CN108166053A - A kind of single crystal growing furnace secondary charging method - Google Patents
A kind of single crystal growing furnace secondary charging method Download PDFInfo
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- CN108166053A CN108166053A CN201810164387.2A CN201810164387A CN108166053A CN 108166053 A CN108166053 A CN 108166053A CN 201810164387 A CN201810164387 A CN 201810164387A CN 108166053 A CN108166053 A CN 108166053A
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- molybdenum
- secondary charging
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- quartz cone
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The invention discloses a kind of single crystal growing furnace secondary charging methods, belong to monocrystalline silicon preparation field.The secondary charging method of the present invention, includes the following steps：Step ST1, the preparation stage；Step ST2, secondary charging device positioning stage；Step ST3, crawl feeding stage；Step ST4, secondary charging device takes out the stage.The present invention mainly realizes the function of adding raw material at any time in single crystal growing furnace drawn monocrystalline silicon rod motion.
Description
Present patent application be directed to application No. is：2015109989358 divisional application, the applying date of original application
For：2015-12-25, invention and created name are：A kind of single crystal growing furnace secondary charging system.
Technical field
The present invention relates to monocrystalline silicon preparation field, more specifically to a kind of single crystal growing furnace secondary charging method.
Background technology
Single crystal growing furnace is the professional equipment for producing silicon single crystal rod.In Conventional process, polycrystalline silicon raw material is disposably packed into
It is melted in silica crucible, vertical pulling method pulling monocrystal silicon rod is used after melt.The effective mass of silicon single crystal rod is fed intake by maximum
Amount limitation, and maximum inventory is determined by the size of silica crucible, the blocky silicon material weight that silica crucible is filled, as most
Big inventory.Therefore, inventory is bigger, and silica crucible expense ratio shared in totle drilling cost is lower, so as to make what is produced
Silicon single crystal rod effective weight ratio is bigger, and this reduces costs.However, in practical operation, different operating personnel are in phase
With the maximum inventory that can reach in the silica crucible of size, there are difference.Moreover, because during melting silicon materials, it is blocky
Solid silicon becomes liquid, and the occupied space in gap is released between expecting block, cannot accomplish enough throwings so as to make disposably to feed intake
Material, reduces maximum inventory to a certain extent
Attempt to solve the above problems using secondary charging device in existing production, such as Authorization Notice No.：CN
204690162 U, authorized announcement date are on October 7th, 2015, and invention and created name is：A kind of feeding device for single crystal furnace, the Shen
Please case be related to matching the attachment used with single crystal growing furnace, the multiple feeding device of more particularly to a kind of single crystal growing furnace.The single crystal growing furnace feeds
Device includes the quartzy cylinder of both ends open, and stainless steel cylinder is arranged in the outer surface of quartzy cylinder, in quartzy cylinder lumen radially
Centre be equipped with pull rod, quartzy conehead is connected in pull rod lower end, the lower port of quartzy cylinder is stretched out in the lower part of quartzy conehead；Pull rod
The upper port of quartzy cylinder is stretched out upwards, is equipped with and the seed crystal weight connecting portion structure phase in auxiliary chamber of single crystal furnace at the top of pull rod
The connecting portion matched；It is connected limit shaft, is equipped on limit shaft axis hole several big by connecting rod on the inside of quartzy cylinder upper port
Gap hole；Limit the center location that axis hole is located at quartzy cylinder cross section；It is fixed on the outside of the upper port end face of stainless steel cylinder
Retainer ring.But in the feeding device of this application, pull rod is directly contacted with the broken silicon material in quartz tube body, is on the one hand increased
The resistance of motion of pull rod, is unfavorable for the speed of control charging, in another aspect pull rod motion process with broken silicon material CONTACT WITH FRICTION,
Metallic pollution easily is formed to broken silicon material.
For another example Authorization Notice No.：202017072 U of CN, authorized announcement date be on October 26th, 2011, invention and created name
For：Secondary charging device for single crystal furnace, this application are related to a kind of secondary charging device for single crystal furnace, it includes single crystal growing furnace, is arranged on
Silica crucible in single crystal growing furnace, the top of silica crucible is equipped with casing drum in single crystal growing furnace, and the top of casing drum is set by ring flange
It puts on fire door, casing is equipped at casing drum center, casing is connect with casing drum by sleeve support；Sunpender passes through from top to bottom
It is through at casing and leads to casing drum bottom；Boom foot is provided with and the matched tray of casing drum；The top surface of tray is taper
Face；The lifting gear of control sunpender lifting is provided at single crystal growing furnace fire door.But in the secondary charging device of this application, set
Pipe is connect with casing drum by sleeve support, and sleeve support is arranged on inside casing drum, hinder in casing drum silicon material to
Under the process that falls, be unfavorable for controlling the speed of secondary charging.
Through retrieval, also has correlation specially about the method that secondary charging is carried out using secondary charging device in the prior art
Profit is open, such as application publication number：103397389 A of CN, data of publication of application be on November 20th, 2013, invention and created name
For：The production method of monocrystal rod, this application provide a kind of production method of monocrystal rod, include the following steps：Step S10：
First silicon material is put into crucible, then heating crucible crystallizes first silicon material after fusing to melt first silicon material
To obtain first monocrystal rod, and take out first monocrystal rod；Step S20：Second batch silicon material is put into crucible, and is heated
Then crucible makes the crystallization of the second batch silicon material after fusing obtain second monocrystal rod to melt second batch silicon material.But the Shen
It please be only that the interior substantially process for putting into second batch silicon material of opposite crucible is introduced in case, how improve existing technical process
So as to which the purity for improving pulled crystal silicon rod is but not involved with.
Invention content
1. technical problems to be solved by the inivention
It is an object of the invention to overcome above-mentioned deficiency of the prior art, a kind of single crystal growing furnace secondary charging side is provided
Method mainly realizes the function of adding raw material at any time in single crystal growing furnace drawn monocrystalline silicon rod motion.
