CN105420806A - Single crystal furnace secondary charging system and charging method thereof - Google Patents
Single crystal furnace secondary charging system and charging method thereof Download PDFInfo
- Publication number
- CN105420806A CN105420806A CN201510998935.8A CN201510998935A CN105420806A CN 105420806 A CN105420806 A CN 105420806A CN 201510998935 A CN201510998935 A CN 201510998935A CN 105420806 A CN105420806 A CN 105420806A
- Authority
- CN
- China
- Prior art keywords
- molybdenum
- secondary charging
- quartz
- raw material
- charging device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a single crystal furnace secondary charging system and a charging method thereof, which belong to the field of monocrystalline silicon preparation. The single crystal furnace secondary charging system comprises a single crystal furnace main body and a secondary charging device, the secondary charging device comprises a molybdenum charging cylinder, a stainless steel sleeve, a molybdenum connecting rod and a quartz pyramid, the stainless steel sleeve is erected on a center position in the molybdenum feeding cylinder; a shape of the quartz pyramid is an equilateral triangular pyramid, an equilateral triangular pyramid groove is arranged at bottom of the quartz pyramid; an included angle of the side surface and the bottom of the quartz pyramid is alpha, the included angle of the side surface and the bottom of the equilateral triangular pyramid groove is beta, and beta is less than alpha by 5 DEG. The secondary charging method comprises the following steps: 1) preparing; 2) positioning of the secondary charging device; 3) charging; and 4) taking the secondary charging device. The charging system mainly realizes a function for adding the raw materials at any time during a monocrystalline silicon rod drawing process by the single crystal furnace.
Description
Technical field
The present invention relates to silicon single crystal preparation field, more particularly, relate to a kind of single crystal growing furnace secondary charging system and charging process.
Background technology
Single crystal growing furnace is the professional equipment of produce single crystal silicon rod.In Conventional process, melt in disposable for polycrystalline silicon raw material loading quartz crucible, melt terminates rear employing vertical pulling method pulling monocrystal silicon rod.The virtual mass of silicon single crystal rod limits by maximum charging capacity, and maximum charging capacity is determined by the size of quartz crucible, the bulk silicon material weight that quartz crucible is filled, and is maximum charging capacity.Therefore, charging capacity is larger, and the ratio shared in total cost of quartz crucible expense is lower, thus makes the silicon single crystal rod effective weight ratio produced larger, this reduces cost.But in actually operating, there is difference in the maximum charging capacity that different operator can reach in the quartz crucible of same size.And due in silicon material melting process, blocks of solid silicon becomes liquid, the space of material shared by interblock gap is discharged, thus makes disposable feeding intake can not accomplish enough feeding intake, and decreases maximum charging capacity to a certain extent
Attempt in existing production to adopt secondary charging device to solve the problem, such as Authorization Notice No.: CN204690162U, authorized announcement date is on October 7th, 2015, invention and created name is: a kind of feeding device for single crystal furnace, this application case relates to the annex mating with single crystal growing furnace and use, particularly a kind of single crystal growing furnace repeatedly feeding device.This feeding device for single crystal furnace comprises the quartzy cylindrical shell of both ends open, at the sheathed stainless steel cylinder of the outside surface of quartzy cylindrical shell, be provided with pull bar in the centre of quartz tube intracoelomic cavity radial direction, connect quartzy conehead in pull bar lower end, the lower port of quartzy cylindrical shell is stretched out in the bottom of quartzy conehead; Pull bar protrudes upward the upper port of quartzy cylindrical shell, is provided with the connection section matched with the seed crystal weight connection section structure in auxiliary chamber of single crystal furnace at pull bar top; To be connected limit shaft by union lever inside quartzy cylindrical shell upper port, limit shaft axis hole is provided with some wide arc gap holes; Spacing axis hole is positioned at the home position of quartzy cylindrical shell cross section; Set collar is set firmly outside the upper port end face of stainless steel cylinder.But in the feeding device of this application case, pull bar directly contacts with the broken silicon material in quartzy cylindrical shell, add the resistance of motion of pull bar on the one hand, be unfavorable for controlling reinforced speed, with broken silicon material friction contact in another aspect pull bar moving process, easily metallic pollution formed to broken silicon material.
And for example Authorization Notice No.: CN202017072U, authorized announcement date is on October 26th, 2011, invention and created name is: secondary charging device for single crystal furnace, this application case relates to a kind of secondary charging device for single crystal furnace, it comprises single crystal growing furnace, the quartz crucible be arranged in single crystal growing furnace, and in single crystal growing furnace, the top of quartz crucible is provided with casing drum, and the top of casing drum is arranged on fire door by ring flange, casing drum center is provided with sleeve pipe, and sleeve pipe is connected by sleeve support with casing drum; Suspension rod leads to bottom casing drum through sleeve pipe from top to bottom; Boom foot is provided with the tray matched with casing drum; The end face of tray is conical surface; Single crystal growing furnace fire door place is provided with the lifting device controlling suspension rod lifting.But in the secondary charging device of this application case, sleeve pipe is connected by sleeve support with casing drum, sleeve support is arranged on casing drum inside, hinders the process that in casing drum, silicon material drops downwards, is unfavorable for the speed controlling secondary charging.
Through retrieval, in prior art about adopt secondary charging device carry out secondary charging method also existing Patents is open, such as application publication number: CN103397389A, Shen Qing Publication day is on November 20th, 2013, invention and created name is: the production method of single crystal rod, this application case provides a kind of production method of single crystal rod, comprise the following steps: step S10: in crucible, drop into first silicon material, heating crucible is to melt first silicon material, then make first silicon material crystallization after fusing to obtain first single crystal rod, and take out first single crystal rod; Step S20: drop into second batch silicon material in crucible, and heating crucible is to melt second batch silicon material, then makes the second batch silicon material crystallization after fusing to obtain second single crystal rod.But be only that the roughly process dropping into second batch silicon material in subtend crucible is introduced in this application case, how improve existing technological process thus the purity improving pulled crystal silicon rod does not but relate to.
Summary of the invention
1. invent the technical problem that will solve
The object of the invention is to overcome above-mentioned deficiency of the prior art, provide a kind of single crystal growing furnace secondary charging system and charging process, mainly achieve the function of adding raw material in single crystal growing furnace drawn monocrystalline silicon rod motion at any time.
2. technical scheme
For achieving the above object, technical scheme provided by the invention is:
Single crystal growing furnace secondary charging system of the present invention, comprise single crystal growing furnace main body and secondary charging device, described single crystal growing furnace main body comprises stove cylinder, isolation cabin and concubine, and the top of described stove cylinder is stove cylinder eck, this stove cylinder eck is connected with the concubine of top by isolation cabin, and stove cylinder eck place is provided with segregaion valve; Be provided with quartz crucible in stove cylinder, the bottom of quartz crucible is connected with the support portion of spinfunction with having to be elevated, and the surrounding of quartz crucible is provided with well heater, and the top of quartz crucible is provided with guide shell, and this guide shell is the cylindrical shell that gradually reduces of diameter from top to bottom; The top of stove cylinder is provided with inlet mouth, and the bottom of stove cylinder is symmetrically arranged with two venting ports, and these two venting ports are all connected with vacuum pump;
Described secondary charging device comprises molybdenum casing drum, stainless steel sleeve, molybdenum connecting rod and quartz cone, the equal opening of upper and lower ends of described molybdenum casing drum is arranged, the upper end of described stainless steel sleeve is respectively equipped with the extension extended to both sides, and the upper end that above-mentioned extension is placed in molybdenum casing drum makes stainless steel sleeve tub be located at the inner hub location of molybdenum casing drum; The shape of described quartz cone is positive triprismo, is provided with the through hole from top-to-bottom in quartz cone, and the bottom of quartz cone is provided with the groove of positive triprismo; Described molybdenum small end passes the inside of stainless steel sleeve and is connected with the seed crystal rope in concubine, the lower end side of molybdenum connecting rod is provided with screw thread, the lower end of molybdenum connecting rod is through the through hole in quartz cone, the lower end of molybdenum connecting rod has been threaded two molybdenum nuts, and two molybdenum nuts lay respectively at the upper and lower both sides of quartz cone;
The upper side of described molybdenum casing drum is provided with outward flange, and the inwall of described stove cylinder eck is provided with the block of equidistantly distribution, and the circular open diameter that the block of above-mentioned equidistant distribution surrounds is greater than the external diameter of molybdenum casing drum, and is less than the external diameter of outward flange; The described side of quartz cone and the angle of bottom surface are α, and its side of groove of positive triprismo that quartz cone bottom is provided with and the angle of bottom surface are β, and β is less than α 5 °.
