CN202144523U - Device for increasing consistency of longitudinal resistivity of mono-crystal silicon - Google Patents

Device for increasing consistency of longitudinal resistivity of mono-crystal silicon Download PDF

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Publication number
CN202144523U
CN202144523U CN201120247524U CN201120247524U CN202144523U CN 202144523 U CN202144523 U CN 202144523U CN 201120247524 U CN201120247524 U CN 201120247524U CN 201120247524 U CN201120247524 U CN 201120247524U CN 202144523 U CN202144523 U CN 202144523U
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quartz
single crystal
crucible
quartz tube
quartz crucible
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周建华
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XI'AN HUAJING ELECTRONIC TECHNOLOGY Co Ltd
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XI'AN HUAJING ELECTRONIC TECHNOLOGY Co Ltd
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Abstract

The utility model discloses a device for increasing the consistency of longitudinal resistivity of mono-crystal silicon. The device comprises a mono-crystal furnace, wherein the mono-crystal furnace comprises a primary furnace chamber and a secondary furnace chamber; the primary furnace chamber is internally provided with a quartz crucible, a diversion cylinder which is arranged right above the quartz crucible, a graphite crucible which is sheathed outside the quartz crucible and a graphite thermal field system which is arranged right below the graphite crucible; the primary furnace chamber also comprises a quartz cylinder which is horizontally placed at the inside middle part of the quartz crucible; the quartz cylinder and the quartz crucible are arranged coaxially, and the top of the quartz cylinder is not higher than the top of the quartz crucible; a plurality of through holes which are used for communicating the inner cavity of the quartz crucible with the inner cavity of the quartz cylinder are arranged at the bottom of the quartz cylinder along the peripheral direction; the structures and the sizes of the through holes are the same; and the through holes are arranged uniformly. The device for increasing the consistency of the longitudinal resistivity of the mono-crystal silicon is simple in structure, reasonable in design, simple and convenient to use and operate, convenient to realize and good in use effect; the resistivity at the head and tail parts of the drawn mono-crystal silicon is basically consistent; and the consistency of the longitudinal resistivity of the mono-crystal silicon is greatly improved.

Description

The conforming device of a kind of raising silicon single crystal longitudinal resistivity
Technical field
The utility model belongs to the monocrystalline silicon production technical field, especially relates to the conforming device of a kind of raising silicon single crystal longitudinal resistivity.
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.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.
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 silicon single-crystal.Adopt single crystal growing furnace to produce in the silicon single-crystal process,, just will select the suitable doping agent for use for drawing the silicon single-crystal of certain model and resistivity.The group-v element N type doping agent of making silicon single crystal commonly used mainly contains phosphorus, arsenic, antimony etc.The group iii elements P type doping agent of making silicon single crystal commonly used mainly contains boron, aluminium, gallium etc.In general, (resistivity is less than 10 to draw the low-resistivity monocrystalline -2Ω cm), generally select the pure element doping agent for use.(resistivity is greater than 10 for the monocrystalline of drawing higher electric resistivity -1Ω cm), generally select for use mother alloy to make doping agent.So-called " mother alloy " is exactly the alloy of impurity element and silicon.Mother alloy commonly used has two kinds of silicon phosphorus and silicon boron, the employing mother alloy do doping agent be for make doping control more easily, more accurate.
But the actual single crystal growing furnace that adopts is produced in the silicon single-crystal process; Because the alloying element of the above-mentioned doping agent velocity of diffusion of growth interface place solid-liquid two in mutually in silicon single-crystal is different; Thereby it is inconsistent to cause drawing moulding silicon single-crystal crystalline longitudinal resistivity, promptly draws moulding silicon single-crystal crystalline resistivity and is reduced gradually by head to afterbody.Especially for N type silicon single-crystal, the resistivity of its silicon single-crystal crystal between end to end differs big especially.For example, the resistivity of the semiconductor grade silicon single crystal of producing is comparatively serious by the decay of head to afterbody at present, the about 38 Ω cm of the resistivity of semiconductor grade silicon single crystal head, the about 32 Ω cm of resistivity at semiconductor grade silicon single crystal middle part, and the about 20 Ω cm of the resistivity of its afterbody.
