary furnace chamber of single crystal growing furnace, taking out in the step III is changed;
After having changed seed crystal in the step IV, the bell of the single crystal growing furnace that closes is also opened said segregaion valve; Subsequently, utilize the seed crystal after changing and press the conventional treatment process of vertical pulling method, accomplish seeding, shouldering, commentaries on classics shoulder and isodiametric growth process successively.
In the present embodiment, the seed crystal of being adorned on the said seed chuck before changing in the step IV is to carry out carrying behind the melt that slag handles carries the slag seed crystal, and the said slag seed crystal of carrying is new seed crystal or the used old seed crystal that had not used after completing; Seed crystal after changing in the step IV is the new seed crystal that had not used after completing.
Thereby during actually operating, the bits (being insolubles) that soon will float on liquid level when crystallisate are fallen and are carried the slag seed crystal when all condensing, and with thin neck crystallisate are clung, and are lifted into secondary furnace chamber, just accomplish the slag process of putting forward.In the present embodiment, said old seed crystal has venturi portion for adopting the seed crystal after vertical pulling method draws completion silicon single crystal on this old seed crystal.
To sum up; In the actual use; Adopt put forward the slag process behind above-mentioned steps I to the described melt of IV after, can be simple, convenient and a large amount of contaminant removals of after melt is accomplished, containing in the silicon material apace, thus bonding crystal silicon production process is carried out safely and fast.If do not understand not fusant of buoyant one deck because do not remove on the silicon melt surface; Not only can influence the inner quality of purification single crystal silicon; And can influence the growth of bill of lading crystal silicon crystalline, exception throw crystallization, intractability this moment high and need cost great amount of time and energy; When reducing production efficiency and silicon single crystal quality, also may cause industrial accident.
Simultaneously; After proposing the slag end, also need among the present invention change to seed crystal; Be that whole monocrystalline silicon production process adopts two seed crystals, wherein put forward the slag process of putting forward after the slag seed crystal is used for melt, finish the pulling process that seed crystal after the back is changed is used for follow-up single crystal silicon and carry slag.Incidental seed crystal breakage problem when the purpose of two seed crystals of employing is effectively to avoid only using a seed crystal to propose slag and crystal drawing, and cause single crystal silicon to crash into quartz crucible and initiation leakage silicon accident after the seed crystal fracture.Because actual carrying in the slag process, the temperature variation of seed crystal is very violent, thereby causes the seed crystal fracture easily; Moreover, carry a large amount of impurity entering seed crystals in the slag process, also can cause the seed crystal fracture.Therefore, adopt the present invention after carrying the seed crystal that more renews after slag finishes, can effectively avoid taking place the seed crystal phenomenon of rupture, improved the security of producing largely, reduced the probability of occurrence that leaks the silicon accident, the silicon material is purified to produce to be significant; And also correspondingly guaranteed the monocrystalline silicon production process fast, effectively carry out; When reducing accident rate; The also corresponding production efficiency that improves silicon single crystal makes because accident causes the temporary transient probability that stops production or keep in repair to reduce, and has not only practiced thrift production and maintenance cost; Save the servicing time after a large amount of accidents, made the monocrystalline silicon production efficient of whole producer be greatly improved.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every technical spirit changes any simple modification, change and the equivalent structure that above embodiment did according to the present invention, all still belongs in the protection domain of technical scheme of the present invention.
