CN203486915U - Directional freezing equipment - Google Patents
Directional freezing equipment Download PDFInfo
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- CN203486915U CN203486915U CN201320596629.8U CN201320596629U CN203486915U CN 203486915 U CN203486915 U CN 203486915U CN 201320596629 U CN201320596629 U CN 201320596629U CN 203486915 U CN203486915 U CN 203486915U
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Abstract
The utility model relates to the field of directional freezing, in particular to directional freezing equipment. An argon tank is arranged outside a furnace body; an inflation valve is mounted on an air outlet of the argon tank; an air outlet of the inflation valve stretches into the center of a water cooling disc by an air duct inside a water cooling shaft; the air outlet end of the air duct is located at the bottom of a quartz crucible; an exhaust funnel fixed on the furnace body stretches into a heat preservation sleeve; the air outlet end of the exhaust funnel is connected with a heat exchanger; the air outlet end of the heat exchange is provided with a valve I; the air outlet end is divided into two branches; one branch is connected with a proportional valve and a vacuum pump unit in sequence; the vacuum pump unit is communicated with the furnace body; the other branch is connected with a differential pressure flowmeter and a vortex vacuum pump in sequence; the air outlet end of the vortex vacuum pump is divided into two branches; one branch is communicated with the air duct and is provided with a valve III; the other branch is communicated with a side-blown air pipe; a valve II is mounted on the side-blown air pipe; the air outlet end of the side-blown air pipe is inserted into the furnace body and is located at the bottom end of the heat preservation sleeve.
Description
Technical field
The utility model relates to directional freeze field, is specifically related to a kind of apparatus for directional solidification and prepares the method for polysilicon.
Background technology
At present, China has become world energy sources production and consumption big country, but energy expenditure level is also very low per capita.Along with economical and social development, China's energy demand is by sustainable growth, for current energy shortage situation, deep thinking is all being carried out in countries in the world, and effort improves efficiency of energy utilization, promote the development and application of renewable energy source, reduce the dependence to Imported oil, strengthen energy security.
The development of photovoltaic industry depends on the purification to polycrystalline silicon raw material.In the process that polycrystalline silicon raw material is purified, there is crucial, a requisite link, exactly polycrystalline silicon raw material is carried out to directional freeze purification, directional solidification technique used is widely used in field of metallurgy purification.Utilize the segregation coefficient between silicon and metallic impurity in polycrystalline silicon raw material to have this feature of larger difference, in process of setting, first the silicon liquid of quartz crucible bottom start to solidify, for reaching fractional condensation balance, the impurity that segregation coefficient is little is out gathered in liquid state to the continuous separation by diffusion of liquid state from the silicon solidifying, along with solidifying constantly, carry out, the concentration of metallic impurity in liquid state is more and more higher, under finally solidifying on the top of ingot casting, after having solidified, under comparatively high temps, be incubated for some time, make each composition fully spread to reach fractional condensation balance, finally the higher one end of metals content impurity is removed, obtain the polycrystalline silicon ingot casting of purifying.
Bridgeman crystal growth method is a kind of conventional growing method, for the material of crystal growth use, be contained in the crucible of cylinder shape, decline lentamente, and by a process furnace with certain temperature gradient, Control for Kiln Temperature is near the fusing point a little more than material.According to the character heater element of material, can select resistance furnace or high frequency furnace.When by heating region, the material in crucible is melted, and when crucible continuous decrease, the temperature of crucible bottom first drops to below fusing point, and starts crystallization, and crystal declines and continues to grow up with crucible.This method is usually used in preparing alkali and alkaline earth metal ions halogenide and fluoride single crystal.
At present in the technology of directional freeze, adopted that crucible bottom water-cooled cooling, crucible rotation are cooling, the drop-down thermal field that leaves of crucible, the technique means such as crucible bottom air blowing.But whole process is all used new argon gas as cooling gas, and cost is very high.Meanwhile, in current directional solidification technique, can't effectively control the concavo-convex and curved transition of solid-liquid interface.
