CN107460539A - A kind of monocrystalline silicon production method of heater and the application heater - Google Patents
A kind of monocrystalline silicon production method of heater and the application heater Download PDFInfo
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- CN107460539A CN107460539A CN201710527688.2A CN201710527688A CN107460539A CN 107460539 A CN107460539 A CN 107460539A CN 201710527688 A CN201710527688 A CN 201710527688A CN 107460539 A CN107460539 A CN 107460539A
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- crucible
- heater
- silicon
- heater body
- groove
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Classifications
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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
- C30B15/14—Heating of the melt or the crystallised materials
-
- 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 provides a kind of heater, including integrally formed cylindric heater body, the heater body is enclosed by connection sheet alternating series connection by multiple long heating plates and multiple short heating plates and formed, the long heating plate is wide with the short heating plate and top is concordant sets, each formed with gap between long heating plate and its adjacent short heating plate, at the top of each long heating plate radially one first groove is offered along heater body, one second groove radially is offered along heater body at the top of each short heating plate, the first groove groove depth is more than the second groove groove depth.Heater of the present invention reduces the reaction of bottom and side lower part during crystal pulling, and then realizes the reduction of oxygen content, meanwhile, by adjusting crucible and heater relative position, avoid melting silicon materials from occurring crystallizing risk again early stage.
Description
Technical field
The invention belongs to monocrystalline silicon production field, more particularly, to the monocrystalline silicon life of a kind of heater and the application heater
Production method.
Background technology
Monocrystalline silicon is the important raw and processed materials of crystal silicon battery, photovoltaic market fast development in recent years, competes and is also growing more intense；For
The technology such as photoelectric transformation efficiency, IBC, HIT, PERC for improving crystal silicon battery starts to be applied to large-scale production；In actual production,
Monocrystalline silicon typically all can be also aerobic, and oxygen distribution is that head height tail is low, the oxygen in raw material monocrystalline silicon, can be with dopant boron element
B-O complexs are formed, cause crystal silicon battery electricity conversion to decline, can also influence the using effect of new technology, therefore reduce
Oxygen content has profound significance to photovoltaic industry in monocrystalline silicon.
There is oxygen content method in current reduction pulling of silicon single crystal：
1st, using magnetic field pulling monocrystal, i.e.,：MCZ techniques, magnetic field can suppress the thermal convection current of melt, turn to draw using low crucible
Monocrystalline, reduces the reaction speed of silica crucible and melt silicon, while magnetic field can weaken in melt oxygen to the fortune in growth boundary layer
It is dynamic, and then reduce oxygen content in monocrystalline silicon.Oxygen positive effect is dropped using magnetic field pulling monocrystal, but magnetic field means are expensive, and transport
Energy consumption is big during row, and crystal-pulling cost is higher, can not be applied to photovoltaic industry with keen competition.
2nd, by work parameter adjustment, such as：Argon flow amount, furnace pressure, crystalline substance turn crucible turn etc., can reduce oxygen content, but effect is poor,
Yield rate can receive influence；Part company, which equally changes heater structure, reduces oxygen content, but its structure is relative complex, and can not
Effectively solves the risk brought after heater structure changes.
In addition, during crystal pulling, typically can all vacuum pumping, the source of oxygen during crystal pulling be carried out to oxygen in thermal field
The bottom of the mainly reaction of melt silicon and silica crucible, especially crucible and side lower part reaction are violent, are the main next of oxygen introducing
Source,
The content of the invention
In view of this, the present invention is directed to propose a kind of heater and application the heater monocrystalline silicon production method, with solution
The quality problems caused by oxygen content height in certainly existing monocrystalline silicon production.
To reach above-mentioned purpose, the technical proposal of the invention is realized in this way：
A kind of heater, including integrally formed cylindric heater body, the heater body is by multiple long heating
Piece and multiple short heating plates, which by connection sheet replace series connection and enclosed, to be formed, and the long heating plate and the short heating plate are wide and push up
Portion is concordantly set, and the heater body top is high-temperature region, and its underpart is low-temperature space, short adjacent with its of each long heating plate
One first groove radially is offered along heater body formed with gap, each long heating plate top between heating plate, each
One second groove radially is offered along heater body at the top of short heating plate, the first groove groove depth is more than the second groove groove depth.
Further, the short heating leaf length and long heating leaf length ratio are between 1/5 to 3/4.