As further improvement of the present invention, described extension is provided with downward flange away from one end of stainless steel sleeve upper end.
As further improvement of the present invention, described α is 45 ~ 60 °.
As further improvement of the present invention, the molybdenum nut of described quartz cone upside bottom it apart from the top 1 ~ 2mm of quartz cone, the bottom 3 ~ 4mm of the molybdenum nut of quartz cone downside distance molybdenum connecting rod bottom it; The groove of above-mentioned positive triprismo its be highly greater than 5mm.
The secondary charging method utilizing above-mentioned single crystal growing furnace secondary charging system to carry out of the present invention, comprises the steps,
Step ST1, preparatory stage;
Step ST2, secondary charging device positioning stage;
Step ST3, crawl feeding stage;
Step ST4, secondary charging device take out the stage.
As further improvement of the present invention, in step ST1, adopt dehydrated alcohol wiping coal charger, molybdenum casing drum, stainless steel sleeve, molybdenum connecting rod and quartz cone;
Secondary charging device is assembled, wherein, first by the molybdenum nut of quartz cone upper and lower both sides, quartz cone is clamped on molybdenum connecting rod, then the molybdenum nut of quartz cone downside is loosened, make the bottom 3 ~ 4mm of the molybdenum nut of quartz cone downside distance molybdenum connecting rod bottom it, loosen the molybdenum nut of quartz cone upside, make the molybdenum nut of quartz cone upside bottom it apart from the quartzy top 1 ~ 2mm bored;
After secondary charging device has been assembled, place it on coal charger, carry out charging action; Wherein, in molybdenum casing drum, raw material layer one, raw material layer two, raw material layer three and raw material layer four are housed from bottom to top successively, install raw material layer additional for the moment, first raw material is put down along molybdenum casing drum inwall, when raw material covers quartz cone top completely, then carry 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, first observe the liquid level in quartz crucible, when the length finding non-melt raw material on the liquid level in quartz crucible is 1/3 ~ 1/4 of quartz crucible internal diameter, just carry out secondary charging action;
Quartz crucible is dropped to extreme lower position by support portion and the quartz crucible that stops the rotation, the power of well heater is adjusted to 60 ~ 62Kw, when segregaion valve cuts out, molybdenum small end is connected with seed crystal rope, by seed crystal rope, secondary charging device is carried in concubine;
At twice secondary charging device is declined: open segregaion valve, first with the speed decline secondary charging device of 800 ~ 850mm/h, until molybdenum casing drum lower end and guide shell upper end are positioned at same level, stop 5min; Then with the speed decline secondary charging device of 800 ~ 1000mm/h, make molybdenum casing drum lower end through stove cylinder eck until the outward flange of molybdenum casing drum upper side is blocked by the block on stove cylinder eck inwall, secondary charging device is located.
As further improvement of the present invention, in step ST3, carry out crawl feeding operation: carry out repeatedly descending operation by seed crystal rope to quartz cone, the raw material in molybdenum casing drum drops down onto in quartz crucible from the gap after the decline of quartz cone; Wherein, each range declined of quartz cone is 60 ~ 70mm, and the time of each descending operation of quartz cone is 2 ~ 3s; In quartz cone decline process, at least ensure that quartz cone bottom and the liquid level in quartz crucible keep the distance of 30mm, otherwise stop quartz cone down maneuver immediately;
In crawl feeding operation process, when the distance finding non-melt raw material and guide shell lower end on the liquid level in quartz crucible is 5 ~ 10mm, stop crawl feeding operation immediately, then promoting secondary charging device makes molybdenum casing drum lower end and guide shell upper end be positioned at same level, stops cooling secondary charging device;
The power of well heater is adjusted to 70 ~ 72Kw, observe the liquid level in quartz crucible, when the length again finding non-melt raw material on the liquid level in quartz crucible is 1/3 ~ 1/4 of quartz crucible internal diameter, with the speed decline secondary charging device of 800 ~ 1000mm/h, secondary charging device is located again, the power of well heater is adjusted to 60 ~ 62Kw, repeat crawl feeding operation, reciprocal with this, till the raw material in molybdenum casing drum adds;
In whole step ST3, the inlet mouth on stove cylinder top passes into rare gas element, and rare gas element arrives in quartz crucible along guide shell, and the impurity be finally entrained with in stove cylinder is discharged from venting port.
As further improvement of the present invention, in step ST4, after the raw material in molybdenum casing drum adds, promote secondary charging device and make molybdenum casing drum lower end and guide shell upper end be positioned at same level, stop 15 ~ 16min;
Continuing to promote secondary charging device arrives in concubine, stops 20 ~ 22min;
Close segregaion valve, taken out in concubine by secondary charging device, be placed on coal charger, the bottom of secondary charging device and the contact part of coal charger use thermal insulation material to isolate, and described thermal insulation material is tetrafluoroethylene pad or high temperature gloves.
As further improvement of the present invention, described raw material layer one is the polycrystalline silicon raw material of particle diameter 3 ~ 25mm, raw material layer two is the polycrystalline silicon raw material of particle diameter 25 ~ 45mm, and raw material layer three is the polycrystalline silicon raw material of particle diameter 45 ~ 60mm, and raw material layer four is the polycrystalline silicon raw material of particle diameter 3 ~ 25mm.
3. beneficial effect
Adopt technical scheme provided by the invention, compared with prior art, there is following unusual effect:
(1) single crystal growing furnace secondary charging system of the present invention is adopted to feed in raw material, the maximum quantitative limitation that feeds intake of quartz crucible can not be subject to, add polycrystalline silicon raw material at twice or repeatedly, relatively improve the virtual mass of silicon single crystal rod, improve the rate of utilization of quartz crucible, and then reduce the production cost of silicon single crystal rod; By single crystal growing furnace secondary charging system of the present invention, as long as find the insufficient raw material after dissolving in quartz crucible, concubine can be opened and add raw material, achieve the object of adding raw material in single crystal growing furnace drawn monocrystalline silicon rod motion at any time.
(2) in the present invention, the angle of quartzy cone flank face and bottom surface is designed to the larger angle of 45 ~ 60 °, the gap occurred after making quartz cone decline comparatively speaking is less, raw material can only pass through bit by bit from above-mentioned gap, be conducive to the speed controlling secondary charging, avoid the accident that disposable overcharge causes.
(3) in the present invention, the groove of positive triprismo is provided with in the bottom of quartz cone, and its side of groove of positive triprismo is less than α 5 ° with the angle of bottom surface, contriver is through repeatedly field experiment summary discovery, positive triprismo groove said structure design can effectively disperse, discharge quartz cone be heated after produce thermal stresses, reduce quartz cone cause rupture event to occur because being heated probability.
(4) contriver through nearly 1 year execute-in-place record find, after adopting crawl feeding operation, the feeding operation that accidents caused incidence compares conventional because of disposable overcharge reduces nearly 80%, therefore, requirement in strict accordance with crawl feeding operation performs, and can save a large number of production cost every year.
Accompanying drawing explanation
Fig. 1 is the structural representation of secondary charging device in the present invention;
Fig. 2 is the structural representation of molybdenum casing drum in the present invention;
Fig. 3 is the structural representation of stainless steel sleeve in the present invention;
Fig. 4 is the structural representation of molybdenum connecting rod in the present invention;
Fig. 5 is the structural representation 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 the structural representation that in the present invention, secondary charging device puts into concubine;
Fig. 8 is that in the present invention, secondary charging device is placed in the structural representation on block;
Fig. 9 is the structural representation that in the present invention, secondary charging device carries out crawl feeding operation;
Figure 10 is the schema of secondary charging method of the present invention.
Label declaration in accompanying drawing: 1, molybdenum casing drum; 101, outward flange; 2, stainless steel sleeve; 201, extension; 202, flange; 3, molybdenum connecting rod; 301, molybdenum nut; 4, quartz cone; 401, through hole; C1, raw material layer one; C2, raw material layer two; C3, raw material layer three; C4, raw material layer four; 5, seed crystal rope; 6, concubine; 7, isolation cabin; 8, segregaion valve; 9, stove cylinder eck; 10, block; 11, stove cylinder; 12, quartz crucible; 13, well heater; 14, support portion; 15, venting port; 16, guide shell.
Embodiment
For understanding content of the present invention further, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.