Utility model content
According to above the deficiencies in the prior art, the utility model proposes a kind of apparatus for directional solidification, be applied to Bridgman method polysilicon directional freezing technical, by the setting of sidepiece ventpipe and the speed of circulation of adjusting argon gas, can accurately control the temperature field of quartz crucible inside, control solid-liquid interface and reach minimum resection rate, by air cooling, accelerate ingot casting cooling.
A kind of apparatus for directional solidification described in the utility model, comprises body of heater, and body of heater outside is provided with vacuumometer, and quartz crucible is installed in body of heater, and quartz crucible outside is provided with heating element, insulation sleeve and ruhmkorff coil from inside to outside successively, quartz crucible bottom is provided with aqueous cold plate, aqueous cold plate is connected with ingot pulling mechanism, body of heater is outside equipped with argon tanks, on the air outlet of argon tanks, inflation valve is installed, the place, air outlet of inflation valve extend into aqueous cold plate center by the breather line in water-cooling shaft, the air outlet end of breather line is positioned at quartz crucible bottom, the aiutage being fixed on body of heater extend in insulation sleeve, the air outlet end of aiutage is connected with interchanger, the air outlet end of interchanger is provided with valve one, air outlet end is divided into two branch roads, on one branch road, be connected with proportional valve and vacuum pump group in turn, vacuum pump group comprises lobe pump and slide valve pump, vacuum pump group is connected with body of heater, on another branch road, be connected with differential flowmeter and DRY SCROLL VACUUM PUMP in turn, the air outlet end of DRY SCROLL VACUUM PUMP is divided into two branch roads, one branch road is connected with breather line, and valve three is installed, another branch road is communicated with side air blowing tube, valve two is installed on side air blowing tube, it is inner that the air outlet end of side air blowing tube inserts body of heater, be positioned at the bottom of insulation sleeve.
Preferred version is as follows:
In interchanger, be provided with annular water-cooled slideway.
The place, air outlet of argon tanks is provided with flow mass controller.
Adopt the working method of this utility model to be: charging vacuumizes, heat and make insulation after silicon material fusing, draw ingot until after ingot casting solidifies completely, cooling down is to EO, in vacuum, after being extracted into 400～600Pa, vacuum tightness in body of heater melts step, when temperature rises to 1500～1550 ℃, open proportional valve, control the interior vacustat of body of heater at 40～60KPa; When drawing ingot process to proceed to 20～40%, in quartz crucible, the solid-liquid interface of silicon material is matrix interface, by by-pass valve control three, regulate solid-liquid interface planeness, after drawing ingot process to proceed to 60～70%, in quartz crucible, the solid-liquid interface of silicon material is convex interface, by by-pass valve control two and valve three, regulates solid-liquid interface planeness; The cooling down stage keeps valve one, DRY SCROLL VACUUM PUMP and valve three in open mode, until temperature drops to below 300 ℃.
In the utility model, what described ingot pulling mechanism adopted is the patent No.: 201320233456.3, and the ingot pulling mechanism that patent name is a kind of apparatus for directional solidification, body of heater is fixedly installed on body frame, fire door is installed on body of heater, is installed with leading screw and vacuum pump on body of heater; Lifting table is movably installed in leading screw lower end by screw; Slow speed motor and fast motor are fixedly installed on lifting table outer wall, and are connected with screw with transmission rig by electromagnetic clutch; Swivel joint is fixedly installed in lifting table inside, and water-cooling shaft lower end is movably installed in swivel joint inside, and its upper end is placed in body of heater inside, and aqueous cold plate is installed on water-cooling shaft top; Rotating machine is fixedly installed in lifting table outer wall, and is connected by swing pinion and water-cooling shaft are intermeshing.This device design is unique, both can make water-cooling shaft move up and down, also can water-cooling shaft rotation.In the process of rotation, can keep the vacuum tightness of equipment in the scope of 1～5Pa.Motor can make hoisting appliance decline with the speed rising of 60mm/min fast, and slow speed motor can make hoisting appliance decline with the speed rising of 0.1mm/min.Simple to operate, be easy to control and calculate.