2. technical solution
In order to achieve the above objectives, technical solution provided by the invention is：
The single crystal growing furnace secondary charging system of the present invention, including monocrystalline furnace main body and secondary charging device, the single crystal growing furnace master
Body includes furnace tube, isolation cabin and concubine, and the top of the furnace tube is furnace tube neck mouth, which passes through isolation cabin and top
Concubine is connected, and isolating valve is equipped at furnace tube neck mouth；Be equipped with silica crucible in furnace tube, the bottom of silica crucible with lifting and
The support portion of spinfunction is connected, and silica crucible is surrounded by heater, and the top of silica crucible is equipped with guide shell, the water conservancy diversion
Cylinder is a cylinder that diameter reduces gradually from top to bottom；The top of furnace tube is equipped with air inlet, and the lower part of furnace tube is symmetrically arranged with
Two exhaust outlets, two exhaust outlets are connected with vacuum pump；
The secondary charging device includes molybdenum casing drum, stainless steel sleeve, molybdenum connecting rod and quartz cone, the molybdenum system and adds
The upper and lower side of barrel is open setting, and the upper end of the stainless steel sleeve is respectively equipped with the extended segment extended to both sides, above-mentioned to prolong
It stretches section and is placed in the upper end of molybdenum casing drum so that stainless steel sleeve bylinder is located at the inner hub location of molybdenum casing drum；The quartz
The shape of cone is positive triangular pyramid, the through hole from top-to-bottom is equipped in quartz cone, and the bottom of quartz cone is equipped with positive trigone
The groove of cone；The molybdenum small end passes through the inside of stainless steel sleeve and is connect with secondary indoor seed crystal rope, molybdenum connecting rod
Lower end side be equipped with screw thread, the lower end of molybdenum connecting rod passes through the through hole in quartz cone, and the lower thread of molybdenum connecting rod connects
It connects there are two molybdenum nut, and two molybdenum nuts are located at the upper and lower both sides of quartz cone respectively；
The upper side of the molybdenum casing drum is equipped with outward flange, and the inner wall of the furnace tube neck mouth is equipped with equidistantly distributed
Block, the circular open diameter that the block of above-mentioned equidistantly distributed surrounds is more than the outer diameter of molybdenum casing drum, and less than outer method
Blue outer diameter；The side of the quartz cone and the angle of bottom surface are α, its side of the groove of positive triangular pyramid that quartz cone bottom is equipped with
Angle with bottom surface is β, and β is 5 ° smaller than α.
As further improvement of the present invention, the one end of the extended segment far from stainless steel sleeve upper end is equipped with downward
Flange.
As further improvement of the present invention, the α is 45~60 °.
As further improvement of the present invention, top of its bottom of molybdenum nut away from quartz cone of the quartz cone upside
1~2mm, quartzy its bottom of molybdenum nut for boring downside 3~4mm away from the bottom of molybdenum connecting rod；The groove of above-mentioned positive triangular pyramid its
Highly it is more than 5mm.
The secondary charging method carried out using above-mentioned single crystal growing furnace secondary charging system of the present invention, is included the following steps,
Step ST1, the preparation stage；
Step ST2, secondary charging device positioning stage；
Step ST3, crawl feeding stage；
Step ST4, secondary charging device takes out the stage.
As further improvement of the present invention, in step ST1, using absolute ethyl alcohol wiping charging car, molybdenum casing drum,
Stainless steel sleeve, molybdenum connecting rod and quartz cone；
Secondary charging device is assembled, wherein, the molybdenum nut for first passing through the upper and lower both sides of quartz cone presss from both sides quartz cone
Tightly on molybdenum connecting rod, then loosen quartz cone downside molybdenum nut so that quartz cone downside its bottom of molybdenum nut away from
3~4mm of bottom of molybdenum connecting rod loosens the molybdenum nut of quartz cone upside so that its bottom of molybdenum nut of quartz cone upside
1~2mm of top away from quartz cone；
It after secondary charging device is completed, places it on charging car, carries out charging action；Wherein, molybdenum system feeds
Raw material layer one, raw material layer two, raw material layer three and raw material layer four are sequentially arranged in cylinder from bottom to top, installs raw material layer additional for the moment, first will
Raw material is put down along molybdenum casing drum inner wall, when quartz cone top is completely covered in raw material, then carries out batch turning operation；In raw material layer two
Doped resistor rate is the monocrystalline silicon piece of 0.001~0.003 Ω cm.
As further improvement of the present invention, in step ST2, the liquid level in silica crucible is looked first at, when finding stone
When the length of unfused raw material is the 1/3~1/4 of silica crucible internal diameter on liquid level in English crucible, just carries out secondary charging and move
Make；
Silica crucible is dropped into extreme lower position and the silica crucible that stops rotating by support portion, by the power tune of heater
To 60~62Kw, molybdenum small end with seed crystal rope is connect in the case where isolating valve is closed, is added by seed crystal rope by secondary
Material device is carried to concubine；
Secondary charging device is declined in two times：Isolating valve is opened, is declined first with the speed of 800~850mm/h
Secondary charging device until molybdenum casing drum lower end is located at same level with guide shell upper end, stops 5min；Then with 800
The speed of~1000mm/h declines secondary charging device so that molybdenum casing drum lower end passes through furnace tube neck mouth until molybdenum casing drum
The outward flange of upper side is blocked by the block on furnace tube neck mouth inner wall, and secondary charging device is positioned.
As further improvement of the present invention, in step ST3, crawl feeding operation is carried out：By seed crystal rope to quartz
The multiple descending operation of coning row, raw material in molybdenum casing drum from quartz cone decline after gap at drop down onto in silica crucible；Its
In, the range that quartz cone declines every time is 60~70mm, and the time that quartz bores each descending operation is 2~3s；In quartz
During cone declines, at least ensure that quartz cone bottom keeps the distance of 30mm with the liquid level in silica crucible, otherwise stop immediately
Quartz cone lowering action；
During crawl feeding operation, when unfused raw material on the liquid level found in silica crucible and guide shell lower end
Distance be 5~10mm when, immediately stop crawl feeding operation, be then lifted out secondary charging device so that molybdenum casing drum lower end with
Guide shell upper end is located at same level, stops cooling secondary charging device；
The power of heater is adjusted to 70~72Kw, observes the liquid level in silica crucible, when in discovery silica crucible again
Liquid level on the length of unfused raw material when being the 1/3~1/4 of silica crucible internal diameter, declined with the speed of 800~1000mm/h
Secondary charging device so that secondary charging device is positioned again, and the power of heater is adjusted to 60~62Kw, is repeated crawl and is added
Material operation, it is reciprocal with this, until the raw material in molybdenum casing drum adds；
In entire step ST3, the air inlet on furnace tube top is passed through inert gas, and inert gas reaches stone along guide shell
In English crucible, finally discharged entrainment of the impurity in furnace tube from exhaust outlet.
As further improvement of the present invention, in step ST4, after the raw material in molybdenum casing drum adds, two are promoted
Secondary feeding device causes molybdenum casing drum lower end to be located at same level with guide shell upper end, stops 15~16min；
It continues to lift up secondary charging device to reach in concubine, stops 20~22min；
Isolating valve is closed, secondary charging device out of concubine is taken out, is placed on charging car, the bottom of secondary charging device
Portion is isolated with the contact portion of charging car using heat-insulating material, and the heat-insulating material is polytetrafluoroethylene (PTFE) pad or high temperature hand
Set.
As further improvement of the present invention, polycrystalline silicon raw material of the raw material layer one for 3~25mm of grain size, raw material layer
Two be the polycrystalline silicon raw material of 25~45mm of grain size, and raw material layer three is the polycrystalline silicon raw material of 45~60mm of grain size, and raw material layer four is grain
The polycrystalline silicon raw material of 3~25mm of diameter.