Claims (6)
1. semiconductor grade monocrystalline silicon production technology is characterized in that this technology may further comprise the steps:
Step 1, transverse magnetic field are laid: a transverse magnetic field is laid in the outside in the middle part of producing the single crystal growing furnace master furnace chamber that needs making semiconductor grade silicon single crystal, and the magneticstrength of said transverse magnetic field is 1300 Gausses ± 100 Gausses;
Step 2, silicon raw material and doping agent are prepared: according to the conventional preparation method of single crystal growing furnace with the silicon raw material, prepare the silicon raw material that the growth pulling of silicon single crystal is used, and press the conventional cleaning method of single crystal growing furnace with the silicon raw material, the silicon raw material of preparing is carried out clean; Simultaneously,, need to confirm the kind and the doping of interpolation doping agent, and the doping agent that the growth pulling of silicon single crystal is used is prepared according to model and the resistivity that need are made semiconductor grade silicon single crystal;
Step 3, charging:, ready silicon raw material and doping agent in the step 1 are put into respectively in the quartz crucible that has been in place according to the conventional loading method of single crystal growing furnace; Simultaneously, the previously prepd seed crystal is installed on the seed chuck in the said single crystal growing furnace;
Step 4, melt: the conventional melt method according to single crystal growing furnace, melt silicon raw material and doping agent in the said quartz crucible of packing in the step 2, until said silicon raw material and whole fusings of doping agent and acquisition silicon melt;
Step 5, draw shoulder and shouldering: after melt is accomplished, adopt single crystal growing furnace and draw shoulder and shouldering method according to the routine of pulling of silicon single crystal, accomplish need to make semiconductor grade silicon single crystal draw shoulder and shouldering process;
Step 6, change shoulder: when changeing shoulder after shouldering finishes, change shoulder with the pulling rate of 3mm/min ± 0.3mm/min;
Step 7, isodiametric growth: after changeing the shoulder end, with pulling rate isodiametric growth 50mm ± 5mm of 1.6mm/min ± 0.1mm/min; Afterwards, press the conventional isodiametric growth method of pulling of silicon single crystal again, accomplish the follow-up isodiametric growth process that needs to make semiconductor grade silicon single crystal;
After melt is accomplished in the step 4 and carry out before the seeding, also need carry out carrying slag behind the melt, it is following that it puies forward the slag process:
I, decrease temperature crystalline: reduce the heating power of single crystal growing furnace, and make the surface temperature of said silicon melt reduce gradually, begin crystallization until the surface of said silicon melt;
II, progressively heat up and keep crystallisation process and carry out continuously; Insolubles until the silicon melt surface flotation is all condensed by crystallisate: after the beginning crystallization of said silicon melt surface, and the surface temperature of the heating power of the single crystal growing furnace that raises again and the said silicon melt that raises gradually; In the surface temperature of said silicon melt gradually in the elevation process; Crystalline polamer to said silicon melt surface carries out simultaneous observation; When the insolubles that observes said silicon melt surface flotation is all condensed by the crystallisate on said silicon melt surface; Through seed crystal rotary lifting mechanism set on the said single crystal growing furnace said seed crystal is dropped to said crystallisate and to contact; And after treating said seed crystal and said crystallisate welding, will condense through said seed crystal rotary lifting mechanism has the crystallisate of insolubles to be promoted in the secondary furnace chamber of single crystal growing furnace; Afterwards, close said segregaion valve, single crystal growing furnace master furnace chamber and the secondary furnace chamber of single crystal growing furnace are isolated;
III, scarfing cinder: the routine according to single crystal growing furnace is got crystal method, in the secondary furnace chamber of single crystal growing furnace, takes out seed crystal, and removes the crystallisate of seed crystal bottom institute welding, then accomplishes the slag process of putting forward behind the melt; Afterwards, close single crystal growing furnace bell and open said segregaion valve.
2. according to the described a kind of semiconductor grade monocrystalline silicon production technology of claim 1, it is characterized in that: the magneticstrength of transverse magnetic field described in the step 1 is 1300 Gausses ± 20 Gausses.
3. according to claim 1 or 2 described a kind of semiconductor grade monocrystalline silicon production technologies; It is characterized in that: when step 5 is drawn shoulder and shouldering; Said single crystal growing furnace is controlled the pulling rate that draws in shoulder and the shouldering process according to predefined pulling rate control curve automatically; Change when shoulder in the step 6,, control said single crystal growing furnace and change shoulder with the pulling rate of 3mm/min ± 0.3mm/min artificially through the electric control box of said single crystal growing furnace; After step 7 transfer shoulder finishes, artificial again through the electric control box of said single crystal growing furnace, control the pulling rate isodiametric growth 50mm ± 5mm of said single crystal growing furnace with 1.6mm/min ± 0.1mm/min; Afterwards, said single crystal growing furnace is accomplished the follow-up isodiametric growth process that needs to make semiconductor grade silicon single crystal according to predefined pulling rate control curve.
4. according to the described a kind of semiconductor grade monocrystalline silicon production technology of claim 3, it is characterized in that: change when shoulder in the step 6, change shoulder with the pulling rate of 3mm/min; After step 7 transfer shoulder finishes, with the pulling rate isodiametric growth 50mm of 1.6mm/min; Afterwards, again by conventional isodiametric growth method, accomplish the follow-up isodiametric growth process that needs to make semiconductor grade silicon single crystal.
5. according to claim 1 or 2 described a kind of semiconductor grade monocrystalline silicon production technologies; It is characterized in that: the transverse magnetic field described in the step 1 is made up of two blocks of PMs that are laid in the left and right sides, single crystal growing furnace master furnace chamber middle part respectively, and two blocks of said PMs are symmetry and lay.
6. according to the described a kind of semiconductor grade monocrystalline silicon production technology of claim 1, it is characterized in that: accomplish in the step III behind the melt put forward the slag process after, also need change to the seed crystal that in the secondary furnace chamber of single crystal growing furnace, takes out in the step III; And after having changed seed crystal, the bell of the single crystal growing furnace that closes is again also opened said segregaion valve.
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