Innovative point of the present utility model is that water-cooling shaft center has been added again to a breather line, and breather line extend into aqueous cold plate center, and aqueous cold plate corresponding position is provided with air outlet.
In the process of directional freeze, exist three recycle systems, the argon gas that system is low temperature is exported via argon tanks, with flow mass controller, control the argon gas amount being filled with, by breather line, to the bottom of quartz crucible, carry out cooling, in equipment running process, gas is entered in interchanger by aiutage, the high temperature argon of discharging becomes gas at normal temperature through interchanger, utilize the opening degree of lobe pump controlled circulation system simultaneously, argon gas reenters body of heater, keeps body of heater vacuum tightness at 40～60KPa; Second system is through differential flowmeter, to measure argon flow amount at the argon gas at heat exchanger exit place, by PLC, control the opening degree that lobe pump carrys out controlled circulation system, thereby the size of regulation and control gas flow, the size of gas flow can be very trickle the curvature of adjusting solid-liquid interface, gas boosts via DRY SCROLL VACUUM PUMP simultaneously, through breather line, is again passed into quartz crucible bottom; The 3rd system is when Open valve two, and during valve-off three, argon gas is blown in body of heater via side air blowing tube, regulates the solid-liquid interface of silicon material in quartz crucible, reaches required effect simultaneously.
When polycrystalline silicon ingot casting solidifies completely, whole crucible temperature can be at 1200～1400 ℃, and during equipment blow-on, temperature is 200～400 ℃, is generally 20～24h this cooling time.DRY SCROLL VACUUM PUMP drives flowing of argon gas, makes argon gas cooling at equipment Rapid Circulation, and be 15～19h cooling time, has greatly reduced the time of cooling, improves the service efficiency of equipment.
The beneficial effect that the utility model has is: this device can complete the needed production status of apparatus for directional solidification effectively.Argon gas cooling recirculation system as hydronic source of the gas, regulates ingot casting periphery thermal field by argon gas, adopts the mode of trickle operation to affect the solid-liquid interface of ingot casting.
Accompanying drawing explanation
Fig. 1 is the utility model schematic diagram.
In figure: 1. aiutage, 2. body of heater, 3. ruhmkorff coil, 4. insulation sleeve, 5. heating element, 6. vacuumometer, 7. quartz crucible, 8. aqueous cold plate, 9. side air blowing tube, 10. breather line, 11. flow mass controllers, 12. argon tanks, 13. interchanger, 14. valve one, 15. vacuum pump groups, 16. proportional valves, 17. differential flowmeters, 18. lobe pumps, 19. slide valve pumps, 20. DRY SCROLL VACUUM PUMP, 21. valve two, 22. valve three, 23. inflation valves.
Embodiment
Below in conjunction with the drawings and specific embodiments, describe the utility model in detail, but the utility model is not limited to specific embodiment.