The utility model content
The utility model technical problem to be solved is to above-mentioned deficiency of the prior art; Provide a kind of raising silicon single crystal longitudinal resistivity conforming device; It is simple in structure, reasonable in design, use is easy and simple to handle, realization is convenient and result of use is good; The resistivity of silicon single-crystal head and the afterbody of drawing is consistent basically, has improved the longitudinal resistivity consistence of silicon single-crystal greatly.
For solving the problems of the technologies described above; The technical scheme that the utility model adopts is: the conforming device of a kind of raising silicon single crystal longitudinal resistivity; Comprise single crystal growing furnace; Said single crystal growing furnace comprises single crystal growing furnace body of heater and the power cabinet that is laid in the single crystal growing furnace body of heater outside; Said single crystal growing furnace body of heater comprises main furnace chamber and the secondary furnace chamber that is positioned at directly over the main furnace chamber; Be provided with quartz crucible in the said main furnace chamber, be laid in guide shell directly over the quartz crucible, be sleeved on the plumbago crucible in the quartz crucible outside and be laid in the graphite thermal field system under the plumbago crucible, set terminals join on said graphite thermal field system and the power cabinet, it is characterized in that: also comprise the quartz tube that lies in a horizontal plane in the quartz crucible middle inside; Said quartz tube is that the cylindrical barrel of equal opening up and down and the wall thickness of said cylindrical barrel are 3mm~10mm, and the external diameter of said quartz tube is 1/2~1/3 of its quartz crucible internal diameter of living in; Said quartz tube is coaxial laying with quartz crucible, and the overhead height of quartz tube is not higher than the overhead height of quartz crucible; Said quartz tube bottom along the circumferential direction has and is used for a plurality of through holes that the quartz crucible inner chamber is communicated with the quartz tube inner chamber, and the structure of a plurality of said through holes and a plurality of said through holes all identical with size are even laying.
The conforming device of above-mentioned a kind of raising silicon single crystal longitudinal resistivity is characterized in that: the top flush of the top of said quartz tube and quartz crucible, perhaps the overhead height of quartz tube is than the low 2cm~3cm of overhead height of quartz crucible.
The conforming device of above-mentioned a kind of raising silicon single crystal longitudinal resistivity, it is characterized in that: the cross-sectional area of said through hole is 6mm 2~40mm 2, and the cross-sectional area of said through hole is big more, and the quantity in the hole of opening is few more.
The conforming device of above-mentioned a kind of raising silicon single crystal longitudinal resistivity, it is characterized in that: the quantity of said through hole is 6~2.
The conforming device of above-mentioned a kind of raising silicon single crystal longitudinal resistivity is characterized in that: said through hole is out the groove on quartz tube bottom sides edge.
The conforming device of above-mentioned a kind of raising silicon single crystal longitudinal resistivity is characterized in that: said groove is that diameter is the semi-circular groove of 2mm~5mm.
The conforming device of above-mentioned a kind of raising silicon single crystal longitudinal resistivity, it is characterized in that: the quantity of said through hole is 3.
The conforming device of above-mentioned a kind of raising silicon single crystal longitudinal resistivity, it is characterized in that: the wall thickness of said cylindrical barrel is 5mm~10mm.
The utility model compared with prior art has the following advantages:
1, simple in structure, reasonable in design and input cost is low.
2, the quartz crucible that only needs to have now single crystal growing furnace is changed into double-deck crucible and is got final product; Thereby the utility model is the novel single crystal growing furnace of quartz crucible being changed into double-deck crucible in fact, and it need not other part-structure, annexation and the principle of work of single crystal growing furnace are carried out any improvement or adjustment.
3, use is easy to operate, and is roughly the same with the operating procedure of existing single crystal growing furnace, and the difference part only is after the quartz crucible shove charge, also needs in the inner placement of the quartz crucible that is in place quartz tube, and guarantees that quartz tube steadily is being positioned over the quartz crucible middle inside.
4, treatment process steps is simple and realize conveniently, is easy to grasp, and all the pulling of crystals method with existing single crystal growing furnace is identical with charging subsequent disposal operation afterwards for the preparatory process before the shove charge, only is that shove charge operation and stocking process have been carried out corresponding adjustment.
5, the silicon single-crystal longitudinal resistivity high conformity of the good and moulding that draws of result of use, the resistivity that adopts the utility model to draw silicon single-crystal head and afterbody is consistent basically, has improved the longitudinal resistivity consistence of silicon single-crystal greatly.