Further, the first groove width, the wide setting of the second groove width and gap, the width are 10-20mm.
Further, the first groove thickness of groove bottom and the second groove thickness of groove bottom are identical, and the thickness is equal to connection sheet
Highly, while the thickness=long heating plate width/2.
Relative to prior art, heater of the present invention has the advantage that：
Heater of the present invention is enclosed and formed by the alternately long heating plate of series connection and short heating plate, and upper part
Fever tablet is intensive, and caloric value is big, is high-temperature region, and lower part caloric value is few, is low-temperature space, and this construction reduces vertical side in crucible
Upward thermograde change, and then the reduction of oxygen content is realized, meanwhile, by adjusting crucible and heater relative position, avoid
Occur melting silicon materials early stages crystallizing risk again, when ensureing crystal pulling, liquid level is in high-temperature region in crucible, and power consumption can drop during such crystal pulling
It is low, lower power consumption can weaker silica crucible and melt silicon reaction, and then oxygen content can be reduced.
A kind of monocrystalline silicon production method using heater, comprise the following steps：
1), prepare：
Heater body is put in thermal field, by a certain amount of solid-state silicon raw material loaded in crucible, adjusted using lifting device
Whole crucible and heater body relative position, ensure crucible top relative to low 60-70mm at the top of heater body, now crucible
Crucible bottom is in heater body low-temperature space；
2), evacuate：
Oxygen in thermal field is drained using vacuum system, while is filled with argon gas as protective gas；
3), material：
To heater body electrified regulation, silicon material starts after there is melt silicon in crucible, passes through the lifting device in thermal field
Crucible is moved up into 45-65mm, now crucible bottom is in high-temperature region lower area；
4), collapse material：
Crucible internal solid silicon continues to melt, and when not molten silicon is all swum in silicon liquid, rise crucible is until crucible top
It is higher by the 1/5 of the short heating leaf length of heater body；
5), temperature stabilization section：
Temperature-resistant in control thermal field when silicon material melt-through is in a liquid state in crucible, lifting bushing position is up to liquid in crucible
Identity distance is from being the 3/10 of short heating leaf length with a distance from the top of heater, and now liquid level is located at high-temperature region upper area, in the temperature
The lower bushing position of degree is kept for constant 1-2 hours；
6), seeding：
Temperature of thermal field is adjusted, seeding production is carried out to silicon liquid in crucible, keeps liquid level in crucible to be in height during seeding
Warm area, and continue keep crucible in distance of the liquid level at the top of heater for it is short heating leaf length 3/10 between；
7), shouldering turns shoulder：
Shouldering is carried out to the silicon rod after seeding and turns shoulder production, shouldering turns in shoulder production, keeps liquid level distance heating in crucible
Between distance at the top of device is the 3/10 of short heating leaf length；
8) it is, isometrical：
The constant isometrical production of progress of bushing position in step 7) is kept, starts gradually to carry using lifting device after isometrical 50mm
Bushing position is risen, 2-10mm will be risen on the basis of bushing position step 7) when isometrical 200mm, ensures that liquid level is located in crucible
Aperture settings position in the production of the crystal pulling setting position of high-temperature region, i.e. crystal pulling, keeps liquid level and heater distance from top in crucible
It is constant until isometrical end；
9), finish up；
10), blowing out cools down.
Further, in step 3), including substep once：
(a), silicon material starts after there is melt silicon in crucible, and crucible is moved up into 30-40mm by the lifting device in thermal field,
Now crucible crucible bottom is in heater body high-temperature region lower area；
(b), during material, when silicon material largely melts, there is solid-state silicon in crucible bottom, continue up lifting crucible position 15-
25mm, ensure crucible bottom in the higher temperature area of high-temperature region lower area.
Further, argon gas is filled with the thermal field as protective gas.
It is of the present invention to be had the advantage that using the monocrystalline silicon production method of heater relative to prior art：
In monocrystalline silicon production method of the present invention using heater, by adjusting material, temperature stabilization section
And isometrical section crucible, liquid level ensure in silicon rod production process, by adjusting crucible and heater phase relative to heater locations
To position, melting silicon materials are avoided to occur crystallizing risk again early stage, meanwhile, when ensureing crystal pulling, liquid level is in high-temperature region in crucible, this
Power consumption can reduce during sample crystal pulling, lower power consumption can weaker silica crucible and melt silicon reaction, and then oxygen content can be reduced.