Embodiment 1:
Erecting equipment, is arranged on body of heater 2 outsides by vacuumometer 6, and body of heater 2 inside are provided with heating element 5, insulation sleeve 4 and ruhmkorff coil 3 from inside to outside successively, and quartz crucible 7 is put into body of heater 2, aqueous cold plate 8 is arranged on to quartz crucible 7 bottoms, aqueous cold plate 8 is connected with ingot pulling mechanism, argon tanks 12 in the outer connection of body of heater 2, the place, air outlet of argon tanks 12 is provided with flow mass controller 11 and inflation valve 23, the place, air outlet of inflation valve 23 extend into aqueous cold plate 8 centers by the breather line 10 in water-cooling shaft, the air outlet end of breather line 10 is positioned at quartz crucible 7 bottoms, the aiutage 1 being fixed on body of heater 2 extend in insulation sleeve 4, the air outlet end of aiutage 1 is connected to interchanger 13, in interchanger 13, be provided with annular water-cooled slideway, the air outlet end of interchanger 13 is provided with valve 1, air outlet end is divided into two branch roads, on one branch road, be connected with proportional valve 16 and vacuum pump group 15 in turn, vacuum pump group 15 comprises lobe pump 18 and slide valve pump 19, vacuum pump group 15 is connected with body of heater 2, on another branch road, be connected with differential flowmeter 17 and DRY SCROLL VACUUM PUMP 20 in turn, the air outlet end of DRY SCROLL VACUUM PUMP 20 is divided into two branch roads, one branch road is connected with breather line 10, and valve 3 22 is installed, another branch road is communicated with side air blowing tube 9, valve 2 21 is installed on side air blowing tube 9, the air outlet end of side air blowing tube 9 inserts body of heater 2 inside, be installed on the bottom of insulation sleeve 4.
Polysilicon 650KG is placed in to quartz crucible 7 inside, starts lifting gantry quartz crucible 7 is raised to melting position, open slide valve pump 19, make the vacuum tightness of device interior drop to 400Pa, open Lodz pump 18, make the vacuum tightness of device interior drop to 2Pa.
To ruhmkorff coil 3 energisings, while being warming up to 800 ℃, close vacuum pump group 15, open inflation valve 23 and flow mass controller 11, the vacuum tightness in body of heater 2 is reached after 50KPa, close inflation valve 23 and flow mass controller 11.Continue to be warming up to 1500 ℃, open proportional valve 16, make the interior vacustat of body of heater 2 at 40KPa, open inflation valve 23, the flow of setting flow mass controller 11 is 30L/min, uses mobile argon gas that the impurity volatilizing in thaw process is taken away.
After polysilicon melts completely, adjust thermal field, the ingot speed of drawing of ingot pulling mechanism is adjusted to 0.12mm/min, open ingot pulling mechanism, quartz crucible 7 is rotated with water-cooling shaft simultaneously.
The flow that flow mass controller 11 is set is 50L/min, opens successively valve 3 22 and DRY SCROLL VACUUM PUMP 20.Through 40 hours, directional freeze process proceeded to 2/3rds, and in the situation that not blowing, solid-liquid interface is convex interface.During operation, more protruding for what liquid level was become, make impurity to the surrounding enrichment of ingot casting, continue to open valve 3 22, make cold argon gas blow to the bottom of quartz crucible 7.When drawing ingot after 60 hours, ingot casting solidifies completely.
The power supply that cuts off ruhmkorff coil 3, is separated from thermal field completely by quartz crucible 7.Close inflation valve 23 and flow mass controller 11, close vacuum pump group 15.Maintain valve 1, DRY SCROLL VACUUM PUMP 20, valve 3 22 in opened condition, make the argon gas of device interior always in recurrent state.6min circulation primary, the convection current of acceleration equipment inside, accelerates heat radiation, and the temperature fall time that makes ingot casting is 19h.
When ingot casting temperature drops to 300 ℃, the equipment of opening takes out ingot casting.Take interchanger 13 apart, the impurity being deposited on heat transfer tube is removed.After cleaning out, reinstall, prepare directional purification next time and produce.