In sum, the utility model is reasonable in design, use is easy and simple to handle, realization is convenient and result of use is good, and the resistivity of silicon single-crystal head and the afterbody of drawing is consistent basically, has improved the longitudinal resistivity consistence of silicon single-crystal greatly.
Through accompanying drawing and embodiment, the technical scheme of the utility model is done further detailed description below.
Description of drawings
Fig. 1 is the structural representation of the utility model.
Fig. 2 is the right view of Fig. 1.
Fig. 3 by in the utility model master furnace chamber the installation site synoptic diagram of the double-deck crucible of employing.
Fig. 4 by the utility model the perspective view of employing quartz tube.
Processing technological flow block diagram when Fig. 5 improves silicon single crystal longitudinal resistivity consistence for adopting the utility model.
Description of reference numerals:
Figure BDA0000075915030000041
Embodiment
Like Fig. 1, Fig. 2, Fig. 3 and shown in Figure 4; The utility model comprises single crystal growing furnace; Said single crystal growing furnace comprises single crystal growing furnace body of heater and the power cabinet 10 that is laid in the single crystal growing furnace body of heater outside; Said single crystal growing furnace body of heater comprises main furnace chamber 6 and the secondary furnace chamber 4 that is positioned at directly over the main furnace chamber 6; Be provided with quartz crucible 17-1 in the said main furnace chamber 6, be laid in guide shell directly over the quartz crucible 17-1, be sleeved on the plumbago crucible 17-2 in the quartz crucible 17-1 outside and be laid in the graphite thermal field system under the plumbago crucible 17-2, set terminals join on said graphite thermal field system and the power cabinet 10.Simultaneously; The utility model also comprises the quartz tube 17-3 that lies in a horizontal plane in quartz crucible 17-1 middle inside; Said quartz tube 17-3 is that the cylindrical barrel of equal opening up and down and the wall thickness of said cylindrical barrel are 3mm~10mm, and the external diameter of said quartz tube 17-3 is 1/2~1/3 of its quartz crucible 17-1 internal diameter of living in.Said quartz tube 17-3 and quartz crucible 17-1 are coaxial laying, and the overhead height of quartz tube 17-3 is not higher than the overhead height of quartz crucible 17-1.Said quartz tube 17-3 bottom along the circumferential direction has and is used for a plurality of through holes that quartz crucible 17-1 inner chamber is communicated with quartz tube 17-3 inner chamber, and the structure of a plurality of said through holes and a plurality of said through holes all identical with size are even laying.Said quartz crucible 17-1 and the quartz tube 17-3 that is positioned at quartz crucible 17-1 form double-deck crucible.
Actual processing and fabricating and installing constantly, the top flush of the top of said quartz tube 17-3 and quartz crucible 17-1, perhaps the overhead height of quartz tube 17-3 hangs down 2cm~3cm than the overhead height of quartz crucible 17-1.Can be according to the concrete needs of reality; Height to quartz tube 17-3 adjusts accordingly; After making that quartz tube 17-3 level is put into quartz tube 17-3 inside; The overhead height of said quartz tube 17-3 is identical with the overhead height of quartz crucible 17-1, and perhaps the overhead height of quartz tube 17-3 is than the low 2cm~3cm of overhead height of quartz crucible 17-1.In the present embodiment, the overhead height of said quartz tube 17-3 is than the low 2cm of overhead height of quartz crucible 17-1.
Reality adds man-hour to said through hole, and the cross-sectional area of said through hole is 6mm 2~40mm 2, and the cross-sectional area of said through hole is big more, and the quantity in the hole of opening is few more.Thereby in the course of processing, can be according to the quantity of processing through hole, the cross-sectional area in opening hole is adjusted accordingly.Actually add man-hour, the quantity of said through hole is 6~2.
Convenient for perforate, in the present embodiment, said through hole is out the groove on quartz tube 17-3 bottom sides edge.The shape of said groove is not limit, and can be rectangular tank, vee gutter, semi-circular groove 20, half elliptic groove or other just changeable shape groove etc.Actually add man-hour, can select the flute profile of said groove according to actual needs.
In the present embodiment, the quantity of said groove is 3, and said groove is that diameter is the semi-circular groove 20 of 2mm~5mm.Actually add man-hour, adjust accordingly according to the diameter of the said quartz tube 17-3 diameter to institute's open semicircle shape groove 20, the diameter of said quartz tube 17-3 is big more, and the diameter of institute's open semicircle shape groove 20 is big more.