3. advantageous effect
Using technical solution provided by the invention, compared with prior art, there is following remarkable result：
(1) single crystal growing furnace secondary charging system using the present invention feeds, can not be by silica crucible maximum inventory
Limitation, add in polycrystalline silicon raw material in two times or repeatedly, the opposite effective mass for improving silicon single crystal rod improves silica crucible
Utilization rate, thereby reduce the production cost of silicon single crystal rod；By the single crystal growing furnace secondary charging system of the present invention, as long as finding
Insufficient raw material after being dissolved in silica crucible, you can open concubine addition raw material, realize in single crystal growing furnace pulling monocrystal silicon rod mistake
The purpose of raw material is added in journey at any time.
(2) angle of quartz cone side and bottom surface in the present invention is designed as to 45~60 ° of larger angle, is comparatively made
The gap smaller occurred after quartzy cone declines is obtained, raw material can only pass through from above-mentioned gap bit by bit, be conducive to control two
The speed of secondary charging avoids accident caused by disposable overcharge.
(3) in the present invention, be equipped with the groove of positive triangular pyramid in the bottom of quartz cone, and positive its side of the groove of triangular pyramid with
The angle of bottom surface is 5 ° smaller than α, and inventor summarizes by multiple field experiment and finds, the said structure design of positive triangular pyramid groove
Can effectively disperse, discharge quartz cone it is heated after generate thermal stress, reducing quartz cone leads to what rupture event occurred when heated
Probability.
(4) inventor had found by the execute-in-place record of nearly 1 year, after crawl feeding operation, because of disposable charging
Incidence that is excessive and causing accident reduces nearly 80% compared to the feeding operation of conventional, therefore, in strict accordance with crawl plus
The requirement of material operation performs, and can save a large number of production cost every year.
Description of the drawings
Fig. 1 is the structure diagram of secondary charging device in the present invention；
Fig. 2 is the structure diagram of molybdenum casing drum in the present invention；
Fig. 3 is the structure diagram of stainless steel sleeve in the present invention；
Fig. 4 is the structure diagram of molybdenum connecting rod in the present invention；
Fig. 5 is the structure diagram of quartz cone in the present invention；
Fig. 6 is the distribution schematic diagram of raw material in secondary charging device in the present invention；
Fig. 7 is put into secondary indoor structure diagram for secondary charging device in the present invention；
Fig. 8 is that secondary charging device is placed in the structure diagram on block in the present invention；
Fig. 9 is the structure diagram that secondary charging device carries out crawl feeding operation in the present invention；
Figure 10 is the flow chart of the secondary charging method of the present invention.
Label declaration in attached drawing：1st, molybdenum casing drum；101st, outward flange；2nd, stainless steel sleeve；201st, extended segment；202、
Flange；3rd, molybdenum connecting rod；301st, molybdenum nut；4th, quartz cone；401st, through hole；C1, raw material layer one；C2, raw material layer two；C3、
Raw material layer three；C4, raw material layer four；5th, seed crystal rope；6th, concubine；7th, isolation cabin；8th, isolating valve；9th, furnace tube neck mouth；10th, block；11、
Furnace tube；12nd, silica crucible；13rd, heater；14th, support portion；15th, exhaust outlet；16th, guide shell.
Specific embodiment
To further appreciate that present disclosure, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.
Embodiment 1
With reference to Fig. 1~5, the single crystal growing furnace secondary charging system of the present embodiment, including monocrystalline furnace main body and secondary charging device,
Monocrystalline furnace main body includes furnace tube 11, isolation cabin 7 and concubine 6, and the top of furnace tube 11 is furnace tube neck mouth 9, the furnace tube neck mouth 9 by every
It is connected from storehouse 7 with the concubine 6 of top, isolating valve 8 is equipped at furnace tube neck mouth 9；Silica crucible 12, quartzy earthenware are equipped in furnace tube 11
The bottom of crucible 12 is connected with the support portion 14 with lifting and spinfunction, and silica crucible 12 is surrounded by heater 13, stone
The top of English crucible 12 is equipped with guide shell 16, which is a cylinder that diameter reduces gradually from top to bottom；Furnace tube 11
Top be equipped with air inlet, the lower part of furnace tube 11 is symmetrical arranged there are two exhaust outlet 15, and two exhaust outlets 15 are and vacuum pump
It is connected.
Secondary charging device includes molybdenum casing drum 1, stainless steel sleeve 2, molybdenum connecting rod 3 and quartz cone 4, molybdenum casing drum
1 upper and lower side is open setting, and the upper end of stainless steel sleeve 2 is respectively equipped with the extended segment 201 extended to both sides, above-mentioned extended segment
201 are placed in the upper end of molybdenum casing drum 1 so that stainless steel sleeve 2 is erected at the inner hub location of molybdenum casing drum 1；Extended segment
201 one end far from 2 upper end of stainless steel sleeve are equipped with downward flange 202, and flange 202 is used to limit extended segment 201 along its
Movement on length direction plays position-limiting action, it is ensured that stainless steel sleeve 2 is erected at molybdenum casing drum 1 to stainless steel sleeve 2
Near inner hub location, with the stability that secondary charging device is maintained integrally to be hung.The shape of quartz cone 4 is positive trigone
Cone, the 4 interior through hole 401 being equipped with from top-to-bottom of quartz cone, and the bottom of quartz cone 4 is equipped with the groove of positive triangular pyramid.Molybdenum
3 upper end of connecting rod processed passes through the inside of stainless steel sleeve 2 and is connect with the seed crystal rope 5 in concubine 6, and molybdenum connecting rod 3 is enclosed in stainless
Inside steel bushing 2, avoid molybdenum connecting rod 3 and be in direct contact with raw material in molybdenum casing drum 1, greatly reduce molybdenum connecting rod 3
The resistance of motion, be conducive to control secondary charging speed, avoid because in 3 motion process of molybdenum connecting rod with molybdenum casing drum 1
Interior raw material CONTACT WITH FRICTION and to raw material formed metallic pollution situation.