Embodiment 1
Composition graphs 1 ~ 5, the single crystal growing furnace secondary charging system of the present embodiment, comprise single crystal growing furnace main body and secondary charging device, single crystal growing furnace main body comprises stove cylinder 11, isolation cabin 7 and concubine 6, the top of stove cylinder 11 is stove cylinder eck 9, this stove cylinder eck 9 is connected with the concubine 6 of top by isolation cabin 7, and stove cylinder eck 9 place is provided with segregaion valve 8; Quartz crucible 12 is provided with in stove cylinder 11, the bottom of quartz crucible 12 is connected with the support portion 14 of spinfunction with having to be elevated, the surrounding of quartz crucible 12 is provided with well heater 13, and the top of quartz crucible 12 is provided with guide shell 16, and this guide shell 16 is the cylindrical shell that gradually reduces of diameter from top to bottom; The top of stove cylinder 11 is provided with inlet mouth, and the bottom of stove cylinder 11 is symmetrically arranged with two venting ports 15, and these two venting ports 15 are all connected with vacuum pump.
Secondary charging device comprises molybdenum casing drum 1, stainless steel sleeve 2, molybdenum connecting rod 3 and quartz cone 4, the equal opening of upper and lower ends of molybdenum casing drum 1 is arranged, the upper end of stainless steel sleeve 2 is respectively equipped with the extension 201 extended to both sides, and the upper end that above-mentioned extension 201 is placed in molybdenum casing drum 1 makes stainless steel sleeve 2 be erected at the inner hub location of molybdenum casing drum 1; Extension 201 is provided with downward flange 202 away from one end of stainless steel sleeve 2 upper end, the movement that flange 202 is gone up along its length for limiting extension 201, position-limiting action is played to stainless steel sleeve 2, guarantee that stainless steel sleeve 2 is erected near the inner hub location of molybdenum casing drum 1, to maintain the stability that secondary charging device entirety is draped.The shape of quartz cone 4 is positive triprismo, is provided with the through hole 401 from top-to-bottom in quartz cone 4, and the bottom of quartz cone 4 is provided with the groove of positive triprismo.Molybdenum connecting rod 3 upper end is passed the inside of stainless steel sleeve 2 and is connected with the seed crystal rope 5 in concubine 6, it is inner that molybdenum connecting rod 3 is enclosed in stainless steel sleeve 2, avoid molybdenum connecting rod 3 to contact with the direct of raw material in molybdenum casing drum 1, greatly reduce the resistance of motion of molybdenum connecting rod 3, be conducive to controlling the speed of secondary charging, avoid because of in molybdenum connecting rod 3 moving process with raw material friction contact in molybdenum casing drum 1 and raw material is formed to the situation of metallic pollution.
The lower end side of molybdenum connecting rod 3 is provided with screw thread, and the lower end of molybdenum connecting rod 3 is through the through hole 401 in quartz cone 4, and the lower end of molybdenum connecting rod 3 has been threaded two molybdenum nuts 301, and two molybdenum nuts 301 lay respectively at quartzy bore 4 upper and lower both sides; Molybdenum nut 301 on the upside of quartz cone 4 bottom it apart from the top 1 ~ 2mm (getting 1mm in the present embodiment) of quartz cone 4, the bottom 3 ~ 4mm (getting 3mm in the present embodiment) of the distance molybdenum connecting rod 3 bottom it of the molybdenum nut 301 on the downside of quartz cone 4; The groove of above-mentioned positive triprismo its be highly greater than 5mm (getting 6mm in the present embodiment); the lower end of molybdenum connecting rod 3 is made to be positioned at the groove of positive triprismo; the bottom avoiding molybdenum connecting rod 3 to stretch out quartz cone 4 directly contacts with the liquid level in quartz crucible 12, to play the effect of protection molybdenum connecting rod 3.By top 1 ~ 2mm that its bottom design of molybdenum nut 301 on the upside of quartz cone 4 is apart from quartz cone 4, its bottom design of molybdenum nut 301 on the downside of quartz cone 4 is the bottom 3 ~ 4mm apart from molybdenum connecting rod 3, mainly play the effect of protection quartz cone 4, be specially: in the actual use procedure of quartz cone 4, easy generation expanded by heating, by top 1 ~ 2mm that its bottom design of molybdenum nut 301 on the upside of quartz cone 4 is apart from quartz cone 4, when making quartz cone 4 expanded by heating not limit by molybdenum nut 301, avoid quartz cone 4 because of expanded by heating squeezed broken possibility; By bottom 3 ~ 4mm that its bottom design of molybdenum nut 301 on the downside of quartz cone 4 is apart from molybdenum connecting rod 3, ensure that the use safety of quartz cone 4, when avoiding quartz cone 4 expanded by heating, the molybdenum nut 301 on the downside of quartz cone 4 is directly squeezed from molybdenum connecting rod 3.
The upper side of molybdenum casing drum 1 is provided with outward flange 101, in the present embodiment, outward flange 101 is connected to the side of molybdenum casing drum 1 by governing screw, make the upper-lower position of outward flange 101 on molybdenum casing drum 1 side adjustable, so that position residing when regulating secondary charging device to be located; The inwall of stove cylinder eck 9 is provided with the block 10 of equidistantly distribution, and the circular open diameter that the block 10 of above-mentioned equidistant distribution surrounds is greater than the external diameter of molybdenum casing drum 1, and is less than the external diameter of outward flange 101; The quartz cone side of 4 and the angle of bottom surface are α, α is 45 ~ 60 ° (getting 45 ° in the present embodiment), its side of groove of positive triprismo be provided with bottom quartz cone 4 and the angle of bottom surface are β, and β less than α 5 ° (getting 40 ° in the present embodiment).
The angle of quartz being bored 4 sides and bottom surface is designed to the larger angle of 45 ~ 60 °, the gap occurred after making quartz cone 4 decline comparatively speaking is less, raw material can only pass through bit by bit from above-mentioned gap, be conducive to the speed that control raw material drops in molybdenum casing drum 1, namely be convenient to the speed controlling secondary charging, avoid the accident that disposable overcharge causes.In the present embodiment, the groove of positive triprismo is provided with in the bottom of quartz cone 4, and its side of groove of positive triprismo is less than α 5 ° with the angle of bottom surface, contriver is through repeatedly field experiment summary discovery, positive triprismo groove said structure design can effectively disperse, discharge quartz cone 4 be heated after produce thermal stresses, reduce quartz bores 4 cause rupture event to occur because being heated probability.
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, up to 2610 DEG C, therefore not easily forms metallic pollution to the preparation of silicon single crystal.
The single crystal growing furnace secondary charging system of the present embodiment is adopted to feed in raw material, the maximum quantitative limitation that feeds intake of quartz crucible 12 can not be subject to, add polycrystalline silicon raw material at twice or repeatedly, relatively improve the virtual mass of silicon single crystal rod, improve the rate of utilization of quartz crucible 12, and then reduce the production cost of silicon single crystal rod; By the single crystal growing furnace secondary charging system of the present embodiment, as long as find the insufficient raw material after dissolving in quartz crucible 12, concubine 6 can be opened and add raw material, achieve the object of adding raw material in single crystal growing furnace drawn monocrystalline silicon rod motion at any time.
Embodiment 2
The single crystal growing furnace secondary charging system of the present embodiment, its structure is substantially the same manner as Example 1, its difference is: the molybdenum nut 301 on the upside of quartz cone 4 bores the top 2mm of 4 bottom it apart from quartz, the bottom 4mm of the distance molybdenum connecting rod 3 bottom it of the molybdenum nut 301 on the downside of quartz cone 4, the quartz cone side of 4 and the angle of bottom surface are 60 °, and its side of groove of positive triprismo be provided with bottom quartz cone 4 and the angle of bottom surface are 55 °.
