CN102808216A - Float-zone monocrystalline silicon production process and float-zone thermal field - Google Patents
Float-zone monocrystalline silicon production process and float-zone thermal field Download PDFInfo
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- CN102808216A CN102808216A CN2012103010114A CN201210301011A CN102808216A CN 102808216 A CN102808216 A CN 102808216A CN 2012103010114 A CN2012103010114 A CN 2012103010114A CN 201210301011 A CN201210301011 A CN 201210301011A CN 102808216 A CN102808216 A CN 102808216A
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Abstract
The invention discloses a float-zone monocrystalline silicon production process and a float-zone thermal field and relates to a monocrystalline silicon production technique. Since the inner diameter of a heating coil is increased and is enabled to be more than or equal to 30mm and at least one stage of step platform is arranged outside the upper inclined surface of the heating coil, to change the effect of a magnetic force line, the float-zone thermal field provided by the embodiment of the invention has the advantages that the polycrystalline silicon with larger diameter can be thoroughly melted and the drawing of zone-melt monocrystalline silicon with larger diameter can be realized.
Description
Technical field
The present invention relates to the monocrystalline silicon production technology, relate in particular to the molten thermal field in a kind of study on floating zone silicon producing and manufacturing technique and district.
Background technology
At present; Carry out the common dull and stereotyped Duckbill type coil of little internal diameter that adopts of the molten thermal field in district that study on floating zone silicon is produced; The sectional view of this heater coil is as shown in Figure 1; Comprise ramp 101, lower inclined plane 102 and water service pipe 103, this heater coil maximum can be dissolved the polycrystalline rod about diameter 80mm, the maximum 105mm of the diameter of silicon single crystal that grows.
Therefore, use this heater coil, it is light to feed intake, and yields poorly, and can not realize drawing large diameter study on floating zone silicon.
Summary of the invention
The embodiment of the invention provides a kind of study on floating zone silicon producing and manufacturing technique and district molten thermal field, to realize drawing the bigger study on floating zone silicon of diameter.
Thermal field is melted in a kind of district that the embodiment of the invention provides, and comprising: preheating ring, heater coil and stay-warm case, wherein:
The ramp of said heater coil is provided with at least one grade of step platform outward, and the internal diameter of said heater coil is more than or equal to 30mm.
Further, said heater coil ramp is provided with the two-stage step platform outward.
Preferable, said heater coil ramp external diameter is 60mm, and the outer first step stepped diameters of said heater coil ramp is 80-85mm, and the outer second stage of said heater coil ramp stepped diameters is 100-110mm.
Wherein, said heater coil internal diameter is 30-32mm, and said heater coil external diameter is 220-240mm.
Further, the mesopore of said preheating ring is up big and down small tapered hole.
Further, the distance between said preheating ring and the said heater coil is 1.5-2.5mm.
Preferable, the internal diameter of said stay-warm case is 160-180mm, said stay-warm case height is 35-45mm.
Better, the distance between said stay-warm case and the said heater coil is 25-35mm.
The embodiment of the invention also provides a kind of district that uses the embodiment of the invention to provide to melt the study on floating zone silicon producing and manufacturing technique of thermal field, comprising:
The polysilicon bar is fixed on the axle lower end, seed crystal is fixed on the lower shaft top;
Through preheating ring said polysilicon bar is preheated;
Polysilicon bar after preheating is displaced downwardly to plane on the heater coil, and axle is gone up in rotation and lower shaft carries out the fusing of polysilicon bar and the growth of silicon single crystal, the internal diameter of said heater coil is more than or equal to 30mm.
Further, the ramp of said heater coil is provided with at least one grade of step platform outward.
Further, said heater coil ramp external diameter is 60mm, and the outer first step stepped diameters of said heater coil ramp is 80-85mm, and the outer second stage of said heater coil ramp stepped diameters is 100-110mm.
Preferable, the mesopore of said preheating ring is up big and down small tapered hole.
Preferable, said heater coil is arranged with stay-warm case, and the internal diameter of said stay-warm case is 160-180mm, and said stay-warm case height is 35-45mm.
Further, said lower shaft translational speed is 2-5mm/min, and the said axle translational speed that goes up is confirmed according to the specification of the silicon single crystal of said lower shaft translational speed, polysilicon bar and growth.
Preferable, saidly said polysilicon bar is preheated through preheating ring, specifically comprise:
Said preheating ring is moved to the heater coil top, and polysilicon bar tapering is moved down into said preheating ring center;
After burner hearth is evacuated to 2pa, reach 0.2-0.6Mpa to being inflated to furnace pressure power in the stove;
Open leaving air control valve and keep furnace pressure power, and open heater supply, start high pressure, said polysilicon bar is preheated.