In the present embodiment, the wall thickness of said cylindrical barrel is 5mm~10mm.Actually add man-hour, according to the diameter of said quartz tube 17-3 its wall thickness is adjusted accordingly, the diameter of said quartz tube 17-3 is big more, and the wall thickness of quartz tube 17-3 is big more.
To sum up, the utility model only partly adjusts accordingly the crucible of existing single crystal growing furnace, specifically is in quartz crucible 17-1, to put into a quartz tube 17-3, so just forms a double-deck crucible of being made up of quartz crucible 17-1 and quartz tube 17-3.And the utility model does not all change other part-structure that has single crystal growing furnace now, and in conjunction with Fig. 1 and Fig. 2, the said single crystal growing furnace body of heater outside also is provided with electric control box 11 and housing 15, and said single crystal growing furnace body of heater is installed on the frame 8.The seed crystal rotation and lifting mechanism 1 that seed crystal is rotated and lifts is equipped with on said secondary furnace chamber 4 tops; And in the crystal pulling process; The main effect of said seed crystal rotation and lifting mechanism 1 provides brilliant the liter and brilliant rotary speed, and the switching value through the PCC control module changes the crystal diameter of controlling the silicon single-crystal that draws.Said seed crystal rotation and lifting mechanism 1 joins through stay cord and weight, and the seed chuck 2 that seed crystal is carried out clamping is fixed under the said weight; Simultaneously, said secondary furnace chamber 4 sidepieces are equipped with body of heater up-down opener 3, and the effect of said body of heater up-down opener 3 is mechanisms that secondary furnace chamber 4 is gone up and down and opens.Be provided with segregaion valve 5 between said secondary furnace chamber 4 and the main furnace chamber 6.Said graphite thermal field system comprises the main heat-preservation cylinder that is laid in the main furnace chamber 6, is laid in well heater, the Graphite Electrodes 7 that is electrically connected with well heater of plumbago crucible 17-2 below and is laid in directly over the quartz crucible 17-1 and the diminishing guide shell of bore from top to bottom.Said guide shell comprises external flow guiding cylinder and the inner draft tube that is sleeved in the external flow guiding cylinder, and the top of said main heat-preservation cylinder is provided with heat-preservation cylinder and its underpart is provided with down heat-preservation cylinder; Said Graphite Electrodes 7 is laid in down in the heat-preservation cylinder and stretch out autonomous furnace chamber 6 bottoms, bottom, and said external flow guiding cylinder and inner draft tube are laid in the heat-preservation cylinder.For silicon monocrystal growth, reasonably thermal field distributes and be: at first, the longitudinal temperature gradient at crystalizing interface place is big as far as possible, so just can make silicon monocrystal growth that enough power is arranged; But can not be excessive, silicon single-crystal can well be grown, and can not produce textural defect again and brilliant the change taken place; And should be that longitudinal temperature gradient changes smoothly, there is not the temperature jump zone, do not make silicon monocrystal growth receive bigger thermal shocking; as far as possible Simultaneously, the radial symmetry gradient at growth interface place approaches zero as far as possible, to guarantee that crystalizing interface is smooth.
Simultaneously, during actual the installation, said plumbago crucible 17-2 bottom is equipped with pot holder 18, and pot holder 18 under pressure pin 19 is installed, said quartz crucible 17-1 is laid in the said main heat-preservation cylinder.In addition, said main furnace chamber 6 belows also are provided with places the crucible driving mechanism 9 of quartz tube 17-3 (the being said double-deck crucible) driving of going up and down to quartz crucible 17-1 together with its inside, and said crucible driving mechanism 9 is in transmission connection with pressure pin 19.Said electric control box 11 respectively with said single crystal growing furnace in need carry out electrical control the electricity consumption assembly join, and the electricity consumption assembly carries out corresponding control.Said single crystal growing furnace also comprises argon gas feed device 12, cooling system 13 and to vacuumizing the vacuum system 14 of processing in the single crystal growing furnace body of heater, the argon gas that joins with argon gas feed device 12 charges into pipeline deeply to secondary furnace chamber 4.In addition, said main furnace chamber 6 outsides also are provided with main furnace body hoisting appliance 16 that main furnace chamber 6 is gone up and down.The argon gas that said argon gas feed device 12 is provided is in czochralski silicon monocrystal technology; Has important effect: on the one hand; It is enclosed in silicon single-crystal crystal and the crucible around the fusion silicon liquid level as a kind of protective atmosphere, and broken belt is not walked the volatile matter in the silicon solution, and the volatile matter at other position under the high temperature; And, protected the normal growth of silicon single-crystal by the mechanical pump eliminating; On the other hand, it from top to bottom forms uniform laminar flow and skims over from the silicon single-crystal plane of crystal, takes away crystallization latent heat, also helps silicon monocrystal growth.The bottom pad of said pot holder 18 is equipped with thermally-insulated body 21, and the middle and upper part of said thermally-insulated body 21 is provided with thermally-insulated body insulation quilt 22.