Embodiment 3
Composition graphs 6 ~ 10, a kind of secondary charging method adopting the single crystal growing furnace secondary charging system described in embodiment 1 to carry out of the present embodiment, comprises the steps,
Step ST1, preparatory stage;
Adopt dehydrated alcohol wiping coal charger, molybdenum casing drum 1, stainless steel sleeve 2, molybdenum connecting rod 3 and quartz cone 4;
Secondary charging device is assembled, wherein, first by the molybdenum nut 301 of quartz cone 4 upper and lower both sides, quartz cone 4 is clamped on molybdenum connecting rod 3, then the molybdenum nut 301 on the downside of quartz cone 4 is loosened, make the bottom 3 ~ 4mm (getting 3mm in the present embodiment) of the molybdenum nut 301 distance molybdenum connecting rod 3 bottom it on the downside of quartz cone 4, loosen the molybdenum nut 301 on the upside of quartz cone 4, make the molybdenum nut 301 on the upside of quartz cone 4 bottom it apart from quartzy bore 4 top 1 ~ 2mm (getting 1mm in the present embodiment);
After secondary charging device has been assembled, place it on coal charger, carry out charging action, wherein, in molybdenum casing drum 1, raw material layer one C1 is housed from bottom to top successively, raw material layer two C2, raw material layer three C3 and raw material layer four C4, when installing raw material layer one C1 additional, first raw material is slowly put down along molybdenum casing drum 1 inwall, until raw material cover completely quartz cone 4 above time, carry out batch turning operation again, wherein, owing to first raw material less for particle diameter slowly being put down along molybdenum casing drum 1 inwall, significantly reduce the impact of raw material to quartz cone 4, simultaneously, batch turning operation is carried out again until time above raw material covers quartz cone 4 completely, reduce further the intensity that quartz cone 4 is knocked, effectively protect quartz cone 4.Raw material layer one C1 is the polycrystalline silicon raw material of particle diameter 3 ~ 25mm, raw material layer two C2 is the polycrystalline silicon raw material of particle diameter 25 ~ 45mm, raw material layer three C3 is the polycrystalline silicon raw material of particle diameter 45 ~ 60mm, raw material layer four C4 is the polycrystalline silicon raw material of particle diameter 3 ~ 25mm, in order to improve the quality of the single crystal rod of preparation in the present embodiment, in raw material layer two C2, doped resistor rate is the monocrystalline silicon piece of 0.001 ~ 0.003 Ω cm especially, further increases the qualification rate of product.
Step ST2, secondary charging device positioning stage;
First the liquid level in quartz crucible 12 is observed, when the length finding non-melt raw material on the liquid level in quartz crucible 12 is 1/3 ~ 1/4 of quartz crucible 12 internal diameter, just carry out secondary charging action, now, floating a certain amount of non-melt raw material on liquid level in quartz crucible 12, effectively can slow down raw material and fall into speed in quartz crucible 12, avoid the generation of spattering material; Meanwhile, on the liquid level now in quartz crucible 12, top temperature is no more than 1414 DEG C (fusing points of silicon), plays a good protection to secondary charging device.
Quartz crucible 12 is dropped to extreme lower position by support portion 14 and the quartz crucible 12 that stops the rotation, the power of well heater 13 is adjusted to 60 ~ 62Kw (getting 60Kw in the present embodiment), when segregaion valve 8 cuts out, molybdenum connecting rod 3 upper end is connected with seed crystal rope 5, by seed crystal rope 5, secondary charging device is carried in concubine 6;
At twice secondary charging device is declined: open segregaion valve 8, first with the speed decline secondary charging device of 800 ~ 850mm/h (getting 800mm/h in the present embodiment), until molybdenum casing drum 1 lower end and guide shell 16 upper end are positioned at same level, stop 5min and carry out preheating; Then with the speed decline secondary charging device of 800 ~ 1000mm/h (getting 800mm/h in the present embodiment), make molybdenum casing drum 1 lower end through stove cylinder eck 9 until the outward flange 101 of molybdenum casing drum 1 upper side is blocked by the block 10 on stove cylinder eck 9 inwall, secondary charging device is located.In the present embodiment; secondary charging device is uniform descent at twice; secondary charging device is played to the effect of slow preheating; the lowering speed of secondary charging device is too fast; then easily make quartz cone 4, because of anxious heat, breakage occur; contriver finds through a large amount of practice summary; first with the speed decline secondary charging device of 800 ~ 850mm/h; stop 5min and carry out preheating; again with the speed decline secondary charging device of 800 ~ 1000mm/h; effectively can protect quartz cone 4, improve the work-ing life of quartz cone 4.
Step ST3, crawl feeding stage;
Carry out crawl feeding operation: carry out repeatedly descending operation by seed crystal rope 5 to quartz cone 4, the raw material in molybdenum casing drum 1 drops down onto in quartz crucible 12 from the gap after quartz cone 4 decline; Wherein, the range that quartz cone 4 declines at every turn is 60 ~ 70mm, and the time of quartz cone 4 each descending operations is 2 ~ 3s; Bore in 4 decline processes at quartz, at least ensure the distance keeping 30mm bottom quartz cone 4 with the liquid level in quartz crucible 12, otherwise stop quartz cone 4 down maneuvers immediately;
In crawl feeding operation process, when the distance finding non-melt raw material and guide shell 16 lower end on the liquid level in quartz crucible 12 is 5 ~ 10mm, stop crawl feeding operation immediately, then promoting secondary charging device makes molybdenum casing drum 1 lower end and guide shell 16 upper end be positioned at same level, stops cooling secondary charging device;
The power of well heater 13 is adjusted to 70 ~ 72Kw (getting 70Kw in the present embodiment), observe the liquid level in quartz crucible 12, (it should be noted that when again finding that the length of non-melt raw material on the liquid level in quartz crucible 12 is 1/3 ~ 1/4 of quartz crucible 12 internal diameter, the density of non-melt raw material is less than the density of melt raw material, therefore non-melt raw material gathers on the liquid level that swims in quartz crucible 12, the length of non-melt raw material refers to the total length gathering the non-melt raw material swum on liquid level herein), with the speed decline secondary charging device of 800 ~ 1000mm/h (getting 800mm/h in the present embodiment), secondary charging device is located again, the power of well heater 13 is adjusted to 60 ~ 62Kw (getting 60Kw in the present embodiment), repeat crawl feeding operation, reciprocal with this, till raw material in molybdenum casing drum 1 adds,
In whole step ST3, the inlet mouth on stove cylinder 11 top passes into rare gas element, and rare gas element arrives in quartz crucible 12 along guide shell 16, and the impurity be finally entrained with in stove cylinder 11 is discharged from venting port 15.
Silicon single crystal is the material foundation stone of microelectronics, more and more higher to the requirement of silicon single crystal quality, a wherein more crucial index is exactly the purity finally obtaining silicon single crystal, but, find in prior art, the silicon single crystal of preparation after secondary charging operation, its purity is at least low than the silicon single crystal prepared without a secondary charging operation order of magnitude often, and its reason is likely in secondary charging operating process and introduces some impurity; But in actual production, in order to improve the virtual mass of silicon single crystal rod, reduce production cost, have in silicon single crystal rod production process, carry out secondary or repeatedly feed in raw material, therefore, how in silicon single crystal rod production process, both to have carried out secondary or repeatedly fed in raw material, having reduced production cost, being improved again the silicon single crystal rod purity of final preparation by the improvement of existing production technique, is the technical barrier that in prior art, is needed badly solution.
By the purging of rare gas element in the present embodiment, the a small amount of impurity produced in secondary charging process is taken to outside stove cylinder 11, discharge from venting port 15 thereupon, therefore, the a small amount of impurity produced in secondary charging process just can all be discharged by purging substantially that analyze rare gas element theoretically, so the silicon single crystal of preparation after secondary charging operation, its purity with operate without secondary charging the silicon single crystal prepared and should be more or less the same, but, but find in production practice actual result and above-mentioned theoretical analysis far from each other, in actual production, the silicon single crystal of preparation after secondary charging operation, its purity is at least low than the silicon single crystal prepared without a secondary charging operation order of magnitude often, such result is that those skilled in the art is difficult to expect, those skilled in the art attempts the root finding huge contrast between above-mentioned theory analysis and production practice always, but never find.
