CN101922040A - Device of oxygen control growth in single crystal furnace - Google Patents
Device of oxygen control growth in single crystal furnace Download PDFInfo
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- CN101922040A CN101922040A CN2009100997103A CN200910099710A CN101922040A CN 101922040 A CN101922040 A CN 101922040A CN 2009100997103 A CN2009100997103 A CN 2009100997103A CN 200910099710 A CN200910099710 A CN 200910099710A CN 101922040 A CN101922040 A CN 101922040A
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Abstract
The invention belongs to the technical field of semiconductor separation and particularly relates to a device of oxygen control growth in processes of producing and separating single crystal silicon. The device is formed by improving a heater, a guiding cylinder and a lower insulation system in a single crystal furnace, the height of a blade of the heater is reduced, the hot source area at the bottom of a crucible is decreased, the bottom of the quartz crucible is heated little and less oxygen in the production process is generated; a sealing guide system is reconstructed, an encryption type guiding cylinder is additionally arranged on an upper cover plate, and can accelerate the cooling speed; and a lower insulation system in the furnace is reconstructed, therefore, the insulation effect of a lower insulation cylinder is reinforced, more oxygen from a crystal and melt interface can be taken away, the oxygen content is reduced and generated boroxol complex is decreased. The invention can effectively reduce generation and retention of the oxygen in the production process and control generation and transportation of the oxygen, reduces the process and the quantity of the oxygen entering a single crystal, and has the advantages of simple structure, low cost and convenient installation, use and operation.
Description
Technical field
The invention belongs to technical field of semiconductor separation, the device of a kind of oxygen control growth when particularly relating to a kind of production, separating single crystal silicon.
Background technology
At present, the manufacturer of China's semiconductor monocrystal silicon rod (heavy stone used as an anchor) adopts the single crystal growing furnace Straight pull to produce silicon single crystal rod (heavy stone used as an anchor) when producing semiconductor silicon material mostly, and these silicon single crystal rods (heavy stone used as an anchor) are used to make monocrystaline silicon solar cell mostly; It is relevant with the boron oxygen concn in the silicon chip that scientific research finds that initial light induced attenuation phenomenon appears in P type (boron-doping) monocrystaline silicon solar cell, when illumination or electric current injection, will cause the boron of silicon chip and oxygen to form boron oxygen complex body, thereby minority carrier life time is reduced, B+2O → (illumination or electric current inject) BO
2. according to relevant document record, the boron in the silicon chip, oxygen level are big more, and the boron oxygen complex body that illumination or electric current injection condition produce down is many more, and it is just big more that minority carrier lifetime reduces amplitude; And in the silicon chip of hypoxemia, minority carrier life time is minimum with the attenuation amplitude of light application time, so oxygen level in the reduction silicon single crystal, just can reduce the decay of the solar monocrystalline silicon power of battery, and for the production of traditional semiconductor monocrystal silicon rod (heavy stone used as an anchor), the oxygen level in the control silicon single crystal rod (heavy stone used as an anchor) in general is difficult to accomplish.Traditional mode of production is produced silicon single crystal rod (heavy stone used as an anchor) with the single crystal growing furnace Straight pull, oxygen mainly is to be subjected to thermogenesis by quartz crucible in crystal growing process, oxygen derives from the quartz crucible of fusion, and constantly transports to crystal and melt free surface by the melt thermal convection and to enter the monocrystalline crystalline and stretch in the whole process of growth; The generating principle of oxygen and transport mechanism and be: pyritous melt (1420 ℃) oxygen and quartz crucible reaction, reaction equation is as follows:
Si+SiO2→2SiO
The SiO that generates enters into silicon melt, and in the pulling process of monocrystalline, brilliant change and convection current that crucible is transferred from a team to another to melt produces a very large impact added the thermal convection of melt itself, therefore, enters the surface that SiO in the silicon melt can be transported to melt.Most SiO this moment (99%) can be in the bath surface volatilization, and the argon gas that is added in the process (Ar) is taken away then, and remaining SiO (1%) can decompose in silicon melt, and is as follows:
SiO→Si+O
The oxygen that is produced after decomposing enters silicon single-crystal in growth drawing process subsequently, and in the end be present in the silicon crystal with the gap attitude, so, for the photoelectric conversion rate that makes monocrystaline silicon solar cell is improved, reduce light decay rate, will set about reducing oxygen level silicon single crystal rod (heavy stone used as an anchor) drawing process from production process: and existing single crystal growing furnace it exist following defective: the depth of blade of well heater is too high, make the thermal source area of crucible bottom big like this, therefore quartz crucible is heated just big, the silicon of quartz crucible bottom and the reaction of oxygen are just violent, longitudinal temperature gradient is big in the single crystal growing furnace simultaneously, thermal convection is strong, oxygen level, oxygen concn is relatively just high, the deflector of cooling blast deflector is not really desirable in addition, so just can not take away oxygen from silicon liquid level fast, thereby increase the duration of contact and the chance of oxygen and monocrystalline, so oxygen enters in the silicon single-crystal in the single crystal growing drawing process and just increases.