Temperature stabilization and the adjustment of isometrical process crucible position, are the characteristics (top caloric value is big) using the heater, by liquid
Face control reduces power consumption in high-temperature region, can equally realize and weaken melt silicon and the purpose of silica crucible reaction, and then drop
Low oxygen content；Crucible position can gradually be lifted during isometrical, can either ensure that head oxygen content reduces, do not influence the later stage into
It is brilliant.
Brief description of the drawings
The accompanying drawing for forming the part of the present invention is used for providing a further understanding of the present invention, schematic reality of the invention
Apply example and its illustrate to be used to explain the present invention, do not form inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 is the heater structure schematic diagram described in the embodiment of the present invention；
Fig. 2 is that the silicon rod oxygen content table of comparisons before and after the heater is applied in example monocrystalline silicon production of the present invention；
Fig. 3 is that silicon rod oxygen content compares figure before and after the heater is applied in example monocrystalline silicon production of the present invention；
Description of reference numerals：
1- heater bodies；The long heating plates of 11-；The grooves of 111- first；
The grooves of 121- second；The short heating plates of 12-；13- gaps；
14- connection sheets；2- crucibles.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
In the description of the invention, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " on ", " under ",
The orientation or position relationship of the instruction such as "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", " outer " are
Based on orientation shown in the drawings or position relationship, it is for only for ease of the description present invention and simplifies description, rather than instruction or dark
Show that the device of meaning or element there must be specific orientation, with specific azimuth configuration and operation, thus it is it is not intended that right
The limitation of the present invention.In addition, term " first ", " second " etc. are only used for describing purpose, and it is not intended that instruction or hint phase
To importance or the implicit quantity for indicating indicated technical characteristic.Thus, the feature for defining " first ", " second " etc. can
To express or implicitly include one or more this feature.In the description of the invention, unless otherwise indicated, " multiple "
It is meant that two or more.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " should be interpreted broadly, for example, it may be being fixedly connected or being detachably connected, or be integrally connected；Can
To be mechanical connection or electrical connection；Can be joined directly together, can also be indirectly connected by intermediary, Ke Yishi
The connection of two element internals.For the ordinary skill in the art, above-mentioned term can be understood by concrete condition
Concrete meaning in the present invention.
Describe the present invention in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
As shown in figure 1, a kind of heater, including integrally formed cylindric heater body 1, the heater body 1
Series connection replaced by connection sheet 14 by multiple long heating plates 11 and multiple short heating plates 12 enclose and form, the short heating plate 12 is grown
Degree and the length ratio of long heating plate 11 are between=1/5 to 3/4, the long heating plate 11 and short heating plate 12 is wide and top horizontal
Neat to set, the long bottom of heating plate 11 is protruded short heating plate 12 and set, therefore the top of heater body 1 is high-temperature region, and bottom is low
Warm area, each formed with gap 13 between long heating plate 11 and its adjacent short heating plate 12, gap width 10-20mm is each
The individual top of long heating plate 11 offers one first groove 111, and the center line of the first groove 111 and length along the radial direction of heater body 1
Heating plate 11 intersects along the axial direction center line of heater body 1, and each short top of heating plate 12 is opened along the radial direction of heater body 1
Provided with one second groove 121, and the center line of the second groove 121 and short heating plate 12 are along the axial direction center line phase of heater body 1
Hand over, the width of the first groove 111, the width of the second groove 121 are wide, and equal with the width of gap 13 respectively, the first groove 111
Groove depth is more than the groove depth of the second groove 121.
In the present embodiment, the thickness of groove bottom of the first groove 111 and the thickness of groove bottom of the second groove 121 are identical, the thickness etc.
In the height of connection sheet 14, while the thickness=width/2 of long heating plate 11, the structure ensure heter temperature uniformity.