Contriver is through repeatedly field experiment discovery, overcome the adjustment of concrete technology parameter in the secondary charging process that has its source in of above-mentioned huge contrast, specific as follows: in the present embodiment, in quartz cone 4 decline processes, (quartzy fusing point of boring 4 is 1750 DEG C at least to ensure to keep with the liquid level in quartz crucible 12 bottom quartz cone 4 distance of 30mm, in quartz cone 4 decline processes, liquid level in quartz crucible 12 there is non-melt raw material all the time, therefore on the liquid level in quartz crucible 12, top temperature is no more than 1414 DEG C (fusing points of silicon), without the need to considering bottom quartz cone 4 by the situation of heat fused), otherwise stop quartz cone 4 down maneuvers immediately, in crawl feeding operation process, when the distance finding non-melt raw material and guide shell 16 lower end on the liquid level in quartz crucible 12 is 5 ~ 10mm, stop crawl feeding operation immediately, then promoting secondary charging device makes molybdenum casing drum 1 lower end and guide shell 16 upper end be positioned at same level, stops cooling secondary charging device, in said process, mainly make restriction from two aspects, one is limit in quartz cone 4 each decline processes, at least keeps the distance of 30mm bottom quartz cone 4 with the liquid level in quartz crucible 12, two is in crawl feeding operation process, and on the liquid level in quartz crucible 12, the distance of non-melt raw material and guide shell 16 lower end is that 5 ~ 10mm is as the foundation stopping crawl feeding operation, the major cause of making above-mentioned two aspects restrictions is: the inlet mouth on stove cylinder 11 top passes into rare gas element, rare gas element arrives in quartz crucible 12 from top to bottom along guide shell 16, to on the liquid level in quartz crucible 12 and the impurity on non-melt raw material surface purge, near the liquid level in quartz crucible 12 position and quartz bore bottom 4 or between guide shell 16 lower end gap deficiency time, inert gas flows can be caused obstructed or occur the disorderly phenomenon of air current flow, havoc rare gas element distribution channel originally, on the liquid level causing a large amount of impurity to gather being attached in quartz crucible 12, the SiO simultaneously volatilized in polycrystalline silicon raw material melting process fails to be blown away by rare gas element in time, jointly the raw material in quartz crucible 12 is formed and pollute, thus reduce the purity of monocrystalline silicon of final preparation, in prior art, the liquid level position in quartz crucible 12 and quartz is not often considered to bore bottom 4 or remain certain gap between guide shell 16 lower end, sometimes spatter material to prevent, often will keep the distance much smaller than 30mm bottom quartz cone 4 with the liquid level in quartz crucible 12, or in order to once add more raw material, even guide shell 16 lower end is directly contacted with non-melt raw material on the liquid level in quartz crucible 12, said circumstances all can destroy rare gas element distribution channel originally, and rare gas element distribution channel is originally once destroyed, impurity just can gather near the liquid level instantaneously in quartz crucible 12, therefore, it is emphasized that, in secondary charging process, must all the time position near the liquid level in quartz crucible 12 and quartz be bored bottom 4 or be maintained certain gap between guide shell 16 lower end, the path of guarantee rare gas element circulation is not destroyed always, all the time the impurity be entrained with in stove cylinder 11 is discharged from venting port 15, to guarantee the silicon single crystal of preparation after secondary charging operation, its purity with operate without secondary charging the silicon single crystal prepared and be more or less the same, through finding the purity of monocrystalline silicon inspection of preparation, adopt silicon single crystal prepared by the scheme of the present embodiment, its purity improves more than 10 times than in prior art through the silicon single crystal of secondary charging operation preparation, market demand can be met better.
In secondary charging process, the speed how effectively controlling secondary charging is very crucial, what in existing secondary charging process, probability of occurrence was the highest is exactly disposable overcharge and the accident caused, therefore the speed how effectively controlling secondary charging is very crucial, and rarely has open about the related art scheme how effectively controlling secondary charging speed in prior art.In the present embodiment, by seed crystal rope 5, repeatedly descending operation is carried out to quartz cone 4, raw material in molybdenum casing drum 1 drops down onto in quartz crucible 12 from the gap after quartz cone 4 decline, wherein, the range that quartz cone 4 declines at every turn is 60 ~ 70mm, the time of quartz cone 4 each descending operations is 2 ~ 3s, the operation that quartz cone 4 is elevated several times forms crawl feeding operation, whether the raw material namely no matter in quartz crucible 12 is filled it up with, each all strict time controlling quartz cone 4 descending operations is 2 ~ 3s, controlling each range declined of quartz cone 4 is 60 ~ 70mm, aforesaid operations can control the speed of secondary charging effectively, largely avoided the accident caused because of disposable overcharge in secondary charging process.Contriver finds through the execute-in-place record of nearly a year, after adopting crawl feeding operation, the feeding operation that accidents caused incidence compares conventional because of disposable overcharge reduces nearly 80%, therefore, although crawl feeding operation is not too complicated, but perform in strict accordance with the requirement of crawl feeding operation, concerning enterprise, a large number of production cost can be saved every year.
In the present embodiment, raw material layer one C1 adopts particle diameter to be the polycrystalline silicon raw material of 3 ~ 25mm, raw material layer two C2 adopts particle diameter to be the polycrystalline silicon raw material of 25 ~ 45mm, raw material layer three C3 adopts particle diameter to be that the polycrystalline silicon raw material of 45 ~ 60mm is (along with a large amount of practical experiences of secondary charging technique find, the size of secondary charging technique to polycrystalline silicon raw material has higher requirement, particle diameter is maximum must not more than 60mm), in raw material layer one C1, raw material layer two C2, raw material layer three C3, the particle diameter of polycrystalline silicon raw material is in increasing progressively distribution, is conducive to the speed controlling secondary charging; Be specially: the particle diameter of polycrystalline silicon raw material is larger, the situation (namely polycrystalline silicon raw material is stuck in the gap place that quartz cone 4 declines between rear and molybdenum casing drum 1) more easily got stuck in secondary charging process, in the present embodiment, raw material layer one C1 adopts particle diameter to be the polycrystalline silicon raw material of 3 ~ 25mm, effectively prevent the probability that secondary charging gets stuck at the very start; Simultaneously, the particle diameter of polycrystalline silicon raw material is larger, the stroke that in crawl feeding operation process, quartz cone 4 declines at every turn is also relatively large, be beneficial to dropping of polycrystalline silicon raw material, but the stroke that quartz cone 4 declines is larger at every turn, gap after quartz cone 4 declines and between molybdenum casing drum 1 is also larger, also more easily there is the situation of disposable overcharge comparatively speaking, in the present embodiment, raw material layer one C1 adopts particle diameter to be the polycrystalline silicon raw material of 3 ~ 25mm, effectively prevent the situation that disposable overcharge appears in secondary charging at the very start; Along with continuing of crawl feeding operation, the process of operator to crawl feeding operation is familiar with gradually, now in order to improve the speed of secondary charging, the present embodiment Central Plains bed of material two C2 adopts particle diameter to be the polycrystalline silicon raw material of 25 ~ 45mm, and raw material layer three C3 adopts particle diameter to be the polycrystalline silicon raw material of 45 ~ 60mm.After the polycrystalline silicon raw material in raw material layer one C1, raw material layer two C2, raw material layer three C3 all adds, quartz crucible 12 internal cause adds a large amount of polycrystalline silicon raw materials, its liquid level is elevated to the upper edge close to quartz crucible 12, now strictly must limit the speed of secondary charging, during to avoid directly dropping into large-sized polycrystalline silicon raw material, there is the situation of spattering material or leaking silicon, guarantee the safety of secondary charging process; In concrete the present embodiment, raw material layer four C4 adopts particle diameter to be the polycrystalline silicon raw material of 3 ~ 25mm, and the particle diameter of this polycrystalline silicon raw material is minimum, not easily spatters material, and is easy to the speed controlling secondary charging, greatly reduces the probability that disposable overcharge situation occurs.
Step ST4, secondary charging device take out the stage;
After the raw material in molybdenum casing drum 1 adds, promoting secondary charging device makes molybdenum casing drum 1 lower end and guide shell 16 upper end be positioned at same level, stop 15 ~ 16min (getting 15min in the present embodiment), temperature now around secondary charging device is about 1000 DEG C, and secondary charging device tentatively cools;
Continuing to promote secondary charging device arrives in concubine 6, and stop 20 ~ 22min (getting 20min in the present embodiment), the temperature now around secondary charging device is about 400 DEG C, and secondary charging device cools further; In the present embodiment, when secondary charging device takes out, carry out preliminary cooling and cooling further successively, avoid quartz cone 4, because of chilling, breakage occurs, protect quartz cone 4.
Close segregaion valve 8, secondary charging device is taken out in concubine 6, be placed on coal charger, the bottom of secondary charging device and the contact part of coal charger use thermal insulation material to isolate, thermal insulation material is tetrafluoroethylene pad or high temperature gloves, the use of thermal insulation material avoids the coal charger of the direct contacting metal material of secondary charging device, thus prevents quartz cone 4, because of chilling, breakage occurs.
Embodiment 4
The secondary charging method of the present embodiment, its step is substantially the same manner as Example 3, and its difference is: in step ST2, quartz crucible 12 is dropped to extreme lower position by support portion 14 and the quartz crucible 12 that stops the rotation, the power of well heater 13 is adjusted to 62Kw; In step ST2, at twice secondary charging device is declined: open segregaion valve 8, first with the speed decline secondary charging device of 850mm/h, until molybdenum casing drum 1 lower end and guide shell 16 upper end are positioned at same level, stop 5min and carry out preheating; Then with the speed decline secondary charging device of 1000mm/h, make molybdenum casing drum 1 lower end through stove cylinder eck 9 until the outward flange 101 of molybdenum casing drum 1 upper side is blocked by the block 10 on stove cylinder eck 9 inwall, secondary charging device is located; In step ST3, the power of well heater 13 is adjusted to 72Kw, observe the liquid level in quartz crucible 12, when again finding that the length of non-melt raw material on the liquid level in quartz crucible 12 is 1/3 ~ 1/4 of quartz crucible 12 internal diameter, with the speed decline secondary charging device of 1000mm/h, secondary charging device is located again, the power of well heater 13 is adjusted to 62Kw, repeat crawl feeding operation, reciprocal with this, till the raw material in molybdenum casing drum 1 adds; In step ST4, after the raw material in molybdenum casing drum 1 adds, promoting secondary charging device makes molybdenum casing drum 1 lower end and guide shell 16 upper end be positioned at same level, stop 16min, secondary charging device tentatively cools, continuing to promote secondary charging device arrives in concubine 6, and stop 22min, secondary charging device cools further.