Summary of the invention
The objective of the invention is to solve, reform the defective that exists in the existing single crystal growing furnace structure, the device of a kind of oxygen control growth in the single crystal growing furnace is provided.It can effectively reduce the content that enters oxygen in the silicon single-crystal in the single crystal growing drawing process this device.
The purpose that the present invention proposes is achieved in that when this structure in the stove of design improvement, we are bigger at the thermal source area of the crucible bottom that exists on the original structure in the stove, be that the quartz crucible bottom is heated more, impel the reaction of the silicon of quartz crucible bottom and oxygen very violent, thus in process of production the oxygen of Chan Shenging with regard to more defective; Take its bottom of former heater blade, promptly this part heater blade at following heat-preservation cylinder has shortened, increased a ciphering type guide shell newly on upper cover plate, the thermal insulation layer carbon felt as heat-preservation cylinder insulation has down been increased the number of plies.
Its bottom of heater blade, promptly this part heater blade at following heat-preservation cylinder has shortened 100mm, just well heater has been removed around the blade of crucible bottom one circle and has been made it to have shortened 100mm; In addition, the structure of its heater blade, material, installation, method of attachment all are the same as the original; Increase a ciphering type guide shell on upper cover plate again, this ciphering type guide shell is exactly the logical graphite garden bobbin in two, and it is shelved on the upper cover plate, between bell and upper cover plate, flexibly connects with bell, upper cover plate; Improved the heat insulation effect of time heat-preservation cylinder besides, the thermal insulation layer carbon carpet veneer number as heat-preservation cylinder insulation down is increased to the 10-12 layer, its installation method has been strengthened the heat insulation effect of time heat-preservation cylinder with original the same; Guiding device after the reform can quicken speed of cooling, reduced longitudinal temperature gradient, reduce thermal convection, can take away more oxygen from crystal and melt interface like this, thereby reduced oxygen level, molten/crucible boundary layer thickness is increased, oxygen level also can descend, reduce the boron oxygen complex body of generation, thereby improved the photoelectric conversion rate of monocrystaline silicon solar cell; Simultaneously, when concrete operations, crystal pulling power is controlled to below the 45KW; Though they look like independently parts, have stronger coupling, thereby reach the purpose of invention.
The present invention can effectively reduce generation, the delay of oxygen in the production process like this owing to improved the well heater in the single crystal growing furnace, increase a ciphering type guide shell, strengthened the heat insulation effect of time heat-preservation cylinder; This apparatus structure is simple, cheap, easy for installation, use operation and original equally make things convenient for, can effectively control generation, the conveying of oxygen and reduced oxygen enters advantages such as the process of monocrystalline and quantity.
Description of drawings
Concrete structure of the present invention is provided by following embodiment and accompanying drawing thereof.
Fig. 1 be the oxygen control growth in single crystal furnace that proposes according to the present invention its structure of device face cross-sectional schematic.
Below in conjunction with Fig. 1, describe the CONSTRUCTED SPECIFICATION and the working condition of the concrete device that proposes according to the present invention in detail.
Among Fig. 1: 1, neck; 2, bell; 3, argon gas is blown into direction; 4, ciphering type guide shell; 5, cool off guide shell fast; 6, upper cover plate [graphite insulation cover]; 7, go up heat-preservation cylinder; 8, go up stay-warm case; 9, middle stay-warm case; 10, quartz crucible; 11, plumbago crucible; 12, middle heat-preservation cylinder; 13, well heater; 14, stove inside clearance; 15, well heater connects the pin of Graphite Electrodes; 16, following heat-preservation cylinder; 17, following stay-warm case; 18, Graphite Electrodes; 19, stove tube; 20, stove aspirating hole; 21, air flow line; 22, furnace chamber; 23, crucible rotating shaft; 24, graphite tray.