The lower end side of molybdenum connecting rod 3 is equipped with screw thread, and the lower end of molybdenum connecting rod 3 passes through the through hole in quartz cone 4
401, the lower thread connection of molybdenum connecting rod 3 is there are two molybdenum nut 301, and two molybdenum nuts 301 are located at quartz cone 4 respectively
Upper and lower both sides；Top 1~2mm of its bottom of molybdenum nut 301 away from quartz cone 4 of 4 upside of quartz cone (takes in the present embodiment
1mm), quartz cone 4 downside its bottom of molybdenum nut 301 away from the bottom of molybdenum connecting rod 3 3~4mm (3mm is taken in the present embodiment)；
Its height of the groove of above-mentioned positive triangular pyramid is more than 5mm (6mm is taken in the present embodiment) so that the lower end of molybdenum connecting rod 3 is located at positive three
In the groove of pyramid, the bottom that molybdenum connecting rod 3 stretches out quartz cone 4 is avoided to be in direct contact with the liquid level in silica crucible 12, to rise
To the effect of protection molybdenum connecting rod 3.Its bottom of molybdenum nut 301 of 4 upside of quartz cone is designed as the top 1 away from quartz cone 4
~2mm, its bottom of molybdenum nut 301 of 4 downside of quartz cone are designed as 3~4mm away from the bottom of molybdenum connecting rod 3, primarily serve guarantor
The effect of shield quartz cone 4, specially：In quartz cone 4 in actual use, expanded by heating easily occurs, it will be on quartz cone 4
Its bottom of the molybdenum nut 301 of side is designed as 1~2mm of top away from quartz cone 4 so that not by molybdenum during quartz 4 expanded by heating of cone
Nut 301 processed is limited, and avoids quartz cone 4 and broken possibility is squeezed due to expanded by heating；By the molybdenum nut of 4 downside of quartz cone
301 its bottom are designed as 3~4mm away from the bottom of molybdenum connecting rod 3, ensure that the safe to use of quartz cone 4, avoid quartz cone 4
The molybdenum nut 301 of 4 downside of quartz cone directly from molybdenum connecting rod 3 is squeezed during expanded by heating and is fallen.
The upper side of molybdenum casing drum 1 is equipped with outward flange 101, and in the present embodiment, outward flange 101 is connected by adjusting screw
It is connected on the side of molybdenum casing drum 1 so that upper-lower position of the outward flange 101 on 1 side of molybdenum casing drum is adjustable, in order to adjust
The location of when section secondary charging device is positioned；The inner wall of furnace tube neck mouth 9 is equipped with the block 10 of equidistantly distributed, above-mentioned
The circular open diameter that the block 10 of equidistantly distributed surrounds is more than the outer diameter of molybdenum casing drum 1, and outer less than outward flange 101
Diameter；The side of quartz cone 4 and the angle of bottom surface are α, and α is 45~60 ° (45 ° are taken in the present embodiment), and 4 bottoms of quartz cone are equipped with
The angle of positive its side of the groove of triangular pyramid and bottom surface is β, and β 5 ° (40 ° are taken in the present embodiment) smaller than α.
The angle of quartz 4 sides of cone and bottom surface is designed as to 45~60 ° of larger angle, comparatively so that quartz cone 4
The gap smaller occurred after decline, raw material can only pass through from above-mentioned gap bit by bit, be conducive to control raw material from molybdenum system
The speed fallen in casing drum 1, the i.e. speed convenient for control secondary charging, avoid accident caused by disposable overcharge.This
In embodiment, the groove of positive triangular pyramid, and the angle of positive its side of the groove of triangular pyramid and bottom surface are equipped in the bottom of quartz cone 4
To be 5 ° smaller than α, inventor summarizes by multiple field experiment and finds, the said structure design of positive triangular pyramid groove can effectively divide
It dissipates, generate thermal stress after release quartz cone 4 is heated, reduce the probability that quartz cone 4 causes rupture event to occur when heated.
In the present embodiment, the material of molybdenum casing drum 1, molybdenum connecting rod 3 and molybdenum nut 301 is molybdenum, and the fusing point of molybdenum is high
Up to 2610 DEG C, therefore it is not easy to form metallic pollution to the preparation of monocrystalline silicon.
It is fed using the single crystal growing furnace secondary charging system of the present embodiment, it can not be by the maximum inventory of silica crucible 12
Limitation, add in polycrystalline silicon raw material in two times or repeatedly, the opposite effective mass for improving silicon single crystal rod improves silica crucible
12 utilization rate thereby reduces the production cost of silicon single crystal rod；Single crystal growing furnace secondary charging system through this embodiment, as long as
It was found that the insufficient raw material after being dissolved in silica crucible 12, you can open concubine 6 and add raw material, realize in single crystal growing furnace pulling monocrystal
The purpose of raw material is added during silicon rod at any time.
Embodiment 2
The single crystal growing furnace secondary charging system of the present embodiment, structure is substantially the same manner as Example 1, the difference is that：
Top 2mm of its bottom of molybdenum nut 301 away from quartz cone 4 of 4 upside of quartz cone, its bottom of molybdenum nut 301 of 4 downside of quartz cone
Portion 4mm away from the bottom of molybdenum connecting rod 3, the side of quartz cone 4 and the angle of bottom surface are 60 °, the positive trigone that 4 bottoms of quartz cone are equipped with
The angle of its side of the groove of cone and bottom surface is 55 °.
Embodiment 3
With reference to Fig. 6~10, a kind of single crystal growing furnace secondary charging system progress using described in embodiment 1 of the present embodiment
Secondary charging method, includes the following steps,
Step ST1, the preparation stage；
Using absolute ethyl alcohol wiping charging car, molybdenum casing drum 1, stainless steel sleeve 2, molybdenum connecting rod 3 and quartz cone 4；
Secondary charging device is assembled, wherein, the molybdenum nut 301 for first passing through 4 upper and lower both sides of quartz cone will be quartzy
Cone 4 is clamped on molybdenum connecting rod 3, then loosens the molybdenum nut 301 of 4 downside of quartz cone so that the molybdenum spiral shell of 4 downside of quartz cone
Female 301 its bottom 3~4mm (3mm is taken in the present embodiment) away from the bottom of molybdenum connecting rod 3 loosens the molybdenum nut of 4 upside of quartz cone
301 so that top 1~2mm (in the present embodiment take 1mm) of its bottom of molybdenum nut 301 away from quartz cone 4 of 4 upside of quartz cone；
It after secondary charging device is completed, places it on charging car, carries out charging action；Wherein, molybdenum system feeds
One C1 of raw material layer, four C4 of two C2 of raw material layer, three C3 of raw material layer and raw material layer are sequentially arranged in cylinder 1 from bottom to top, installs raw material layer additional
During one C1, first raw material along 1 inner wall of molybdenum casing drum is slowly put down, when quartz 4 top of cone is completely covered in raw material, then is fallen
Material operation, wherein, due to first slowly putting down the smaller raw material of grain size along 1 inner wall of molybdenum casing drum, significantly reduce raw material pair
The impact of quartz cone 4, meanwhile, batch turning operation is carried out again when quartz 4 top of cone is completely covered in raw material, further reduced quartz
The intensity that cone 4 is knocked is effectively protected quartz cone 4.Polycrystalline silicon raw materials of one C1 of raw material layer for 3~25mm of grain size, raw material
The polycrystalline silicon raw material that two C2 of layer are 25~45mm of grain size, polycrystalline silicon raw materials of three C3 of raw material layer for 45~60mm of grain size, raw material layer
Four C4 are the polycrystalline silicon raw material of 3~25mm of grain size, in order to improve the quality of the monocrystal rod of preparation in the present embodiment, especially in raw material
The monocrystalline silicon piece that doped resistor rate is 0.001~0.003 Ω cm in two C2 of layer further improves the qualification rate of product.