Better, in the process of growth of the fusing of said polysilicon bar and silicon single crystal, charge flow rate is 15-20L/m in the stove, and wherein, the upper outlet flow is 13-25L/m, and following rate of discharge is 0-13L/m.
Further, axle and lower shaft in the said rotation specifically comprise:
Last axle speed of rotation is 0.3-5 rev/min, and the lower shaft speed of rotation is 6-25 rev/min.
The embodiment of the invention provides a kind of study on floating zone silicon producing and manufacturing technique and district molten thermal field; Enlarged the internal diameter of heater coil; Make the internal diameter of heater coil more than or equal to 30mm, outside the ramp of heater coil, be provided with one-level step platform at least simultaneously, thereby change the effect of magneticline of force; Make the bigger polycrystalline silicon material of diameter (polycrystalline rod diameter 110mm) thoroughly to melt, and then realize drawing the bigger study on floating zone silicon (single crystal diameter 130mm) of diameter.
Description of drawings
Fig. 1 is a heater coil structural representation in the prior art;
The molten thermal field structure synoptic diagram in district that Fig. 2 provides for the embodiment of the invention;
The heater coil structural representation that Fig. 3 provides for the embodiment of the invention;
The study on floating zone silicon producing and manufacturing technique schema that Fig. 4 provides for the embodiment of the invention;
The study on floating zone silicon production status synoptic diagram that Fig. 5 provides for the embodiment of the invention.
Embodiment
The embodiment of the invention provides a kind of study on floating zone silicon producing and manufacturing technique and district molten thermal field; Enlarged the internal diameter of heater coil; Make the internal diameter of heater coil more than or equal to 30mm, outside the ramp of heater coil, be provided with one-level step platform at least simultaneously, thereby change the effect of magneticline of force; Make the bigger polycrystalline silicon material of diameter thoroughly to melt, and then realize drawing the bigger study on floating zone silicon of diameter.
As shown in Figure 2, the molten thermal field in the district that the embodiment of the invention provides comprises: preheating ring 201, heater coil 202 and stay-warm case 203, wherein:
Outside the ramp 2021 of heater coil 202 at least one grade of step platform is set, and the internal diameter r of heater coil is more than or equal to 30mm.
The shape that step platform can change magneticline of force is set, and then makes the bigger polycrystalline silicon material of diameter thoroughly to melt, thereby realize using larger-diameter polycrystalline silicon material to make silicon single crystal.
Usually, the two-stage step platform is set outside the heater coil ramp gets final product, certainly, those skilled in the art can be according to practical situation, and the diameter of the polycrystalline silicon material that will melt, suitably increase and decrease the quantity of step platform.
The embodiment of the invention provides a kind of preferable district to melt thermal field, and the heater coil ramp of the molten thermal field in this district is provided with two-stage step platform at least outward, and is as shown in Figure 2; Heater coil ramp external diameter r1 is 60mm; The outer first step stepped diameters r2 of heater coil ramp is 80-85mm, and the outer second stage stepped diameters r3 of heater coil ramp is 100-110mm, certainly; Numbers of steps can suitably increase, and is as shown in Figure 3.
In order to melt the bigger polycrystalline silicon material of diameter preferably, the specification of heater coil also suitably increases better, and for example heater coil internal diameter r can be 30-32mm; The heater coil external diameter can be 220-240mm; When external diameter is 220mm, when internal diameter was 32mm, the fusing effect was better.
In the molten thermal field in the district that the embodiment of the invention provides, can use preheating ring well known to those skilled in the art, for obtaining better to melt effect, can further use mesopore is the preheating ring of up big and down small tapered hole.
Wherein, the distance h between preheating ring and the heater coil is 1.5-2.5mm, and promptly about 2mm, when being arranged on 2mm, the fusing effect is preferable.
In the molten thermal field in the district that the embodiment of the invention provides; For reducing next section (about 50mm) long longitudinal temperature gradient of monocrystalline solid-liquid interface, make solid-liquid interface more smooth, the internal diameter that can suitably increase specification to the stay-warm case of stay-warm case is 160-180mm; The stay-warm case height is 35-45mm; When the internal diameter of stay-warm case is 180mm, when the stay-warm case height was 35mm, heat insulation effect was preferable.
The stay-warm case upper surface is welded with ventilating water pipe, and water-flowing amount is provided with according to the distance between the diameter of silicon single crystal that generates and stay-warm case and the heater coil, and usually, maintenance hydraulic pressure is 0.2-0.6Mpa.