Embodiment
As shown in Figure 1, the operation steps of Grown by CZ Method silicon single-crystal oxygen control growth device provided by the invention mainly comprises: thermal field installation, charging, heating, crystal pulling, cooling etc.; Thermal field is installed: each parts (being graphite piece) in the stove are installed, are installed from the bottom up (be exactly to adorn after the graphite piece of tearing open earlier, after the graphite piece of tearing open dress earlier); Key is when dress well heater (13), electrode and electrode screw must be tightened, guarantee that well heater (13) does not have and rock, each parts is installed the centering of will trying one's best, strengthen the heat insulation effect of heat-preservation cylinder (16) down, carbon carpet veneer number is increased to the 10-12 layer, middle heat-preservation cylinder (12), last heat-preservation cylinder (7), on carbon carpet veneer number be the 6-8 layer, after stay-warm case installed, install cover plate [graphite insulation cover] (6), make upper cover plate [graphite insulation cover] (6) and graphite tray (24) centering, each thermal field component remains on a concentrically ringed state as far as possible.Concrete erection sequence is as follows: graphite piece is inhaled one time with suction cleaner before installing again; Well heater (13) connects to tighten to after the pin (15) of Graphite Electrodes and Graphite Electrodes (18) join with the graphite screw is fastening by well heater guarantees on the metal electrode screw that well heater (13) nothing rocks; Put into ready carbon felt, be generally 6 layers, cover upper cover plate [graphite insulation cover] (6) then; Put down stay-warm case (17) successively, middle stay-warm case (9) and last stay-warm case three stay-warm cases such as (8) note not running into when putting well heater (13); Crucible rotating shaft (23) and fastening with the metal screw is installed, opens crucible from housing and change power supply, it is no abnormal to see that rotation has, and then loads onto graphite tray (24) and plumbago crucible (11); Then, with alcohol wipe stove tube sealing-ring and cover upper furnace tube (19).The gloves of charging usefulness and the clothes of feeding are changed in charging; Dress quartz crucible (10), there is quartz crucible (10) candle in elder generation no abnormal, uses alcohol wipe quartz crucible (10) inwall then and puts into plumbago crucible (11); Put into the silicon small powder in quartz crucible (10) bottom and make it to spread a substratum, put into mother alloy, cover with small powder again, put into silicon material not of uniform size again, in the middle of aniseed was put, middle moulding mixture was placed on around the aniseed, sprinkle fritter silicon material it is entered in the slit, so repeatedly, charging 50-55kg; After charging is finished crucible is given to and arrive 2rpm surely, confirm to have or not friction to collide, and the crucible position is reduced to 0.5 inch place fast; Stopping crucible after the crucible potential drop puts in place changes, and installs upper cover plate [graphite insulation cover] (6), cools off guide shell (5) fast, puts ciphering type guide shell (4) again; Check upper cover plate [graphite insulation cover] (6), cool off the stopping property of guide shell (5) and ciphering type guide shell (4) fast, big slit cannot occur; Bell (2) closes; Then check the body of heater vacuum condition: open vacuum-pump power supply, open extraction valve after 1 minute; Be evacuated to and open argon gas air blowing 2 minutes about 10pa again, carry out so repeatedly three times; After treating that vacuum is evacuated to below the 5pa in the stove, closing extraction valve, check the body of heater leak rate, is qualified less than 0.67pa/3min side.Heating melt: open extraction valve and argon flow amount switch; On housing, open heater switch; Progressively increase voltage according to following table:
| Time | 0min | 20min | 40min | 60min |
| Power | 20kw | 45kw | 65kw | 95kw |