Embodiment 2:
Erecting equipment, is arranged on body of heater 2 outsides by vacuumometer 6, and quartz crucible 7 is installed in body of heater 2 inside, and quartz crucible 7 outsides are installed heating element 5, insulation sleeve 4 and ruhmkorff coil 3 from inside to outside successively, aqueous cold plate 8 is arranged on to quartz crucible 7 bottoms, aqueous cold plate 8 is connected with ingot pulling mechanism, argon tanks 12 in the outer connection of body of heater 2, the place, air outlet of argon tanks 12 is provided with flow mass controller 11 and inflation valve 23, the place, air outlet of inflation valve 23 extend into aqueous cold plate 8 centers by the breather line 10 in water-cooling shaft, the air outlet end of breather line 10 is positioned at quartz crucible 7 bottoms, the aiutage 1 being fixed on body of heater 2 extend in insulation sleeve 4, the air outlet end of aiutage 1 is connected to interchanger 13, in interchanger 13, be provided with annular water-cooled slideway, the air outlet end of interchanger 13 is provided with valve 1, air outlet end is divided into two branch roads, on one branch road, be connected with proportional valve 16 and vacuum pump group 15 in turn, vacuum pump group 15 comprises lobe pump 18 and slide valve pump 19, vacuum pump group 15 is connected with body of heater 2, on another branch road, be connected with differential flowmeter 17 and DRY SCROLL VACUUM PUMP 20 in turn, the air outlet end of DRY SCROLL VACUUM PUMP 20 is divided into two branch roads, one branch road is connected with breather line 10, and valve 3 22 is installed, another branch road is communicated with side air blowing tube 9, valve 2 21 is installed on side air blowing tube 9, the air outlet end of side air blowing tube 9 inserts body of heater 2 inside, be installed on the bottom of insulation sleeve 4.
Polysilicon 650KG is placed in to quartz crucible 7 inside, starts lifting gantry quartz crucible 7 is raised to melting position, open slide valve pump 19, make the vacuum tightness of device interior drop to 500Pa, open Lodz pump 18, make the vacuum tightness of device interior drop to 3Pa.
To ruhmkorff coil 3 energisings, while being warming up to 800 ℃, close vacuum pump group 15, open inflation valve 23 and flow mass controller 11, the vacuum tightness in body of heater 2 is reached after 50KPa, close inflation valve 23 and flow mass controller 11.Continue to be warming up to 1500 ℃, open proportional valve 16, make the interior vacustat of body of heater 2 at 50KPa, open inflation valve 23, the flow of setting flow mass controller 11 is 40L/min, uses mobile argon gas that the impurity volatilizing in thaw process is taken away.
After polysilicon melts completely, adjust thermal field, the ingot speed of drawing of ingot pulling mechanism is adjusted to 0.1mm/min, open ingot pulling mechanism, quartz crucible 7 is rotated with water-cooling shaft simultaneously.
The flow that flow mass controller 11 is set is 40L/min, opens successively valve 3 22 and DRY SCROLL VACUUM PUMP 20.Through 38 hours, directional freeze process proceeded to 2/3rds, and in the situation that not blowing, solid-liquid interface is convex interface.During operation, for liquid level is flattened, impurity, to top plane enrichment, is opened valve 2 21, and valve-off 3 22 makes cold argon gas through side air blowing tube 9, blow to the sidewall of quartz crucible 7, and silicon liquid interface is flattened.When drawing ingot after 58 hours, ingot casting solidifies completely.
The power supply that cuts off ruhmkorff coil 3, is separated from thermal field completely by quartz crucible 7.Close inflation valve 23 and flow mass controller 11, close vacuum pump group 15.Maintain valve 1, DRY SCROLL VACUUM PUMP 20, valve 3 22 in opened condition, make the argon gas of device interior always in recurrent state.5min circulation primary, the convection current of acceleration equipment inside, accelerates heat radiation, and the temperature fall time that makes ingot casting is 18.5h.
When ingot casting temperature drops to 350 ℃, the equipment of opening takes out ingot casting.Take interchanger 13 apart, the impurity being deposited on heat transfer tube is removed.After cleaning out, reinstall, prepare directional purification next time and produce.
This device can be realized the oriented growth of silicon melt, can be good at realizing the object that directional freeze is removed metallicity impurity in polysilicon.Use this device to can be good at the interception of the thermal radiation in downdraw process by quartz crucible 7 sidewalls, effectively reduce the heat loss through radiation of sidewall, make directional solidification effect better compared with usual manner, and sidewall reduces more than 90% with respect to conventional equipment to the crystal grain of center position growth, and ingot casting is effective.