Step ST2, secondary charging device positioning stage；
The liquid level in silica crucible 12 is looked first at, when the length of unfused raw material on the liquid level found in silica crucible 12
For 12 internal diameter of silica crucible 1/3~1/4 when, secondary charging action is just carried out, at this point, being floated on liquid level in silica crucible 12
A certain amount of unfused raw material can effectively slow down the speed that raw material is fallen into silica crucible 12, avoid splashing the generation of material；Meanwhile
Maximum temperature is no more than 1414 DEG C (fusing points of silicon) on the liquid level in silica crucible 12 at this time, secondary charging device is played well
Protective effect.
Silica crucible 12 is dropped into extreme lower position by support portion 14 and the silica crucible 12 that stops rotating, by heater 13
Power be adjusted to 60~62Kw (60Kw is taken in the present embodiment), in the case where isolating valve 8 is closed by 3 upper end of molybdenum connecting rod and seed
5 connection of crystalline substance rope, is carried secondary charging device to concubine 6 by seed crystal rope 5；
Secondary charging device is declined in two times：Isolating valve 8 is opened, first with 800~850mm/h (the present embodiment
In take 800mm/h) speed decline secondary charging device, until 1 lower end of molybdenum casing drum and 16 upper end of guide shell are positioned at same
Horizontal plane stops 5min and is preheated；Then decline two with the speed of 800~1000mm/h (800mm/h is taken in the present embodiment)
Secondary feeding device so that 1 lower end of molybdenum casing drum passes through furnace tube neck mouth 9 until the outward flange 101 of 1 upper side of molybdenum casing drum
It is blocked by the block 10 on 9 inner wall of furnace tube neck mouth, secondary charging device is positioned.In the present embodiment, secondary charging device is divided to two
Secondary uniform descent plays the role of secondary charging device slowly to preheat, and the decrease speed of secondary charging device is too fast, then easily
Quartz cone 4 is made to occur due to anxious heat damaged, inventor has found by a large amount of practice summaries, first with the speed of 800~850mm/h
Decline secondary charging device, stop 5min and preheated, then secondary charging device, energy are declined with the speed of 800~1000mm/h
Enough effectively protection quartz cones 4 improve the service life of quartz cone 4.
Step ST3, crawl feeding stage；
Carry out crawl feeding operation：Multiple descending operations carry out quartz cone 4 by seed crystal rope 5, in molybdenum casing drum 1
Raw material is dropped down onto at the gap after 4 decline of quartz cone in silica crucible 12；Wherein, quartzy 4 ranges declined every time of boring are
60~70mm, the time of quartz 4 each descending operations of cone is 2~3s；During quartz cone 4 declines, at least ensure quartz cone 4
Bottom keeps the distance of 30mm with the liquid level in silica crucible 12, otherwise stops quartz 4 lowering actions of cone immediately；
During crawl feeding operation, when under unfused raw material and guide shell 16 on the liquid level found in silica crucible 12
When the distance at end is 5~10mm, stops crawl feeding operation immediately, be then lifted out secondary charging device so that molybdenum casing drum 1
Lower end is located at same level with 16 upper end of guide shell, stops cooling secondary charging device；
The power of heater 13 is adjusted to 70~72Kw (70Kw is taken in the present embodiment), observes the liquid in silica crucible 12
Face, when the length of unfused raw material on the liquid level found again in silica crucible 12 is the 1/3~1/4 of 12 internal diameter of silica crucible
(it should be noted that the density of unfused raw material is less than the density of melt raw material, therefore unfused raw material gathers and swims in quartz
On liquid level in crucible 12, the length of unfused raw material refers to gather the overall length for swimming in the unfused raw material on liquid level herein
Degree), secondary charging device is declined with the speed of 800~1000mm/h (800mm/h is taken in the present embodiment) so that secondary charging fills
It puts and is positioned again, the power of heater 13 is adjusted to 60~62Kw (60Kw is taken in the present embodiment), repeats crawl feeding operation,
It is reciprocal with this, until the raw material in molybdenum casing drum 1 adds；
In entire step ST3, the air inlet on 11 top of furnace tube is passed through inert gas, and inert gas is arrived along guide shell 16
Up in silica crucible 12, finally discharged entrainment of the impurity in furnace tube 11 from exhaust outlet 15.
Monocrystalline silicon is the material foundation stone of microelectric technique, and the requirement to monocrystalline silicon quality is higher and higher, wherein more crucial
An index be exactly final obtained monocrystalline silicon purity, still, find, prepared after secondary charging operates in the prior art
Monocrystalline silicon, purity is often at least than the monocrystalline silicon order of magnitude lower without secondary charging operation preparation, and reason is very
May be that some impurity are introduced in secondary charging operating process；But in actual production, in order to improve effective matter of silicon single crystal rod
Amount reduces production cost, it has to secondary or multiple charging is carried out in silicon single crystal rod production process, therefore, how in monocrystalline
Both secondary or multiple charging had been carried out in silicon rod production process, production cost has been reduced, is carried further through the improvement of existing production technology
The silicon single crystal rod purity that height is finally prepared is the technical barrier of a urgent need to resolve in the prior art.
By the purging of inert gas in the present embodiment, a small amount of impurity generated during secondary charging is taken to furnace tube 11
Outside, it is discharged therewith from exhaust outlet 15, therefore, the purging for theoretically analyzing inert gas substantially just can be by secondary charging process
A small amount of impurity of middle generation is all discharged, so the monocrystalline silicon prepared after secondary charging operates, purity with without two
Monocrystalline silicon prepared by secondary feeding operation should be not much different, and still, in production practices have been found that actual result and above-mentioned theory
Analyze it is far from each other, in actual production, the monocrystalline silicon that is prepared after secondary charging operates, purity often at least than without
The monocrystalline silicon order of magnitude lower of secondary charging operation preparation, it is such the result is that those skilled in the art is difficult to expect
, those skilled in the art always strives to find the root of huge contrast between above-mentioned theory analysis and production practices, and but one
It does not find directly.