During melt, [the crucible position is higher before the reform than well heater] should be put into the crucible position earlier+0.5 inch to+1.0 inches between, according to the melt situation crucible position that progressively descends.Materialization is to three/for the moment, see obviously spoil down after, crucible potential drop to 0.But can not be lower than 0 again.Cooling is stable: opening crucible after materialization is intact changes the brilliant power supply that changes, and given crucible changes 2 and changes brilliant commentaries on classics 8 commentaries on classics, keeps high temperature half an hour; Divide and three times power to be reduced to [seeding power last time] 45kw, stable maintenance 1 hour; Crystal-pulling: seeding, when waiting liquid level temperature not fluctuate, slowly descend and go up axle, make seed crystal just touch liquid level.As find temperature drift or on the low side, should adjust power immediately.As temperature when 1416 spend, wait aperture to take all of after, open and brilliant rise power switch, slowly lift seed crystal, when four ribs (＜100〉crystal) appear in the thin neck of pulling out, seeding is described successfully, otherwise welding seed crystal again; Necking down, draw monocrystalline with seed crystal after, the thin neck that begins to contract, the thin neck that contracts is the dislocation of drawing in the monocrystalline in order to get rid of.The diameter of thin neck generally is controlled at 3-5mm, and the length of thin neck is about 6-8 times of thin neck diameter.Contracting the pulling rate of thin neck can soon can be slow, is generally 3-6mm/min; Shouldering, after the thin neck that contracts was finished, pulling rate was reduced to about 0.4mm/min, and suitably cooling, made crystal long thick.The angle of shouldering generally is controlled to be about 150 degree.Change shoulder, when waiting the diameter of shouldering to grow up 75-80% to aimed dia, slowly improve pulling rate, if find that crystal growth is too fast or lift when speed surpasses 0.6mm/min and will suitably heat up, beginning changes shoulder, makes crystal reach aimed dia smoothly.Change and take on when finishing soon, little by little pulling rate is adjusted to and drawn isometrical pulling rate, open crucible and rise power supply, and give last crucible servo-actuated.Isometrical, change the shoulder back when crystal diameter is suitable, adjust the camera lens of diameter control, it is about 1/3 to press aperture, drops into control pulling monocrystal automatically, controls furnace chamber pressure simultaneously, the crystalline pulling rate, argon gas flow velocity and brilliant commentaries on classics, Crucible change, given suitable crucible ratio, and the distance that the Crucible position is remained between quick guide shell (4) lower edge and the liquid level remains on 10-20mm.According to the characteristics of heating of the well heater (13) after the reform, the compensation of warm school is slightly larger.Ending when the surplus material of molten silicon in the quartz crucible (8)≤10%, begins ending.Withdraw from diameter control, heat up gradually, also can suitably improve some pulling rates in case of necessity, it is thin that crystal is received, and the half that finishes up can stop the crucible servo-actuated, the best harvest taper shape of afterbody.After having finished up, promote crystal or reduce the crucible position, make crystal throw off liquid level 30-40 millimeter, prevent that molten silicon crystallographic expansion hits crystal in the quartz crucible.After blowing out, crystal pull and be separated from liquid level, stop the crucible rotation, the pass is closed axle and is lifted, slowly until being zero, the given 2mm/min of pulling rate withdraws from temp autocontrolled, must use heat preservation method last axle rotating speed accent, falling power earlier kept 15 minutes to 25kw, half an hour, internal power reduced to 0 altogether, closed heating power supply, also will rationally fall the crucible position during this, fall crucible position 20mm after the crystallization of pot bottom material liquid level in 5 minutes, be sure not to fall lowly excessively.Stop to heat after one hour and close argon gas, treat that vacuum is extracted into the limit, close the pipeline valve of finding time earlier, stop vacuum pump again; Stop to heat 4.5-5 hour later removable stove and get crystal.
Claims (2)
1. the device of oxygen control growth in single crystal furnace, the device that it is characterized in that this oxygen control growth is its bottom of former heater blade, promptly this part heater blade at following heat-preservation cylinder has shortened, on upper cover plate, increased a ciphering type guide shell newly, the thermal insulation layer carbon felt as heat-preservation cylinder insulation has down been increased the number of plies.