Schematically above be described the present invention and embodiment thereof, this description does not have restricted, and also just one of the embodiments of the present invention shown in accompanying drawing, actual structure is not limited thereto.So, if those of ordinary skill in the art enlightens by it, when not departing from the invention aim, designing the frame mode similar to this technical scheme and embodiment without creationary, all should protection scope of the present invention be belonged to.
Claims (10)
1. a single crystal growing furnace secondary charging system, comprise single crystal growing furnace main body, it is characterized in that: also comprise secondary charging device, described single crystal growing furnace main body comprises stove cylinder (11), isolation cabin (7) and concubine (6), the top of described stove cylinder (11) is stove cylinder eck (9), this stove cylinder eck (9) is connected with the concubine (6) of top by isolation cabin (7), and stove cylinder eck (9) place is provided with segregaion valve (8); Quartz crucible (12) is provided with in stove cylinder (11), the bottom of quartz crucible (12) is connected with the support portion of spinfunction (14) with having to be elevated, the surrounding of quartz crucible (12) is provided with well heater (13), the top of quartz crucible (12) is provided with guide shell (16), and this guide shell (16) is the cylindrical shell that gradually reduces of diameter from top to bottom; The top of stove cylinder (11) is provided with inlet mouth, and the bottom of stove cylinder (11) is symmetrically arranged with two venting ports (15), and these two venting ports (15) are all connected with vacuum pump;
Described secondary charging device comprises molybdenum casing drum (1), stainless steel sleeve (2), molybdenum connecting rod (3) and quartz cone (4), the equal opening of upper and lower ends of described molybdenum casing drum (1) is arranged, the upper end of described stainless steel sleeve (2) is respectively equipped with the extension (201) extended to both sides, and the upper end that above-mentioned extension (201) are placed in molybdenum casing drum (1) makes stainless steel sleeve (2) be erected at the inner hub location of molybdenum casing drum (1); The shape of described quartz cone (4) is positive triprismo, is provided with the through hole (401) from top-to-bottom in quartz cone (4), and the bottom of quartz cone (4) is provided with the groove of positive triprismo; Described molybdenum connecting rod (3) upper end is passed the inside of stainless steel sleeve (2) and is connected with the seed crystal rope (5) in concubine (6), the lower end side of molybdenum connecting rod (3) is provided with screw thread, the lower end of molybdenum connecting rod (3) is through the through hole (401) in quartz cone (4), the lower end of molybdenum connecting rod (3) has been threaded two molybdenum nuts (301), and two molybdenum nuts (301) lay respectively at the upper and lower both sides of quartz cone (4);
The upper side of described molybdenum casing drum (1) is provided with outward flange (101), the inwall of described stove cylinder eck (9) is provided with the block (10) of equidistantly distribution, the circular open diameter that the block (10) of above-mentioned equidistant distribution surrounds is greater than the external diameter of molybdenum casing drum (1), and is less than the external diameter of outward flange (101); The described quartz cone side of (4) and the angle of bottom surface are α, and its side of groove of positive triprismo that quartz cone (4) bottom is provided with and the angle of bottom surface are β, and β is less than α 5 °.
2. a kind of single crystal growing furnace secondary charging system according to claim 1, is characterized in that: described extension (201) are provided with downward flange (202) away from one end of stainless steel sleeve (2) upper end.
3. a kind of single crystal growing furnace secondary charging system according to claim 1, is characterized in that: described α is 45 ~ 60 °.
4. a kind of single crystal growing furnace secondary charging system according to claim 1, it is characterized in that: the molybdenum nut (301) of described quartz cone (4) upside bottom it apart from the top 1 ~ 2mm of quartz cone (4), the bottom 3 ~ 4mm of the molybdenum nut (301) of quartz cone (4) downside distance molybdenum connecting rod (3) bottom it; The groove of above-mentioned positive triprismo its be highly greater than 5mm.
5. the secondary charging method utilizing the single crystal growing furnace secondary charging system as described in Claims 1 to 4 any one to carry out, is characterized in that: comprise the steps,
Step ST1, preparatory stage;
Step ST2, secondary charging device positioning stage;
Step ST3, crawl feeding stage;
Step ST4, secondary charging device take out the stage.
6. secondary charging method according to claim 5, it is characterized in that: in step ST1, adopt dehydrated alcohol wiping coal charger, molybdenum casing drum (1), stainless steel sleeve (2), molybdenum connecting rod (3) and quartz cone (4);
Secondary charging device is assembled, wherein, first by quartz cone (4), quartz cone (4) is clamped on molybdenum connecting rod (3) by the molybdenum nut (301) of lower both sides, then the molybdenum nut (301) of quartz cone (4) downside is loosened, make the bottom 3 ~ 4mm of molybdenum nut (301) distance molybdenum connecting rod (3) bottom it of quartz cone (4) downside, loosen the molybdenum nut (301) of quartz cone (4) upside, the molybdenum nut (301) of quartz cone (4) upside is made to bore the top 1 ~ 2mm of (4) bottom it apart from quartz,
After secondary charging device has been assembled, place it on coal charger, carry out charging action; Wherein, raw material layer one (C1), raw material layer two (C2), raw material layer three (C3) and raw material layer four (C4) are housed in molybdenum casing drum (1) from bottom to top successively, when installing raw material layer one (C1) additional, first raw material is put down along molybdenum casing drum (1) inwall, when raw material covers quartz cone (4) top completely, then carry out batch turning operation; In raw material layer two (C2), doped resistor rate is the monocrystalline silicon piece of 0.001 ~ 0.003 Ω cm.
7. secondary charging method according to claim 5, it is characterized in that: in step ST2, first the liquid level in quartz crucible (12) is observed, when the length finding non-melt raw material on the liquid level in quartz crucible (12) is 1/3 ~ 1/4 of quartz crucible (12) internal diameter, just carry out secondary charging action;
Quartz crucible (12) is dropped to extreme lower position and the quartz crucible that stops the rotation (12) by support portion (14), the power of well heater (13) is adjusted to 60 ~ 62Kw, when segregaion valve (8) cuts out, molybdenum connecting rod (3) upper end is connected with seed crystal rope (5), by seed crystal rope (5), secondary charging device is carried in concubine (6);
At twice secondary charging device is declined: open segregaion valve (8), first with the speed decline secondary charging device of 800 ~ 850mm/h, until molybdenum casing drum (1) lower end and guide shell (16) upper end are positioned at same level, stop 5min; Then with the speed decline secondary charging device of 800 ~ 1000mm/h, make molybdenum casing drum (1) lower end through stove cylinder eck (9) until the outward flange (101) of molybdenum casing drum (1) upper side is blocked by the block (10) on stove cylinder eck (9) inwall, secondary charging device is located.
8. secondary charging method according to claim 5, it is characterized in that: in step ST3, carry out crawl feeding operation: carry out repeatedly descending operation by seed crystal rope (5) to quartz cone (4), the raw material in molybdenum casing drum (1) drops down onto in quartz crucible (12) from the gap after quartz cone (4) decline; Wherein, the range that quartz cone (4) declines at every turn is 60 ~ 70mm, and the time of each descending operation of quartz cone (4) is 2 ~ 3s; In quartz cone (4) decline process, at least ensure that quartz cone (4) bottom and the liquid level in quartz crucible (12) keep the distance of 30mm, otherwise stop quartz cone (4) down maneuver immediately;
In crawl feeding operation process, when the distance finding non-melt raw material and guide shell (16) lower end on the liquid level in quartz crucible (12) is 5 ~ 10mm, stop crawl feeding operation immediately, then promoting secondary charging device makes molybdenum casing drum (1) lower end and guide shell (16) upper end be positioned at same level, stops cooling secondary charging device;
The power of well heater (13) is adjusted to 70 ~ 72Kw, observe the liquid level in quartz crucible (12), when again finding that the length of non-melt raw material on the liquid level in quartz crucible (12) is 1/3 ~ 1/4 of quartz crucible (12) internal diameter, with the speed decline secondary charging device of 800 ~ 1000mm/h, secondary charging device is located again, the power of well heater (13) is adjusted to 60 ~ 62Kw, repeat crawl feeding operation, reciprocal with this, till the raw material in molybdenum casing drum (1) adds;
In whole step ST3, the inlet mouth on stove cylinder (11) top passes into rare gas element, rare gas element arrives in quartz crucible (12) along guide shell (16), and the impurity be finally entrained with in stove cylinder (11) is discharged from venting port (15).