Inventor has found by multiple field experiment, overcomes the tool during having its source in secondary charging of above-mentioned huge contrast
The adjustment of body technology parameter, it is specific as follows：In the present embodiment, quartz cone 4 decline during, at least ensure quartz cone 4 bottoms with
Liquid level in silica crucible 12 keep 30mm distance (fusing point of quartz cone 4 is 1750 DEG C, during quartz cone 4 declines, quartz
Always there is unfused raw material on liquid level in crucible 12, therefore maximum temperature is no more than 1414 DEG C on the liquid level in silica crucible 12
(fusing point of silicon), without considering quartz 4 bottoms of cone by the situation of heating fusing), otherwise stop quartz 4 lowering actions of cone immediately；
During crawl feeding operation, when unfused raw material on the liquid level found in silica crucible 12 and the distance of 16 lower end of guide shell
During for 5~10mm, stop crawl feeding operation immediately, be then lifted out secondary charging device so that 1 lower end of molybdenum casing drum is with leading
16 upper end of flow cartridge is located at same level, stops cooling secondary charging device；In the above process, rising limit is mainly done in terms of two
Fixed, first, during restriction quartz cone 4 declines every time, 4 bottoms of quartzy cone at least keep 30mm with the liquid level in silica crucible 12
Distance；Second is that during crawl feeding operation, under unfused raw material on the liquid level in silica crucible 12 and guide shell 16
The distance at end is 5~10mm as the foundation for stopping crawl feeding operation；Making the main reason for above-mentioned two aspect limits is：Stove
The air inlet on 11 tops of cylinder is passed through inert gas, and inert gas is reached in silica crucible 12 from top to bottom along guide shell 16, right
On liquid level in silica crucible 12 and the impurity on unfused raw material surface is purged, the position near the liquid level in silica crucible 12
When putting the gap deficiency between quartz cone 16 lower end of 4 bottoms or guide shell, inert gas flows can be caused obstructed or gone out
Existing air-flow movement disorder phenomenon, seriously destroys the distribution channel of inert gas script, a large amount of impurity is caused to gather and are attached to stone
On liquid level in English crucible 12, while the SiO to volatilize in polycrystalline silicon raw material fusion process fails to be blown away by inert gas in time, altogether
Pollution is formed with to the raw material in silica crucible 12, so as to reduce the purity of monocrystalline silicon finally prepared；In the prior art, often
Do not consider to remain certain between the liquid level position in silica crucible 12 and quartz cone 16 lower end of 4 bottoms or guide shell
Material is sometimes splashed in gap in order to prevent, often keeps quartz 4 bottoms of cone much smaller than 30mm's with the liquid level in silica crucible 12
Distance or in order to once plus more raw materials in addition by 16 lower end of guide shell with it is unfused on the liquid level in silica crucible 12
Raw material is in direct contact, and said circumstances can all destroy the distribution channel of inert gas script, and the distribution channel of inert gas script
Once being destroyed, impurity can just gather near liquid level of the moment in silica crucible 12, accordingly, it is emphasized that, secondary
During charging, it is necessary to always by the liquid level neighbouring position in silica crucible 12 and quartz cone 16 lower end of 4 bottoms or guide shell
Between maintain certain gap, just can guarantee that the access that inert gas flow leads to is not destroyed always, always entrainment of in furnace tube 11
Impurity discharged from exhaust outlet 15, to ensure the monocrystalline silicon prepared after secondary charging operates, purity with without secondary
Monocrystalline silicon prepared by feeding operation is not much different, and examines and finds by the purity of monocrystalline silicon to preparation, using the side of the present embodiment
Monocrystalline silicon prepared by case, monocrystalline silicon of the purity than in the prior art Jing Guo secondary charging operation preparation improve 10 times or more,
Market needs can preferably be met.
During secondary charging, the speed for how efficiently controlling secondary charging is very crucial, existing secondary charging mistake
The highest accident for being exactly disposable overcharge and causing of probability of occurrence in journey, therefore how to efficiently control secondary charging
Speed is very crucial, and rarely has public affairs in the prior art on how to efficiently control the related art scheme of secondary charging speed
It opens.In the present embodiment, multiple descending operations carry out quartz cone 4 by seed crystal rope 5, the raw material in molybdenum casing drum 1 is from quartz
Cone 4 decline after gap at drop down onto in silica crucible 12, wherein, 4 ranges that decline every time of quartz cone are 60~70mm, stone
The time that English bores 4 each descending operations is 2~3s, and no matter the operation that quartz cone 4 lifts several times forms crawl feeding operation, i.e.,
Whether the raw material in silica crucible 12 is filled it up with, every time stringent to control the time that quartz bores 4 descending operations as 2~3s, control
The range that system quartz cone 4 declines every time is 60~70mm, and aforesaid operations can efficiently control the speed of secondary charging, greatly
It is big to avoid the accident caused due to disposable overcharge during secondary charging.Inventor passes through the execute-in-place of nearly 1 year
Record is found, after crawl feeding operation, causes the incidence of accident due to disposable overcharge compared to conventional
Feeding operation reduces nearly 80%, therefore, although crawl feeding operation is not too complicated, in strict accordance with crawl feeding operation
It is required that performing, a large number of production cost can be saved every year for enterprise.
In the present embodiment, one C1 of raw material layer uses polycrystalline silicon raw material of the grain size for 3~25mm, and two C2 of raw material layer uses grain size
For the polycrystalline silicon raw material of 25~45mm, it is the polycrystalline silicon raw material of 45~60mm (with secondary charging that three C3 of raw material layer, which uses grain size,
A large amount of practical experiences of technique find that secondary charging technique has the particle size of polycrystalline silicon raw material the high requirement of comparison, grain size
Maximum must not exceed 60mm), the grain size of polycrystalline silicon raw material is in incremental point in one C1 of raw material layer, two C2 of raw material layer, three C3 of raw material layer
Cloth is conducive to control the speed of secondary charging；Specially：The grain size of polycrystalline silicon raw material is bigger, easier during secondary charging
There is a situation where get stuck (at the gap that i.e. polycrystalline silicon raw material is stuck in after quartz cone 4 declines between molybdenum casing drum 1), this implementations
In example, one C1 of raw material layer uses grain size as the polycrystalline silicon raw material of 3~25mm, effectively prevents secondary charging and blocks at the very start
The probability of material；Meanwhile the grain size of polycrystalline silicon raw material is bigger, the stroke that quartz cone 4 declines every time during crawl feeding operation
Relatively large, in favor of falling for polycrystalline silicon raw material, but the strokes that quartz cone 4 declines every time are bigger, quartz cone 4 decline after with molybdenum
Gap between casing drum 1 processed is also bigger, is comparatively also more susceptible to the situation of disposable overcharge, this implementation
In example, one C1 of raw material layer uses grain size as the polycrystalline silicon raw material of 3~25mm, effectively prevents secondary charging and occurs one at the very start
The situation of secondary property overcharge；With continuing for crawl feeding operation, operating personnel are gradually ripe to the process of crawl feeding operation
It knows, at this time in order to improve the speed of secondary charging, two C2 of raw material layer uses polysilicon of the grain size for 25~45mm in the present embodiment
Raw material, three C3 of raw material layer use polycrystalline silicon raw material of the grain size for 45~60mm.When one C1 of raw material layer, two C2 of raw material layer, raw material layer
After polycrystalline silicon raw material in three C3 all adds, 12 internal cause of silica crucible adds a large amount of polycrystalline silicon raw material, and liquid level is increased to
Close to the upper edge of silica crucible 12, the speed of secondary charging must be strictly limited at this time, it is large-sized more to avoid direct plungeing into
During crystal silicon raw material, occur splashing material or leak the situation of silicon, it is ensured that the safety of secondary charging process；In specific the present embodiment, raw material
Four C4 of layer use polycrystalline silicon raw material of the grain size for 3~25mm, and the grain size of the polycrystalline silicon raw material is minimum, are not susceptible to splash material, and easily
In the speed of control secondary charging, the probability that disposable overcharge situation occurs is greatly reduced.