2. device according to claim 1 is characterized in that said heater blade has shortened 100mm, and the structure of its heater blade, material, installation, method of attachment are all with original the same; Said ciphering type guide shell is exactly the logical graphite garden bobbin in two, and it is shelved on the upper cover plate, between bell and upper cover plate, flexibly connects with bell, upper cover plate; Said thermal insulation layer carbon carpet veneer number as heat-preservation cylinder insulation down is increased to the 10-12 layer, and its installation method is with original the same.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100997103A CN101922040A (en) | 2009-06-10 | 2009-06-10 | Device of oxygen control growth in single crystal furnace |
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| CN2009100997103A CN101922040A (en) | 2009-06-10 | 2009-06-10 | Device of oxygen control growth in single crystal furnace |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618920A (en) * | 2012-04-25 | 2012-08-01 | 浙江华友电子有限公司 | Heat energy controlling method for melting process of single crystal furnace |
| CN103305905A (en) * | 2013-05-30 | 2013-09-18 | 浙江长兴众成电子有限公司 | Variable crucible ratio monocrystal silicon growth method |
| CN103422167A (en) * | 2012-05-23 | 2013-12-04 | 浙江锦锋光伏科技有限公司 | Control method of oxygen content in single crystal furnace |
| CN106435715A (en) * | 2016-11-03 | 2017-02-22 | 保山新澳泰能源有限公司 | Single-crystal thermal field gradient additional adjustment system |
| CN107604430A (en) * | 2016-07-11 | 2018-01-19 | 上海超硅半导体有限公司 | Low oxygen content monocrystalline silicon growing method |
| CN108796602A (en) * | 2018-07-04 | 2018-11-13 | 江西中昱新材料科技有限公司 | A kind of single crystal growing furnace inner draft tube |
| CN110923807A (en) * | 2019-12-31 | 2020-03-27 | 宁晋晶兴电子材料有限公司 | Thermal field and method for improving quality of monocrystalline silicon |
| CN113463181A (en) * | 2021-09-03 | 2021-10-01 | 江苏矽时代材料科技有限公司 | Semiconductor monocrystalline silicon growth device |
| CN116479525A (en) * | 2023-06-25 | 2023-07-25 | 苏州晨晖智能设备有限公司 | Single crystal furnace, single crystal furnace adjusting method and method for producing low-oxygen crystal bar |
-
2009
- 2009-06-10 CN CN2009100997103A patent/CN101922040A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618920A (en) * | 2012-04-25 | 2012-08-01 | 浙江华友电子有限公司 | Heat energy controlling method for melting process of single crystal furnace |
| CN103422167A (en) * | 2012-05-23 | 2013-12-04 | 浙江锦锋光伏科技有限公司 | Control method of oxygen content in single crystal furnace |
| CN103305905A (en) * | 2013-05-30 | 2013-09-18 | 浙江长兴众成电子有限公司 | Variable crucible ratio monocrystal silicon growth method |
| CN103305905B (en) * | 2013-05-30 | 2015-08-05 | 浙江中晶科技股份有限公司 | A kind of monocrystalline silicon growing method becoming crucible ratio |
| CN107604430A (en) * | 2016-07-11 | 2018-01-19 | 上海超硅半导体有限公司 | Low oxygen content monocrystalline silicon growing method |
| CN106435715A (en) * | 2016-11-03 | 2017-02-22 | 保山新澳泰能源有限公司 | Single-crystal thermal field gradient additional adjustment system |
| CN108796602A (en) * | 2018-07-04 | 2018-11-13 | 江西中昱新材料科技有限公司 | A kind of single crystal growing furnace inner draft tube |
| CN110923807A (en) * | 2019-12-31 | 2020-03-27 | 宁晋晶兴电子材料有限公司 | Thermal field and method for improving quality of monocrystalline silicon |
| CN110923807B (en) * | 2019-12-31 | 2021-06-08 | 宁晋晶兴电子材料有限公司 | Thermal field and method for improving quality of monocrystalline silicon |
| CN113463181A (en) * | 2021-09-03 | 2021-10-01 | 江苏矽时代材料科技有限公司 | Semiconductor monocrystalline silicon growth device |
| CN113463181B (en) * | 2021-09-03 | 2021-11-02 | 江苏矽时代材料科技有限公司 | Semiconductor monocrystalline silicon growth device |
| CN116479525A (en) * | 2023-06-25 | 2023-07-25 | 苏州晨晖智能设备有限公司 | Single crystal furnace, single crystal furnace adjusting method and method for producing low-oxygen crystal bar |
| CN116479525B (en) * | 2023-06-25 | 2023-09-15 | 苏州晨晖智能设备有限公司 | Method for producing low-oxygen crystal bar |
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