As shown in Figure 2 and Figure 3, a kind of monocrystalline silicon production method using heater, comprises the following steps：
1), prepare：
Heater body 1 is put in thermal field, by a certain amount of solid-state silicon raw material loaded in crucible 2, utilizes lifting device
Crucible 2 and the relative position of heater body 1 are adjusted, ensures the top of crucible 2 relative to the low 60-70mm in the top of heater body 1, this
When the crucible bottom of crucible 2 in the low-temperature space of heater body 1；
2), evacuate：
Oxygen in thermal field is drained using vacuum system, while is filled with argon gas as protective gas；
3), material：
To the electrified regulation of heater body 1, silicon material starts after there is melt silicon in crucible 2, is filled by the lifting in thermal field
Put and crucible 2 is moved up into 30-40mm, now the crucible bottom of crucible 2 is in the high-temperature region lower area of heater body 1；During material, silicon
Material starts a large amount of fusings, and now also solid-state silicon has crucible bottom, while liquid-state silicon flows to bottom, continues up lifting crucible position
15-25mm, heat gradient is formed after being heated because of heater, second lift crucible ensures crucible bottom in high-temperature region bottom in this step
The higher temperature area in region, avoids crucible bottom from solidification phenomenon occur；
4), collapse material：
The internal solid silicon of crucible 2 continues to melt, and a large amount of melt silicon occur, and material in crucible is monitored in good time, when not molten silicon is complete
When portion is swum in silicon liquid, now liquid level is located at following at the top of heater, and rise crucible 2 is until the top of crucible 2 is higher by heater
The 1/5 of the short heating leaf length of body 1, because crucible crucible bottom is in high-temperature region, therefore effectively melt solidification phenomenon is avoided to occur；
5), temperature stabilization section：
Temperature-resistant in control thermal field when silicon material melt-through is in a liquid state in crucible 2, lifting bushing position is up to liquid in crucible
Identity distance is from being the 3/10 of short heating leaf length with a distance from the top of heater, and now liquid level is located at high-temperature region upper area, in the temperature
The lower position of crucible 2 of degree is kept for constant 1-2 hours；
6), seeding：
Temperature of thermal field is adjusted, seeding production is carried out to silicon liquid in crucible 2, keeps liquid level in crucible to be in height during seeding
Warm area, and continue keep crucible in distance of the liquid level at the top of heater for it is short heating leaf length 3/10 between；
7), shouldering turns shoulder：
Shouldering is carried out to the silicon rod after seeding and turns shoulder production, shouldering turns in shoulder production, keeps liquid level distance heating in crucible
Between distance at the top of device is the 3/10 of short heating leaf length；
8) it is, isometrical：
Silicon single crystal rod turns to carry out after shoulder etc. through production, keeps in step 7) bushing position is constant to carry out isometrical production, isometrical
Start using lifting device gradually to lift bushing position after 50mm, by the basis of bushing position step 7) when isometrical 200mm
2-10mm is risen, ensures that liquid level is located in the crystal pulling setting position of high-temperature region, i.e. aperture settings position in crystal pulling production in crucible, protects
It is constant until isometrical end to hold liquid level and heater distance from top in crucible；In the step, gradually carried again using after isometrical 50mm
Bushing position is risen, and ensures that liquid level lifting capacity is 2-10mm in isometrical 50-200mm, the operation effectively reduces silicon single crystal rod
In isometrical head oxygen content, drop oxygen effect is shown in accompanying drawing 2 and accompanying drawing 3, while in order to avoid due to the liquid level distance big unfavorable later stage
Cheng Jing, therefore crystal pulling liquid level distance is reduced using gradually lifting bushing position after isometrical 50mm, ensure the later stage into crystalloid amount；
9), finish up；
10), blowing out cools down.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (7)
- A kind of 1. heater, it is characterised in that：Including integrally formed cylindric heater body (1), the heater body (1) enclosed and formed by connection sheet (14) alternating series connection by multiple long heating plates (11) and multiple short heating plates (12), the length Heating plate (11) is wide with the short heating plate (12) and top is concordant sets, and the heater body top is high-temperature region, its Bottom is low-temperature space, each formed with gap (13), each length between long heating plate (11) and its adjacent short heating plate (12) One first groove (111) is radially offered along heater body (1) at the top of heating plate (11), at the top of each short heating plate (12) One second groove (121) is radially offered along heater body (1), the first groove (111) groove depth is more than the second groove (121) groove It is deep.
- A kind of 2. heater according to claim 1, it is characterised in that：Short heating plate (12) length and long heating plate (11) length ratio is between 1/5 to 3/4.
- A kind of 3. heater according to claim 1, it is characterised in that：First groove (111) width, the second groove (121) width and gap (13) wide setting, the width are 10-20mm.
- A kind of 4. heater according to claim 1, it is characterised in that：First groove (111) thickness of groove bottom and Two grooves (121) thickness of groove bottom is identical, and the thickness is equal to connection sheet (14) height, while the thickness=long heating plate (11) is wide Degree/2.