Usually, the distance between stay-warm case and the heater coil is according to the specification setting of stay-warm case and heater coil, and in embodiments of the present invention, the distance H between stay-warm case and the heater coil is that 25-35mm is preferable.
When thermal field is melted in this district of installation, can adopt following installation procedure:
Heater coil is installed earlier, is required horizontal heater coil center on the medullary ray of last axle, lower shaft.Then with the heater coil installation stay-warm case that is as the criterion; Promptly; Stay-warm case is installed in heater coil below, and the center of stay-warm case also need be on last, the medullary ray of lower shaft, and the distance between stay-warm case and coil is controlled between the 25-35mm (look diameter of silicon single crystal and decide); Corresponding setting device can be set, adjust the distance between stay-warm case and coil at any time according to practical situation.Preheating ring is arranged on the heater coil top; About preheating ring and heater coil spacing 2mm; Preheating ring is fixed on the motion cylinder on the furnace wall and can passes in and out, and turnover distance can be controlled by computer, preheating ring at work the time its center also on last, the medullary ray of lower shaft.
After the molten thermal field in district installs, can carry out flushing test, if water-tight; Can lead to 30%-40% left and right sides high pressure (low pressure), carry out the preheating ring heat test, preheating ring is rubescent because of induction; At this moment, provable heater wire can works better, owing to be to try in air hollow; So when heating, should avoid power excessive, in order to avoid the preheating ring oxidation.
The molten thermal field in the district that provides through the embodiment of the invention, the silicon single crystal bar diameter that is melted is bigger, can every feeds intake about 40kg, and the silicon single crystal weight of being produced can reach 37kg, has realized producing the bigger silicon single crystal of diameter.
The embodiment of the invention is also corresponding to provide a kind of study on floating zone silicon producing and manufacturing technique, as shown in Figure 4, comprising:
Step S401, with the polysilicon bar be fixed on the axle lower end, seed crystal is fixed on the lower shaft top;
Step S402, the polysilicon bar is preheated through preheating ring;
Step S403, the polysilicon bar after will preheating are displaced downwardly to plane on the heater coil, and rotation, move and go up axle and lower shaft carries out the fusing of polysilicon bar and the growth of silicon single crystal, and wherein, the internal diameter of heater coil is more than or equal to 30mm.
The molten thermal field in the district that this process method can use the embodiment of the invention to provide carries out, and also can use the molten thermal field in district of other accords with production condition to carry out, and usually, employed heater coil internal diameter need be more than or equal to 30mm.
When thermal field was melted in the district that uses the embodiment of the invention to provide, the heater coil ramp of the molten thermal field in this district was provided with at least one grade of step platform outward.
Further; Can the two-stage step platform be set outside the heater coil ramp, for example, heater coil ramp external diameter r1 is 60mm; The outer first step stepped diameters r2 of heater coil ramp is 80-85mm; The outer second stage stepped diameters r3 of heater coil ramp is 100-110mm, and certainly, numbers of steps can suitably increase.
Preferable, heater coil internal diameter r can be 30-32mm, and the heater coil external diameter can be 220-240mm, and when external diameter is 220mm, when internal diameter was 32mm, the fusing effect was better.
In this study on floating zone silicon producing and manufacturing technique, employed preheating ring can be preheating ring well known to those skilled in the art, and for obtaining better to melt effect, can further use mesopore is the preheating ring of up big and down small tapered hole.
Wherein, the distance h between preheating ring and the heater coil is 1.5-2.5mm, and promptly about 2mm, when being arranged on 2mm, the fusing effect is preferable.
In the molten thermal field in this district, the specification of set stay-warm case also can suitably increase under the heater coil, for example; The internal diameter of stay-warm case is 160-180mm, and the stay-warm case height is 35-45mm, when the internal diameter of stay-warm case is 180mm; When the stay-warm case height was 35mm, heat insulation effect was preferable.
The stay-warm case upper surface is welded with ventilating water pipe, and water-flowing amount is provided with according to the distance between the diameter of silicon single crystal that generates and stay-warm case and the heater coil, and usually, maintenance hydraulic pressure is 0.2-0.6Mpa.
Usually, the distance between stay-warm case and the heater coil is according to the specification setting of stay-warm case and heater coil, and in embodiments of the present invention, the distance H between stay-warm case and the heater coil is that 25-35mm is preferable.
In the study on floating zone silicon producing and manufacturing technique that the embodiment of the invention provides; Step S403 need move axle and lower shaft; For the bigger silicon single crystal of growth diameter that can be more stable, can slow down the translational speed of lower shaft, it is preferable that the lower shaft translational speed is set to 2-5mm/min; The translational speed of last axle can be confirmed according to the specification of the silicon single crystal of lower shaft translational speed, polysilicon bar and growth, go up axle usually and move speed in the 3-6mm/min scope.