Step ST4, secondary charging device takes out the stage；
After the raw material in molybdenum casing drum 1 adds, promote secondary charging device and cause 1 lower end of molybdenum casing drum and water conservancy diversion
16 upper ends of cylinder are located at same level, 15~16min (15min is taken in the present embodiment) are stopped, at this time around secondary charging device
Temperature for 1000 DEG C or so, secondary charging device is tentatively cooled down；
It continues to lift up secondary charging device to reach in concubine 6, stops 20~22min (20min is taken in the present embodiment), at this time
Temperature around secondary charging device is 400 DEG C or so, and secondary charging device is further cooled down；It is secondary in the present embodiment
Feeding device carries out tentatively cooling down successively when taking out and further cooling, avoids quartz cone 4 that breakage occurs due to chilling, protects
Quartz cone 4.
Isolating valve 8 is closed, secondary charging device out of concubine 6 is taken out, is placed on charging car, secondary charging device
Bottom is isolated with the contact portion of charging car using heat-insulating material, heat-insulating material be polytetrafluoroethylene (PTFE) pad or high temperature gloves,
The use of heat-insulating material avoids the charging car that secondary charging device is in direct contact metal material, so as to prevent quartz cone 4 because
Chilling and breakage occurs.
Embodiment 4
The secondary charging method of the present embodiment, step is substantially the same manner as Example 3, the difference is that：Step ST2
In, silica crucible 12 is dropped into extreme lower position by support portion 14 and the silica crucible 12 that stops rotating, by the work(of heater 13
Rate is adjusted to 62Kw；In step ST2, secondary charging device is declined in two times：Isolating valve 8 is opened, first with 850mm/h's
Speed declines secondary charging device, until 1 lower end of molybdenum casing drum is located at same level with 16 upper end of guide shell, stops 5min
It is preheated；Then secondary charging device is declined with the speed of 1000mm/h so that 1 lower end of molybdenum casing drum passes through furnace tube neck mouth
9 are blocked up to the outward flange 101 of 1 upper side of molybdenum casing drum by the block 10 on 9 inner wall of furnace tube neck mouth, secondary charging device
It is positioned；In step ST3, the power of heater 13 is adjusted to 72Kw, observes the liquid level in silica crucible 12, when finding stone again
When the length of unfused raw material is the 1/3~1/4 of 12 internal diameter of silica crucible on liquid level in English crucible 12, with the speed of 1000mm/h
Degree declines secondary charging device so that secondary charging device is positioned again, and the power of heater 13 is adjusted to 62Kw, repeats point
Dynamic feeding operation, it is reciprocal with this, until the raw material in molybdenum casing drum 1 adds；In step ST4, when in molybdenum casing drum 1
Raw material add after, promote secondary charging device and so that 1 lower end of molybdenum casing drum and 16 upper end of guide shell are located at same level,
16min is stopped, secondary charging device is tentatively cooled down, and is continued to lift up secondary charging device and is reached in concubine 6, stops 22min,
Secondary charging device is further cooled down.
Schematically the present invention and embodiments thereof are described above, this describes no restricted, institute in attached drawing
What is shown is also one of embodiments of the present invention, and practical structure is not limited thereto.So if common skill of this field
Art personnel are enlightened by it, without departing from the spirit of the invention, are not inventively designed and the technical solution
Similar frame mode and embodiment, are within the scope of protection of the invention.
Claims (10)
- A kind of 1. single crystal growing furnace secondary charging method, it is characterised in that：Include the following steps,Step ST1, the preparation stage；Step ST2, secondary charging device positioning stage；Step ST3, crawl feeding stage；Step ST4, secondary charging device takes out the stage.
- 2. single crystal growing furnace secondary charging method according to claim 1, it is characterised in that：It is used in step ST1 to step ST4 Single crystal growing furnace secondary charging system is operated, and the single crystal growing furnace secondary charging system includes monocrystalline furnace main body and secondary charging fills It puts, the monocrystalline furnace main body includes furnace tube (11), isolation cabin (7) and concubine (6), and the top of the furnace tube (11) is furnace tube neck mouth (9), which is connected by isolation cabin (7) with the concubine (6) of top, and isolating valve is equipped at furnace tube neck mouth (9) (8)；Silica crucible (12), the bottom of silica crucible (12) and the support portion with lifting and spinfunction are equipped in furnace tube (11) (14) it is connected, silica crucible (12) is surrounded by heater (13), and the top of silica crucible (12) is equipped with guide shell (16), should Guide shell (16) is a cylinder that diameter reduces gradually from top to bottom；The top of furnace tube (11) is equipped with air inlet, furnace tube (11) Lower part be symmetrical arranged there are two exhaust outlet (15), which is connected with vacuum pump；The secondary charging device includes molybdenum casing drum (1), stainless steel sleeve (2), molybdenum connecting rod (3) and quartz cone (4), institute The upper and lower side for stating molybdenum casing drum (1) is open setting, and the upper end of the stainless steel sleeve (2) is respectively equipped with what is extended to both sides Extended segment (201), above-mentioned extended segment (201) is placed in the upper end of molybdenum casing drum (1) so that stainless steel sleeve (2) is erected at molybdenum system The inner hub location of casing drum (1)；The shape of the quartz cone (4) be equipped with for positive triangular pyramid, in quartz cone (4) from top to The through hole (401) of bottom, and the bottom of quartz cone (4) is equipped with the groove of positive triangular pyramid；Molybdenum connecting rod (3) upper end passes through The inside of stainless steel sleeve (2) is simultaneously connect with the seed crystal rope (5) in concubine (6), and the lower end side of molybdenum connecting rod (3) is equipped with spiral shell Line, the lower end of molybdenum connecting rod (3) pass through the through hole (401) in quartz cone (4), and the lower thread of molybdenum connecting rod (3) is connected with Two molybdenum nuts (301), and two molybdenum nuts (301) are located at the upper and lower both sides of quartz cone (4) respectively；The upper side of the molybdenum casing drum (1) is equipped with outward flange (101), and the inner wall of the furnace tube neck mouth (9) is equipped with etc. The block (10) of spacing distribution, the circular open diameter that the block (10) of above-mentioned equidistantly distributed surrounds are more than molybdenum casing drum (1) outer diameter, and less than the outer diameter of outward flange (101)；The side of the quartz cone (4) and the angle of bottom surface are α, quartz cone (4) its side of the groove of positive triangular pyramid and the angle of bottom surface that bottom is equipped with are β, and β is 5 ° smaller than α.