Claims (3)
1. an apparatus for directional solidification, comprises body of heater, and body of heater outside is provided with vacuumometer, and quartz crucible is installed in body of heater, and quartz crucible outside is provided with heating element, insulation sleeve and ruhmkorff coil from inside to outside successively, quartz crucible bottom is provided with aqueous cold plate, aqueous cold plate is connected with ingot pulling mechanism, it is characterized in that body of heater is outside equipped with argon tanks, on the air outlet of argon tanks, inflation valve is installed, the place, air outlet of inflation valve extend into aqueous cold plate center by the breather line in water-cooling shaft, the air outlet end of breather line is positioned at quartz crucible bottom, the aiutage being fixed on body of heater extend in insulation sleeve, the air outlet end of aiutage is connected with interchanger, the air outlet end of interchanger is provided with valve one, air outlet end is divided into two branch roads, on one branch road, be connected with proportional valve and vacuum pump group in turn, vacuum pump group comprises lobe pump and slide valve pump, vacuum pump group is connected with body of heater, on another branch road, be connected with differential flowmeter and DRY SCROLL VACUUM PUMP in turn, the air outlet end of DRY SCROLL VACUUM PUMP is divided into two branch roads, one branch road is connected with breather line, and valve three is installed, another branch road is communicated with side air blowing tube, valve two is installed on side air blowing tube, it is inner that the air outlet end of side air blowing tube inserts body of heater, be positioned at the bottom of insulation sleeve.
2. a kind of apparatus for directional solidification according to claim 1, is characterized in that being provided with in interchanger annular water-cooled slideway.
3. a kind of apparatus for directional solidification according to claim 1, is characterized in that the place, air outlet of argon tanks is provided with flow mass controller.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320596629.8U CN203486915U (en) | 2013-09-26 | 2013-09-26 | Directional freezing equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320596629.8U CN203486915U (en) | 2013-09-26 | 2013-09-26 | Directional freezing equipment |
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| Publication Number | Publication Date |
|---|---|
| CN203486915U true CN203486915U (en) | 2014-03-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201320596629.8U Withdrawn - After Issue CN203486915U (en) | 2013-09-26 | 2013-09-26 | Directional freezing equipment |
Country Status (1)
| Country | Link |
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| CN (1) | CN203486915U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103498194A (en) * | 2013-09-26 | 2014-01-08 | 青岛隆盛晶硅科技有限公司 | Directional solidification equipment and method for preparing polycrystalline silicon by equipment |
| CN109222556A (en) * | 2018-08-22 | 2019-01-18 | 浙江西溪玻璃有限公司 | A kind of glass rapid cooling system |
-
2013
- 2013-09-26 CN CN201320596629.8U patent/CN203486915U/en not_active Withdrawn - After Issue
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103498194A (en) * | 2013-09-26 | 2014-01-08 | 青岛隆盛晶硅科技有限公司 | Directional solidification equipment and method for preparing polycrystalline silicon by equipment |
| CN103498194B (en) * | 2013-09-26 | 2016-01-13 | 青岛隆盛晶硅科技有限公司 | A kind of apparatus for directional solidification and prepare the method for polysilicon |
| CN109222556A (en) * | 2018-08-22 | 2019-01-18 | 浙江西溪玻璃有限公司 | A kind of glass rapid cooling system |
| CN109222556B (en) * | 2018-08-22 | 2020-07-17 | 浙江西溪玻璃有限公司 | Quick cooling system of glass cup |
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Legal Events
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20140319 Effective date of abandoning: 20160113 |
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| AV01 | Patent right actively abandoned |
Granted publication date: 20140319 Effective date of abandoning: 20160113 |
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| C25 | Abandonment of patent right or utility model to avoid double patenting |