In the study on floating zone silicon producing and manufacturing technique that the embodiment of the invention provides, step S402 preheats the polysilicon bar through preheating ring, specifically comprises:
Preheating ring is moved to the heater coil top, and polysilicon bar tapering is moved down into the preheating ring center;
After burner hearth is evacuated to 2pa, reach 0.2-0.6Mpa to being inflated to furnace pressure power in the stove;
Open leaving air control valve and keep furnace pressure power, and open heater supply, start high pressure, the polysilicon bar is preheated.
In the process of growth of the fusing of polysilicon bar and silicon single crystal, charge flow rate can suitably increase with rate of discharge up and down in the stove, and preferable, the interior charge flow rate of stove is 15-20L/m, and wherein, the upper outlet flow is 13-25L/m, and following rate of discharge is 0-13L/m.
When axle and lower shaft carried out the growth of fusing and silicon single crystal of polysilicon bar in rotation, last speed of rotation was 0.3-5 rev/min, the lower shaft speed of rotation be 6-25 rev/min preferable.
When carrying out monocrystalline silicon production, employed equipment can satisfy above-mentioned parameter and condition is set gets final product, for example; Can use the equipment of condition specific as follows: go up axle stroke 2000mm, fast 0-300mm/min, 0-30mm/min at a slow speed; Rotating speed 0-30rpm, lower shaft stroke 2600mm, 0-300mm/min fast; 0-30mm/min at a slow speed, rotating speed 0-30rpm, peak power output 120kw; Water coolant: intake pressure 04-05MPa, inflow temperature 20-25 ℃, water outlet 30-35 ℃; Protective atmosphere: argon gas (purity more than or equal to 99.9995%, dew point smaller or equal to-75 ℃).
Concrete; When carrying out monocrystalline silicon production, mainly be according to the high-frequency induction heating principle, utilize the magnetic field that produces behind the logical high voltage electric of heater coil; Produce inductive current (being eddy current) at polysilicon surface; Make the fusing of polycrystalline silicon rod local heating, the melting zone is flowed on the crystal seed (being seed crystal) of coil below, under the protection of high-purity argon gas slowly; Carry out seeding, the crystalline substance that contracts, the thin neck that contracts, shouldering, get rid of bag, close rib, expand shoulder, change processes such as shoulder, isodiametric growth, ending, obtain required study on floating zone silicon.
After confirming that the molten thermal field in district can normally use, can carry out the production of study on floating zone silicon: the polysilicon bar is fixed on the axle lower end, and seed crystal is fixed on axle top in the lower shaft, aims at the heater coil center simultaneously; Preheating ring is moved to center, coil top, polysilicon bar tapering is moved down into the preheating ring center, then, close all fire doors and purging valve; Burner hearth is found time, start cooling water recirculation system simultaneously, control cooling water flow and temperature of cooling water well; When vacuum is evacuated to about 2Pa, close vacuum system, to inflating in the stove; When furnace pressure power reached 0.2-0.6MPa, leaving air control valve made air inlet and gives vent to anger the maintenance balance about opening, at this moment; Open heater supply, start high pressure, charge bar is preheated.
After the heating of polysilicon bar; Shift out preheating ring, lower shaft rotation in the startup, last axle rotating speed is controlled at 0.3-5 rev/min; The lower shaft rotating speed is controlled at 6-25 rev/min; Material is displaced downwardly on the coil place, plane beginning material, after material melt, moves to below the coil on seed crystal and the fusion polycrystalline carries out welding, as shown in Figure 5.At this moment the power of will controlling well maintenance welding is not flowed and is collapsed; Do not solidify; Begin seeding then, the crystalline substance that contracts, the thin neck that contracts, shouldering, get rid of bag, close rib, amplification (expanding shoulder), change shoulder, isodiametric growth, finish up, break, blowing out, tear process such as stove open, realize the production of silicon single crystal.
Usually, when being 2-5mm/min through isometrical production rate, the speed that the polysilicon bar moves down can be according to equal-volume than calculating.
The embodiment of the invention provides a kind of study on floating zone silicon producing and manufacturing technique and district molten thermal field; Enlarged the internal diameter of heater coil; Make the internal diameter of heater coil more than or equal to 30mm, outside the ramp of heater coil, be provided with one-level step platform at least simultaneously, thereby change the effect of magneticline of force; Make the bigger polycrystalline silicon material of diameter thoroughly to melt, and then realize drawing the bigger study on floating zone silicon of diameter.