- 3. single crystal growing furnace secondary charging method according to claim 2, it is characterised in that：The extended segment (201) is not far from One end of rust steel bushing (2) upper end is equipped with downward flange (202).
- 4. single crystal growing furnace secondary charging method according to claim 2, it is characterised in that：The α is 45~60 °.
- 5. single crystal growing furnace secondary charging method according to claim 2, it is characterised in that：Molybdenum on the upside of the quartz cone (4) Its bottom of nut (301) processed away from quartz cone (4) 1~2mm of top, quartz cone (4) on the downside of molybdenum nut (301) its bottom away from 3~4mm of bottom of molybdenum connecting rod (3)；Its height of the groove of above-mentioned positive triangular pyramid is more than 5mm.
- 6. the single crystal growing furnace secondary charging method according to claim 2-5 any one, it is characterised in that：In step ST1, adopt With absolute ethyl alcohol wiping charging car, molybdenum casing drum (1), stainless steel sleeve (2), molybdenum connecting rod (3) and quartz cone (4)；Secondary charging device is assembled, wherein, the molybdenum nut (301) for first passing through the upper and lower both sides of quartz cone (4) will be quartzy Cone (4) is clamped on molybdenum connecting rod (3), then loosens the molybdenum nut (301) on the downside of quartz cone (4) so that under quartz cone (4) Bottom 3~4mm of molybdenum nut (301) its bottom of side away from molybdenum connecting rod (3) loosens the molybdenum nut on the upside of quartz cone (4) (301) so that top 1~2mm of molybdenum nut (301) its bottom away from quartz cone (4) on the upside of quartz cone (4)；It after secondary charging device is completed, places it on charging car, carries out charging action；Wherein, molybdenum casing drum (1) It is inside sequentially arranged with raw material layer one (C1), raw material layer two (C2), raw material layer three (C3) and raw material layer four (C4) from bottom to top, installs additional former During the bed of material one (C1), first raw material is put down along molybdenum casing drum (1) inner wall, when raw material is completely covered above quartz cone (4), then Carry out batch turning operation；Doped resistor rate is the monocrystalline silicon piece of 0.001~0.003 Ω cm in raw material layer two (C2).
- 7. single crystal growing furnace secondary charging method according to claim 6, it is characterised in that：In step ST2, quartz is looked first at Liquid level in crucible (12), when the length of unfused raw material on the liquid level found in silica crucible (12) is in silica crucible (12) Diameter 1/3~1/4 when, just carry out secondary charging action；Silica crucible (12) by support portion (14) is dropped into extreme lower position and the silica crucible that stops rotating (12), by heater (13) power is adjusted to 60~62Kw, in the case where isolating valve (8) is closed by molybdenum connecting rod (3) upper end and seed crystal rope (5) even It connects, is carried secondary charging device to concubine (6) by seed crystal rope (5)；Secondary charging device is declined in two times：Isolating valve (8) is opened, declines two first with the speed of 800~850mm/h Secondary feeding device until molybdenum casing drum (1) lower end is located at same level with guide shell (16) upper end, stops 5min；Then Secondary charging device is declined with the speed of 800~1000mm/h so that molybdenum casing drum (1) lower end passes through furnace tube neck mouth (9) straight Outward flange (101) to molybdenum casing drum (1) upper side is blocked by the block (10) on furnace tube neck mouth (9) inner wall, secondary to add Material device is positioned.
- 8. single crystal growing furnace secondary charging method according to claim 6, it is characterised in that：In step ST3, crawl charging is carried out Operation：Multiple descending operation carries out quartz cone (4) by seed crystal rope (5), the raw material in molybdenum casing drum (1) is bored from quartz (4) it is dropped down onto at the gap after declining in silica crucible (12)；Wherein, quartz cone (4) range that declines every time for 60~ 70mm, the time of each descending operation of quartz cone (4) is 2~3s；During quartz cone (4) declines, at least ensure quartz cone (4) bottom keeps the distance of 30mm with the liquid level in silica crucible (12), otherwise stops quartz cone (4) lowering action immediately；During crawl feeding operation, when under unfused raw material and guide shell (16) on the liquid level found in silica crucible (12) When the distance at end is 5~10mm, stops crawl feeding operation immediately, be then lifted out secondary charging device so that molybdenum casing drum (1) lower end is located at same level with guide shell (16) upper end, stops cooling secondary charging device；The power of heater (13) is adjusted to 70~72Kw, the liquid level in observation silica crucible (12), when finding quartzy earthenware again When the length of unfused raw material is the 1/3~1/4 of silica crucible (12) internal diameter on liquid level in crucible (12), with 800~1000mm/ The speed of h declines secondary charging device so that and secondary charging device is positioned again, the power of heater (13) is adjusted to 60~ 62Kw repeats crawl feeding operation, reciprocal with this, until the raw material in molybdenum casing drum (1) adds；In entire step ST3, the air inlet on furnace tube (11) top is passed through inert gas, and inert gas is arrived along guide shell (16) In up to silica crucible (12), finally discharged entrainment of the impurity in furnace tube (11) from exhaust outlet (15).
- 9. single crystal growing furnace secondary charging method according to claim 6, it is characterised in that：In step ST4, when molybdenum casing drum (1) it after the raw material in adds, promotes secondary charging device and molybdenum casing drum (1) lower end is located at together with guide shell (16) upper end One horizontal plane stops 15~16min；It continues to lift up secondary charging device to reach in concubine (6), stops 20~22min；Isolating valve (8) is closed, secondary charging device out of concubine (6) is taken out, is placed on charging car, secondary charging device Bottom is isolated with the contact portion of charging car using heat-insulating material, and the heat-insulating material is polytetrafluoroethylene (PTFE) pad or high temperature hand Set.
- 10. single crystal growing furnace secondary charging method according to claim 6, it is characterised in that：The raw material layer one (C1) is grain The polycrystalline silicon raw material of 3~25mm of diameter, raw material layer two (C2) are the polycrystalline silicon raw material of 25~45mm of grain size, and raw material layer three (C3) is grain The polycrystalline silicon raw material of 45~60mm of diameter, raw material layer four (C4) are the polycrystalline silicon raw material of 3~25mm of grain size.
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| CN106012010A (en) * | 2016-08-15 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Method and apparatus for secondary addition of doping agent |
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Also Published As
| Publication number | Publication date |
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| CN108166053B (en) | 2019-12-13 |
| CN105420806B (en) | 2018-04-03 |
| CN105420806A (en) | 2016-03-23 |
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