- A kind of 5. monocrystalline silicon production method using claim 1-5 heaters, it is characterised in that：Comprise the following steps：1), prepare：Heater body (1) is put in thermal field, by a certain amount of solid-state silicon raw material loaded in crucible (2), utilizes lifting device Crucible (2) and heater body (1) relative position is adjusted, is ensured at the top of crucible (2) relative to low at the top of heater body (1) 60-70mm, now crucible (2) crucible bottom is in heater body (1) low-temperature space；2), evacuate：Oxygen in thermal field is drained using vacuum system, while is filled with argon gas as protective gas；3), material：To heater body (1) electrified regulation, crucible (2) interior silicon material starts after there is melt silicon, is filled by the lifting in thermal field Put and crucible (2) is moved up into 45-65mm, now crucible bottom is in high-temperature region lower area；4), collapse material：Crucible (2) internal solid silicon continues to melt, and when not molten silicon is all swum in silicon liquid, rise crucible (2) is until crucible (2) Top is higher by the 1/5 of the short heating leaf length of heater body (1)；5), temperature stabilization section：Temperature-resistant in control thermal field when the interior silicon material melt-through of crucible (2) is in a liquid state, lifting crucible (2) position is until in crucible Distance of the liquid level at the top of heater body (1) is the 3/10 of short heating leaf length, and now liquid level is located at high-temperature region upper zone Domain, at such a temperature bushing position kept for constant 1-2 hours；6), seeding：Temperature of thermal field is adjusted, seeding production is carried out to the interior silicon liquid of crucible (2), keeps crucible (2) interior liquid level to be in during seeding High-temperature region, and continue to keep distance of crucible (2) the interior liquid level at the top of heater body (1) as the 3/10 of short heating leaf length Between；7), shouldering turns shoulder：Shouldering is carried out to the silicon rod after seeding and turns shoulder production, shouldering turns in shoulder production, keeps crucible (2) interior liquid level apart from heater Between distance at the top of body (1) is the 3/10 of short heating leaf length；8) it is, isometrical：The constant isometrical production of progress of bushing position in step 7) is kept, starts gradually to lift earthenware using lifting device after isometrical 50mm Crucible position, 2-10mm will be risen on the basis of bushing position step 7) when isometrical 200mm, ensure that liquid level is located in high temperature in crucible Aperture settings position in the production of the crystal pulling setting position in area, i.e. crystal pulling, keep the interior liquid level of crucible (2) and heater body (1) top Portion this apart from constant until isometrical end；9), finish up；10), blowing out cools down.
- 6. monocrystalline silicon production method according to claim 5, it is characterised in that：In step 3), including substep once：(a), crucible (2) interior silicon material starts after there is melt silicon, and crucible (2) is moved up into 30- by the lifting device in thermal field 40mm, now crucible (2) crucible bottom is in heater body high-temperature region lower area；(b), during material, when silicon material largely melts, there is solid-state silicon in crucible bottom, continues up lifting crucible position 15-25mm, protects Crucible bottom is demonstrate,proved in the higher temperature area of high-temperature region lower area.
- 7. monocrystalline silicon production method according to claim 5, it is characterised in that：Argon gas is filled with the thermal field as protection Gas.
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| CN109371459A (en) * | 2018-12-21 | 2019-02-22 | 内蒙古中环光伏材料有限公司 | A kind of ladder-like heater improving melt temperature gradient |
| CN112391676A (en) * | 2019-08-13 | 2021-02-23 | 新特能源股份有限公司 | Single crystal furnace thermal field, control method thereof and single crystal furnace |
| CN113350023A (en) * | 2021-07-17 | 2021-09-07 | 左点实业（湖北）有限公司 | Massage intensity adjusting method and device |
| CN115044966A (en) * | 2022-05-26 | 2022-09-13 | 西安奕斯伟材料科技有限公司 | Heater and working method thereof |
| CN115198350A (en) * | 2022-07-15 | 2022-10-18 | 麦斯克电子材料股份有限公司 | Thermal field system capable of reducing oxygen content of silicon crystal and process method |
| CN115216834A (en) * | 2022-07-27 | 2022-10-21 | 四川晶科能源有限公司 | Heater and single crystal furnace |
| WO2023029708A1 (en) * | 2021-08-31 | 2023-03-09 | 银川隆基硅材料有限公司 | Heater and single crystal furnace thermal field |
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