Obviously, those skilled in the art can carry out various changes and modification to the present invention and not break away from the spirit and scope of the present invention.Like this, belong within the scope of claim of the present invention and equivalent technologies thereof if of the present invention these are revised with modification, then the present invention also is intended to comprise these changes and modification interior.
Claims (13)
1. thermal field is melted in a district, comprising: preheating ring, heater coil and stay-warm case, it is characterized in that, wherein:
The ramp of said heater coil is provided with at least one grade of step platform outward, and the internal diameter of said heater coil is more than or equal to 30mm.
2. thermal field is melted in district as claimed in claim 1, it is characterized in that, said heater coil ramp is provided with the two-stage step platform outward.
3. thermal field is melted in district as claimed in claim 2, it is characterized in that, said heater coil ramp external diameter is 60mm, and the outer first step stepped diameters of said heater coil ramp is 80-85mm, and the outer second stage of said heater coil ramp stepped diameters is 100-110mm.
4. thermal field is melted in district as claimed in claim 1, it is characterized in that, said heater coil internal diameter is 30-32mm, and said heater coil external diameter is 220-240mm.
5. thermal field is melted in district as claimed in claim 1, it is characterized in that, the mesopore of said preheating ring is up big and down small tapered hole.
6. thermal field is melted in district as claimed in claim 1, it is characterized in that, the distance between said preheating ring and the said heater coil is 1.5-2.5mm.
7. thermal field is melted in district as claimed in claim 1, it is characterized in that, the internal diameter of said stay-warm case is 160-180mm, and said stay-warm case height is 35-45mm.
8. thermal field is melted in district as claimed in claim 1, it is characterized in that, the distance between said stay-warm case and the said heater coil is 25-35mm.
9. a study on floating zone silicon producing and manufacturing technique is characterized in that, comprising:
The polysilicon bar is fixed on the axle lower end, seed crystal is fixed on the lower shaft top;
Through preheating ring said polysilicon bar is preheated;
Polysilicon bar after preheating is displaced downwardly to plane on the heater coil, and rotation, move goes up axle and lower shaft carries out the fusing of polysilicon bar and the growth of silicon single crystal, the internal diameter of said heater coil is more than or equal to 30mm.
10. method as claimed in claim 9 is characterized in that, said lower shaft translational speed is 2-5mm/min, and the said axle translational speed that goes up is confirmed according to the specification of the silicon single crystal of said lower shaft translational speed, polysilicon bar and growth.
11. method as claimed in claim 9 is characterized in that, saidly through preheating ring said polysilicon bar is preheated, and specifically comprises:
Said preheating ring is moved to the heater coil top, and polysilicon bar tapering is moved down into said preheating ring center;
After burner hearth is evacuated to 2pa, reach 0.2-0.6Mpa to being inflated to furnace pressure power in the stove;
Open leaving air control valve and keep furnace pressure power, and open heater supply, start high pressure, said polysilicon bar is preheated.
12. method as claimed in claim 11 is characterized in that, in the process of growth of the fusing of said polysilicon bar and silicon single crystal, charge flow rate is 15-20L/m in the stove, and wherein, the upper outlet flow is 13-25L/m, and following rate of discharge is 0-13L/m.
13. method as claimed in claim 9 is characterized in that, axle and lower shaft in the said rotation specifically comprise:
Last axle speed of rotation is 0.3-5 rev/min, and the lower shaft speed of rotation is 6-25 rev/min.
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| CN105200512A (en) * | 2015-10-19 | 2015-12-30 | 天津市环欧半导体材料技术有限公司 | Thermal field structure for drawing zone-melting 8-12-inch silicon single crystal |
| US9797062B2 (en) | 2013-04-25 | 2017-10-24 | Zhejiang Jingsheng M & E Co., Ltd | Zone melting furnace thermal field with dual power heating function and heat preservation method |
| CN107366017A (en) * | 2017-09-04 | 2017-11-21 | 青海鑫诺光电科技有限公司 | A kind of monocrystalline silicon ending equipment and its application method |
| CN108179462A (en) * | 2016-12-08 | 2018-06-19 | 有研半导体材料有限公司 | A kind of heating coil for being used to prepare area and melting major diameter single crystal |
| US10138573B2 (en) | 2013-04-25 | 2018-11-27 | Zhejiang Jingsheng M & E Co., Ltd | Auxiliary heating device for zone melting furnace and heat preservation method for single crystal rod thereof |
| CN112210819A (en) * | 2019-07-10 | 2021-01-12 | 芯恩（青岛）集成电路有限公司 | Preparation method and equipment of crystal bar |
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