As shown in Figure 5, the working process of the utility model may further comprise the steps:
Step 1, silicon feedstock production and clean:, prepare the silicon raw material that the growth pulling of silicon single crystal is used according to the preparation method of conventional single crystal growing furnace with the silicon raw material; According to the cleaning method of conventional single crystal growing furnace, the silicon raw material of preparing is carried out clean simultaneously with the silicon raw material.
In the present embodiment, identical with the method for silicon raw material with routine preparation growth pulling of silicon single crystal, elder generation is according to the specification and the size of need making 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 the making silicon single-crystal.The prepared silicon raw material that goes out refers to the raw material that carries out crystal-pulling among the quartz crucible 17-2 for 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 guarantee the quality of production silicon single-crystal, the used polycrystalline silicon material of drawing silicon single-crystal 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 doping agent, make the model and the resistivity of silicon single-crystal earlier according to need, and confirm to add the kind and the doping of doping agent according to ordinary method.
Step 2, shove charge, its loading furnace process is following:
201, quartz crucible is packed into: according to the conventional shove charge method of crucible in the single crystal growing furnace, the quartz crucible 17-1 that the outside is set with plumbago crucible 17-2 packs in the main furnace chamber 6.
202, quartz tube is packed into: quartz tube 17-3 is lain in a horizontal plane in the quartz crucible 17-1 of the main furnace chamber (6) of packing into, and make quartz tube 17-3 be positioned at the middle inside of quartz crucible 17-1.That is to say that the central axis of the quartz tube 17-3 in the quartz crucible 17-1 that packs into and the central axis of quartz crucible 17-1 are located along the same line.
Step 3, charging, its charging process is following:
301, quartz tube is fixed: in step 1, take out 1000g~2000g silicon raw material in the silicon raw material after the clean earlier and be tiled in the inside bottom of quartz tube 17-3, and corresponding acquisition one layer thickness is d 1Silicon raw material shop layer; Afterwards, with the silicon raw material after the clean in the step 1, silicon material packing layer is filled and formed to the annular region between quartz tube 17-3 and the quartz crucible 17-1, and the bed thickness of said silicon material packing layer is 2d 1± 0.5d 1
In the present embodiment, the thickness d of the raw material of silicon described in the step 301 shop layer 1=3cm~5cm, and the bed thickness of said silicon material packing layer is 2d 1In the actual process, should the thickness of silicon raw material shop layer and the bed thickness of silicon material packing layer be adjusted accordingly according to the concrete needs of reality.
302, silicon raw material and doping agent are packed into: with the silicon raw material after the clean in the step 1, be respectively charged in quartz tube 17-3 and the said annular region; And in the silicon raw material process of in quartz tube 17-3, packing into, the charge level height of the silicon raw material of adorning in the quartz tube 17-3 is carried out simultaneous observation, the charge level height of the silicon raw material of adorning rises to height h in quartz tube 17-3 1The time, grow doping agent that pulling of silicon single crystal uses of previously prepd is all packed in the quartz tube 17-3; Afterwards, the silicon raw material after the clean in the step 1 is all packed in quartz tube 17-3 and the said annular region, just accomplish the charging process; After charging finishes, in the quartz tube 17-3 with said annular region in the charge level height flush of the silicon raw material of adorning, and the charge level height of the interior silicon raw material of adorning of quartz tube 17-3 is h 0Wherein, h 1=0.7h 0± 0.5h 0
In the present embodiment, the height h described in the step 302 1=0.7h0.In the actual process, can be according to the concrete needs of reality, to height h 1Adjust accordingly.