9. secondary charging method according to claim 5, it is characterized in that: in step ST4, after the raw material in molybdenum casing drum (1) adds, promoting secondary charging device makes molybdenum casing drum (1) lower end and guide shell (16) upper end be positioned at same level, stops 15 ~ 16min;
Continuing to promote secondary charging device arrives in concubine (6), stops 20 ~ 22min;
Close segregaion valve (8), secondary charging device is taken out in concubine (6), be placed on coal charger, the bottom of secondary charging device and the contact part of coal charger use thermal insulation material to isolate, and described thermal insulation material is tetrafluoroethylene pad or high temperature gloves.
10. secondary charging method according to claim 5, it is characterized in that: the polycrystalline silicon raw material that described raw material layer one (C1) is particle diameter 3 ~ 25mm, the polycrystalline silicon raw material that raw material layer two (C2) is particle diameter 25 ~ 45mm, the polycrystalline silicon raw material that raw material layer three (C3) is particle diameter 45 ~ 60mm, the polycrystalline silicon raw material that raw material layer four (C4) is particle diameter 3 ~ 25mm.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810164387.2A CN108166053B (en) | 2015-12-25 | 2015-12-25 | secondary feeding method for single crystal furnace |
| CN201510998935.8A CN105420806B (en) | 2015-12-25 | 2015-12-25 | A kind of single crystal growing furnace secondary charging system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510998935.8A CN105420806B (en) | 2015-12-25 | 2015-12-25 | A kind of single crystal growing furnace secondary charging system |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810164387.2A Division CN108166053B (en) | 2015-12-25 | 2015-12-25 | secondary feeding method for single crystal furnace |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105420806A true CN105420806A (en) | 2016-03-23 |
| CN105420806B CN105420806B (en) | 2018-04-03 |
Family
ID=55499331
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510998935.8A Active CN105420806B (en) | 2015-12-25 | 2015-12-25 | A kind of single crystal growing furnace secondary charging system |
| CN201810164387.2A Active CN108166053B (en) | 2015-12-25 | 2015-12-25 | secondary feeding method for single crystal furnace |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810164387.2A Active CN108166053B (en) | 2015-12-25 | 2015-12-25 | secondary feeding method for single crystal furnace |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN105420806B (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106757309A (en) * | 2016-11-11 | 2017-05-31 | 宝鸡市宏佳有色金属加工有限公司 | A kind of multiple charging mechanism of single crystal growing furnace continuous crystal-pulling |
| CN107460538A (en) * | 2017-07-19 | 2017-12-12 | 内蒙古中环光伏材料有限公司 | It is a kind of to improve the method for throwing monocrystalline silicon crystal forming rate again and the material block for launching barium carbonate |
| CN107604428A (en) * | 2017-10-18 | 2018-01-19 | 青海日晶光电有限公司 | A kind of monocrystalline silicon continuous production crystallization charging (feeding) equipment and technique |
| CN109778306A (en) * | 2019-03-25 | 2019-05-21 | 中国恩菲工程技术有限公司 | Secondary charging device for single crystal furnace |
| CN110093662A (en) * | 2019-05-23 | 2019-08-06 | 内蒙古中环光伏材料有限公司 | A kind of novel pulling of crystals throwing device and its application method again |
| CN111455452A (en) * | 2020-04-10 | 2020-07-28 | 西安奕斯伟硅片技术有限公司 | Feeding device, crystal pulling furnace and feeding method |
| CN112048763A (en) * | 2020-10-09 | 2020-12-08 | 西安奕斯伟硅片技术有限公司 | Polycrystalline silicon secondary feeding device and polycrystalline silicon ingot casting equipment |
| CN112760704A (en) * | 2020-12-28 | 2021-05-07 | 晶澳太阳能有限公司 | Boron-gallium co-doped single crystal preparation equipment and preparation method thereof |
| CN113046823A (en) * | 2021-02-07 | 2021-06-29 | 宇泽半导体(云南)有限公司 | Single crystal feeding method |
| CN113930843A (en) * | 2021-10-22 | 2022-01-14 | 中国电子科技集团公司第二十六研究所 | Method for growing crystal based on horizontal directional solidification method |
| TWI845224B (en) * | 2022-03-24 | 2024-06-11 | 中國大陸商中環領先半導體科技股份有限公司 | Feeding assembly, single crystal growth device and feeding method having the same |
| WO2024217088A1 (en) * | 2023-04-18 | 2024-10-24 | Tcl中环新能源科技股份有限公司 | Automatic refeeding method |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111717919A (en) * | 2019-03-21 | 2020-09-29 | 新疆大全新能源股份有限公司 | Manufacturing process of silicon core for polycrystalline silicon reduction furnace |
| JP7216340B2 (en) * | 2019-09-06 | 2023-02-01 | 株式会社Sumco | Method for growing silicon single crystal and apparatus for pulling silicon single crystal |
| CN115961336A (en) * | 2022-12-13 | 2023-04-14 | 西安奕斯伟材料科技有限公司 | Single crystal furnace and secondary feeding method |
| CN115976630A (en) * | 2022-12-13 | 2023-04-18 | 西安奕斯伟材料科技有限公司 | Secondary feeding system and secondary feeding method |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201089803Y (en) * | 2007-06-13 | 2008-07-23 | 浙江昱辉阳光能源有限公司 | Charge pipe for elemental crystal furnace |
| CN201261817Y (en) * | 2008-06-12 | 2009-06-24 | 新疆新能源股份有限公司 | Charging device for crystal pulling |
| CN201331263Y (en) * | 2008-12-12 | 2009-10-21 | 浙江舒奇蒙能源科技有限公司 | Mono-crystalline silicon thermal-field secondary feeding device |
| CN202017072U (en) * | 2010-11-29 | 2011-10-26 | 镇江环太硅科技有限公司 | Secondary charging device for single crystal furnace |
| CN202450183U (en) * | 2011-11-17 | 2012-09-26 | 江西旭阳雷迪高科技股份有限公司 | Secondary feeder for single crystal furnace |
| CN202671707U (en) * | 2012-05-07 | 2013-01-16 | 常州顺风光电材料有限公司 | Secondary feeding device for vertical pulling silicon monocrystal |
| CN202865390U (en) * | 2012-04-09 | 2013-04-10 | 江苏通宁新能源科技有限公司 | Secondary feeding device for silicon single crystal rod processing |
| CN202968746U (en) * | 2012-10-11 | 2013-06-05 | 特变电工新疆新能源股份有限公司 | Feeding device |
| CN203487279U (en) * | 2013-08-13 | 2014-03-19 | 上海汉虹精密机械有限公司 | Secondary charging device of quartz tube |
| CN203668558U (en) * | 2014-04-25 | 2014-06-25 | 上海合晶硅材料有限公司 | Single crystal furnace feeder and single crystal furnace including single crystal furnace feeder |
| CN204690162U (en) * | 2015-06-01 | 2015-10-07 | 山东大海新能源发展有限公司 | A kind of feeding device for single crystal furnace |
| CN204849114U (en) * | 2015-07-31 | 2015-12-09 | 包头市山晟新能源有限责任公司 | A secondary feeding ware for monocrystalline silicon is grown |
| CN205223404U (en) * | 2015-12-25 | 2016-05-11 | 安徽华芯半导体有限公司 | Single crystal growing furnace secondary feeding system |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202054922U (en) * | 2011-04-13 | 2011-11-30 | 济宁佳华电子材料有限公司 | Feeding device for single crystal furnace |
| CN202220214U (en) * | 2011-07-26 | 2012-05-16 | 青海华硅能源有限公司 | Secondary feeding device of czochralski crystal growing furnace |
| CN103215636A (en) * | 2012-01-19 | 2013-07-24 | 宁夏日晶新能源装备股份有限公司 | Mono-crystalline furnace secondary feeding funnel apparatus |
| CN202925152U (en) * | 2012-11-23 | 2013-05-08 | 万向硅峰电子股份有限公司 | Quartz feeding device of single crystal furnace |
| CN203295666U (en) * | 2013-05-15 | 2013-11-20 | 宁晋晶兴电子材料有限公司 | Second-time feeding device |