Step 4, subsequent disposal: after charging is accomplished in the step 3; Adopt said single crystal growing furnace and by conventional vertical pulling method treatment process; Accomplish successively and close stove, vacuumize, after melt, seeding, shouldering, commentaries on classics shoulder, isometrical, ending and the blowing out operation, just obtain to draw the silicon single-crystal of moulding.
In the actual production process; Before in step 2, feeding; Also need tear stove earlier open; The purpose of tearing stove open is in order to have drawn the silicon single-crystal crystal 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 7, 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 4 afterwards, and close when being inflated to furnace pressure for barometric point.Actual when getting crystalline substance, through body of heater up-down opener 3 secondary furnace chamber 4 (perhaps with secondary furnace chamber 4 together with bell together) is raised to upper limit position earlier after, slow revolute furnace chamber 4 is got crystalline substance afterwards again till taking out the silicon single-crystal crystal.When reality is torn stove open to main furnace chamber 6, take out guide shell, quartz crucible 17-1 and plumbago crucible 17-2 and quartz tube 17-3, pot holder, pressure pin and thermal field heating 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.
In the present embodiment, when carrying out subsequent disposal in the step 4, need to handle by conventional vertical pulling method treatment process.At first, before the melt, closed fire door earlier,, just can hunt leak, and confirmed that the voltage rise rate meets the requirements and just can heat by starting power cabinet 10 until being extracted into pressure drop to 3Pa to vacuumizing in the burner hearth.Before starting power cabinet 10 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 plumbago crucible 17-2 and the quartz tube 17-3 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 double-deck crucible of crucible driving mechanism 9.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, double-deck 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 1.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 double-deck 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, the silicon single-crystal crystal 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.
Treat the silicon single-crystal isodiametric growth of crystal to afterbody, remain under the few situation of material and will carry out tailing in work that the length that generally finishes up equals the silicon single-crystal crystalline diameter that draws.After ending is accomplished, stops 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 finishes.
To sum up; The conforming device of the said raising silicon single crystal of the utility model longitudinal resistivity is the novel single crystal growing furnace of the crucible to existing single crystal growing furnace after improving, and the subsequent treatment process after the preparatory process before its shove charge and the shove charge end all the treatment process with existing single crystal growing furnace is identical.When adopting the utility model to draw silicon single-crystal; Quartz tube 17-3 through have through hole with the bottom is separated into two portions with the molten silicon of the liquid phase in the quartz crucible 17-1; And only the molten silicon of the liquid phase in the quartz tube 17-3 is mixed during actual the doping; The silicon single-crystal crystal is only grown in quartz tube 17-3 like this, and along with the growth of silicon single-crystal crystalline, the through hole that the molten silicon of liquid phase of quartz tube 17-3 outside undoped is constantly opened through quartz tube 17-3 bottom gets in the quartz tube 17-3; And constantly dilute the molten silicon of adulterated liquid phase in the quartz tube 17-3, make the molten sila matter concentration of liquid phase in the quartz tube 17-3 be stabilized in the impurity concentration value of mixing the target resistivity correspondence in advance always.Thereby the silicon single-crystal head that employing the utility model draws out and the resistivity of afterbody are consistent basically, have improved the longitudinal resistivity consistence of silicon single-crystal greatly.
The above; It only is the preferred embodiment of the utility model; Be not that the utility model is done any restriction; Everyly any simple modification that above embodiment did, change and equivalent structure are changed, all still belong in the protection domain of the utility model technical scheme according to the utility model technical spirit.

Claims (8)

1. one kind is improved the conforming device of silicon single crystal longitudinal resistivity; Comprise single crystal growing furnace; Said single crystal growing furnace comprises single crystal growing furnace body of heater and the power cabinet (10) that is laid in the single crystal growing furnace body of heater outside; Said single crystal growing furnace body of heater comprises main furnace chamber (6) and is positioned at the secondary furnace chamber (4) directly over the main furnace chamber (6); Be provided with quartz crucible (17-1) in the said main furnace chamber (6), be laid in guide shell directly over the quartz crucible (17-1), be sleeved on the plumbago crucible (17-2) in quartz crucible (17-1) outside and be laid in the graphite thermal field system under the plumbago crucible (17-2); Said graphite thermal field system and power cabinet (10) are gone up set terminals and are joined; It is characterized in that: also comprise the quartz tube (17-3) that lies in a horizontal plane in quartz crucible (17-1) middle inside, said quartz tube (17-3) is that the cylindrical barrel of equal opening up and down and the wall thickness of said cylindrical barrel are 3mm~10mm, and the external diameter of said quartz tube (17-3) is 1/2~1/3 of its quartz crucible of living in (17-1) internal diameter; Said quartz tube (17-3) is coaxial laying with quartz crucible (17-1), and the overhead height of quartz tube (17-3) is not higher than the overhead height of quartz crucible (17-1); Said quartz tube (17-3) bottom along the circumferential direction has and is used for a plurality of through holes that quartz crucible (17-1) inner chamber is communicated with quartz tube (17-3) inner chamber, and the structure of a plurality of said through holes and a plurality of said through holes all identical with size are even laying.
2. according to the conforming device of the described a kind of raising silicon single crystal longitudinal resistivity of claim 1; It is characterized in that: the top flush of the top of said quartz tube (17-3) and quartz crucible (17-1), perhaps the overhead height of quartz tube (17-3) is than the low 2cm~3cm of overhead height of quartz crucible (17-1).
3. according to claim 1 or the conforming device of 2 described a kind of raising silicon single crystal longitudinal resistivities, it is characterized in that: the cross-sectional area of said through hole is 6mm2~40mm2, and the cross-sectional area of said through hole is big more, and the quantity in the hole of opening is few more.
4. according to the conforming device of the described a kind of raising silicon single crystal longitudinal resistivity of claim 3, it is characterized in that: the quantity of said through hole is 6~2.
5. according to the conforming device of the described a kind of raising silicon single crystal longitudinal resistivity of claim 4, it is characterized in that: said through hole is for opening in quartz tube (17-3) bottom sides along last groove.
6. according to the conforming device of the described a kind of raising silicon single crystal longitudinal resistivity of claim 5, it is characterized in that: said groove is that diameter is the semi-circular groove (20) of 2mm~5mm.
7. according to the conforming device of the described a kind of raising silicon single crystal longitudinal resistivity of claim 4, it is characterized in that: the quantity of said through hole is 3.
8. according to claim 1 or the conforming device of 2 described a kind of raising silicon single crystal longitudinal resistivities, it is characterized in that: the wall thickness of said cylindrical barrel is 5mm~10mm.
CN201120247524U 2011-07-14 2011-07-14 Device for increasing consistency of longitudinal resistivity of mono-crystal silicon Expired - Lifetime CN202144523U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102260900A (en) * 2011-07-14 2011-11-30 西安华晶电子技术股份有限公司 Device for improving consistency of longitudinal resistivity of single crystal silicon and treatment process thereof
CN109374685A (en) * 2018-11-23 2019-02-22 遵义市精科信检测有限公司 The quality inspection method of polycrystal silicon ingot
CN109576779A (en) * 2019-02-18 2019-04-05 衢州晶哲电子材料有限公司 A kind of production technology and its production equipment improving heavy Sb-admixed silicon monocrystal oxygen content
CN113832537A (en) * 2021-09-30 2021-12-24 西安奕斯伟材料科技有限公司 Quartz crucible and crystal pulling furnace
CN115354388B (en) * 2022-08-24 2023-03-10 宇泽半导体(云南)有限公司 Silicon single crystal rod with cross-shaped cross section and growth device and growth method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102260900A (en) * 2011-07-14 2011-11-30 西安华晶电子技术股份有限公司 Device for improving consistency of longitudinal resistivity of single crystal silicon and treatment process thereof
CN102260900B (en) * 2011-07-14 2013-11-27 西安华晶电子技术股份有限公司 Device for improving consistency of longitudinal resistivity of single crystal silicon and treatment process thereof
CN109374685A (en) * 2018-11-23 2019-02-22 遵义市精科信检测有限公司 The quality inspection method of polycrystal silicon ingot
CN109576779A (en) * 2019-02-18 2019-04-05 衢州晶哲电子材料有限公司 A kind of production technology and its production equipment improving heavy Sb-admixed silicon monocrystal oxygen content
CN113832537A (en) * 2021-09-30 2021-12-24 西安奕斯伟材料科技有限公司 Quartz crucible and crystal pulling furnace
CN115354388B (en) * 2022-08-24 2023-03-10 宇泽半导体(云南)有限公司 Silicon single crystal rod with cross-shaped cross section and growth device and growth method thereof

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