| CN203393264U (en) * | 2013-05-27 | 2014-01-15 | 开化县同欣硅业有限公司 | Charging cylinder for single crystal furnace |
| CN203546198U (en) * | 2013-10-24 | 2014-04-16 | 山东泰岱光伏科技有限公司 | Feeding device of mono-crystal furnace |
-
2015
- 2015-12-25 CN CN201510998935.8A patent/CN105420806B/en active Active
- 2015-12-25 CN CN201810164387.2A patent/CN108166053B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201089803Y (en) * | 2007-06-13 | 2008-07-23 | 浙江昱辉阳光能源有限公司 | Charge pipe for elemental crystal furnace |
| CN201261817Y (en) * | 2008-06-12 | 2009-06-24 | 新疆新能源股份有限公司 | Charging device for crystal pulling |
| CN201331263Y (en) * | 2008-12-12 | 2009-10-21 | 浙江舒奇蒙能源科技有限公司 | Mono-crystalline silicon thermal-field secondary feeding device |
| CN202017072U (en) * | 2010-11-29 | 2011-10-26 | 镇江环太硅科技有限公司 | Secondary charging device for single crystal furnace |
| CN202450183U (en) * | 2011-11-17 | 2012-09-26 | 江西旭阳雷迪高科技股份有限公司 | Secondary feeder for single crystal furnace |
| CN202865390U (en) * | 2012-04-09 | 2013-04-10 | 江苏通宁新能源科技有限公司 | Secondary feeding device for silicon single crystal rod processing |
| CN202671707U (en) * | 2012-05-07 | 2013-01-16 | 常州顺风光电材料有限公司 | Secondary feeding device for vertical pulling silicon monocrystal |
| CN202968746U (en) * | 2012-10-11 | 2013-06-05 | 特变电工新疆新能源股份有限公司 | Feeding device |
| CN203487279U (en) * | 2013-08-13 | 2014-03-19 | 上海汉虹精密机械有限公司 | Secondary charging device of quartz tube |
| CN203668558U (en) * | 2014-04-25 | 2014-06-25 | 上海合晶硅材料有限公司 | Single crystal furnace feeder and single crystal furnace including single crystal furnace feeder |
| CN204690162U (en) * | 2015-06-01 | 2015-10-07 | 山东大海新能源发展有限公司 | A kind of feeding device for single crystal furnace |
| CN204849114U (en) * | 2015-07-31 | 2015-12-09 | 包头市山晟新能源有限责任公司 | A secondary feeding ware for monocrystalline silicon is grown |
| CN205223404U (en) * | 2015-12-25 | 2016-05-11 | 安徽华芯半导体有限公司 | Single crystal growing furnace secondary feeding system |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106757309A (en) * | 2016-11-11 | 2017-05-31 | 宝鸡市宏佳有色金属加工有限公司 | A kind of multiple charging mechanism of single crystal growing furnace continuous crystal-pulling |
| CN106757309B (en) * | 2016-11-11 | 2020-01-14 | 宝鸡市宏佳有色金属加工有限公司 | Continuous crystal pulling multiple feeding mechanism of single crystal furnace |
| CN107460538A (en) * | 2017-07-19 | 2017-12-12 | 内蒙古中环光伏材料有限公司 | It is a kind of to improve the method for throwing monocrystalline silicon crystal forming rate again and the material block for launching barium carbonate |
| CN107604428A (en) * | 2017-10-18 | 2018-01-19 | 青海日晶光电有限公司 | A kind of monocrystalline silicon continuous production crystallization charging (feeding) equipment and technique |
| CN109778306A (en) * | 2019-03-25 | 2019-05-21 | 中国恩菲工程技术有限公司 | Secondary charging device for single crystal furnace |
| CN110093662A (en) * | 2019-05-23 | 2019-08-06 | 内蒙古中环光伏材料有限公司 | A kind of novel pulling of crystals throwing device and its application method again |
| CN110093662B (en) * | 2019-05-23 | 2023-10-10 | 内蒙古中环光伏材料有限公司 | Re-casting device for Czochralski single crystal and application method thereof |
| CN111455452B (en) * | 2020-04-10 | 2021-11-30 | 西安奕斯伟材料科技有限公司 | Feeding device, crystal pulling furnace and feeding method |
| CN111455452A (en) * | 2020-04-10 | 2020-07-28 | 西安奕斯伟硅片技术有限公司 | Feeding device, crystal pulling furnace and feeding method |
| CN112048763A (en) * | 2020-10-09 | 2020-12-08 | 西安奕斯伟硅片技术有限公司 | Polycrystalline silicon secondary feeding device and polycrystalline silicon ingot casting equipment |
| CN112048763B (en) * | 2020-10-09 | 2022-07-12 | 西安奕斯伟材料科技有限公司 | Polycrystalline silicon secondary feeding device and polycrystalline silicon ingot casting equipment |
| CN112760704A (en) * | 2020-12-28 | 2021-05-07 | 晶澳太阳能有限公司 | Boron-gallium co-doped single crystal preparation equipment and preparation method thereof |
| CN113046823A (en) * | 2021-02-07 | 2021-06-29 | 宇泽半导体(云南)有限公司 | Single crystal feeding method |
| CN113046823B (en) * | 2021-02-07 | 2023-10-17 | 宇泽半导体(云南)有限公司 | Single crystal feeding method |
| CN113930843A (en) * | 2021-10-22 | 2022-01-14 | 中国电子科技集团公司第二十六研究所 | Method for growing crystal based on horizontal directional solidification method |
| TWI845224B (en) * | 2022-03-24 | 2024-06-11 | 中國大陸商中環領先半導體科技股份有限公司 | Feeding assembly, single crystal growth device and feeding method having the same |
| WO2024217088A1 (en) * | 2023-04-18 | 2024-10-24 | Tcl中环新能源科技股份有限公司 | Automatic refeeding method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108166053A (en) | 2018-06-15 |
| CN105420806B (en) | 2018-04-03 |
| CN108166053B (en) | 2019-12-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105420806A (en) | Single crystal furnace secondary charging system and charging method thereof | |
| JP4959456B2 (en) | Apparatus and method for supplying solid raw material to single crystal growth apparatus | |
| JP5413354B2 (en) | Silicon single crystal pulling apparatus and silicon single crystal manufacturing method | |
| CN102418140A (en) | Czochralski silicon monocrystal growth furnace and method for filling silicon melts continuously | |
| CN202380122U (en) | Straight-pull silicon single crystal growth furnace continuously filled with silicon melt | |
| WO2001057293A1 (en) | Single crystal growing device and production method of single crystal using the device and single crystal | |
| CN103556220B (en) | Polycrystalline silicon ingot or purifying furnace | |
| KR101540225B1 (en) | Single Crystal Manufacturing Apparatus and Single Crystal Manufacturing Method | |
| CN205223404U (en) | Single crystal growing furnace secondary feeding system | |
| WO2008067700A1 (en) | Dislocation-free silicon monocrystal, its preparation method and a graphite heating device used | |
| JP2008285351A (en) | Material supply apparatus, single crystal drawing apparatus equipped with the same, and material supply method | |
| CN204690162U (en) | A kind of feeding device for single crystal furnace | |
| JP2023509531A (en) | Hot zone structure of single crystal furnace, single crystal furnace and crystal bar | |
| WO2024016879A1 (en) | Crucible melting machine and crucible melting method | |
| KR101563221B1 (en) | Single crystal manufacturing apparatus and manufacturing method | |
| JP4184725B2 (en) | Single crystal semiconductor manufacturing method and single crystal semiconductor manufacturing apparatus | |
| CN1412353A (en) | Gas flow control method of thermal field of vertical pulling silicon monocrystal furnace and its device | |
| CN112048758A (en) | Continuous Czochralski single crystal rod process | |
| WO2021128643A1 (en) | Semiconductor silicon material consumable growth furnace and preparation method for silicon material | |
| CN206721391U (en) | A kind of feeding device for single crystal furnace for possessing movable protective sleeve | |
| JP2009274928A (en) | Segmentation-type heater and apparatus and method for pulling single crystal using the same | |
| KR101528055B1 (en) | Ingot growing apparatus | |
| JP5500672B2 (en) | Quartz glass crucible manufacturing apparatus and quartz glass crucible manufacturing method | |
| US9476141B2 (en) | Weir for inhibiting melt contamination | |
| CN221371351U (en) | Single crystal furnace water cooling screen and single crystal furnace |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |