CN101173838A - Novel directional solidification and purification stove - Google Patents
Novel directional solidification and purification stove Download PDFInfo
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- CN101173838A CN101173838A CNA2007101454425A CN200710145442A CN101173838A CN 101173838 A CN101173838 A CN 101173838A CN A2007101454425 A CNA2007101454425 A CN A2007101454425A CN 200710145442 A CN200710145442 A CN 200710145442A CN 101173838 A CN101173838 A CN 101173838A
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Abstract
The invention relates to a purification device for materials, in particular to a new type directional solidification and purification furnace for the materials with high purity, belonging to the field of semiconductor metallurgy purification, which provides a technical proposal of condensate purification and a purification furnace with convenient production, large yield, rapid speed and low cost. The invention is characterized in that: the outer furnace housing is formed by a double-layer steel plate; the thermal insulation material and refractory material are lined internally; as a result, a whole closed straight barrel vertical furnace body is formed; in the furnace body, a plurality of resistance heaters are hung vertically and evenly to the upper part of the inner wall of the furnace; an induction heater is positioned at the lower part of the resistance heater; a water-cooling assembly, a graphite heating block, and a graphite crucible are positioned on a hydraulic pressure lifting underframe positioned on the central axis of the furnace body; the graphite crucible and the resistance heater are the same in height, and the induction heating and the heating method of resistance are combined organically without the vacuum technique. The invention has the advantages of improving productivity, saving energy and having wide raw material sources, which has profound and realistic significance to the development of the photovoltaic industry and the standing on the independent development.
Description
Technical field
The present invention relates to a kind of material purifying plant, particularly high-purity material a kind of novel directional solidification and purification stove of purifying, this device belongs to semiconductor metallurgy purification category.
Background technology
At present, in high-precision pointed collar territories such as aerospace, highly purified material is widely used, especially the demand of semiconductor source material such as silicon is increasing, and the method that material is purified adopts zone-melting method usually, be that the alleged usually district of those skilled in the art is molten, promptly the melting zone of a bar-shaped material ingot is carried out local heat by eddy-current heating, and traveling heater, this melting zone is slowly moved along the material ingot by certain orientation, utilize the difference of impurity equilibrium concentration segregation coefficient between solid phase and liquid phase, impurity just segregates in solid phase or the liquid phase and is redistributed in fusing and process of setting repeatedly, thereby reaches the purpose of removing impurity.But this traditional method is because speed of production is slow, and output is little, and the price height has limited using and developing of high-purity material.The silicon materials ingot furnace has only Germany and U.S. GT ingot furnace at present, their price is very expensive, every and the used silicon raw material of ingot casting will use the remaining material end to end of crystal-pulling silicon greatly more than 1,500 ten thousand RMB, and is expensive, it is per ton to be roughly equal to RMB 1,700,000, therefore raw material sources are very in short supply, even like this, offshore company also implements blockade on new techniques to China, so the method for purification of semiconductor source materials such as silicon is outmoded, can satisfy the needs of development far from.Also have, because energy shortage, earth environment worsen, press for green energy resource, the development of solar cell is main developing direction, and the production of solar cell is because the raw material problems cost is very high, press for solar cell raw material cheaply, the low cost of semiconductor source material productions such as silicon makes the photovoltaic industry promise well.How making semiconductor source material such as silicon produce cost degradation is semiconductor source material manufacturing industry urgent problems such as domestic silicon.
Summary of the invention
The purpose of this invention is to provide a kind of novel directional solidification and purification stove, output is little in the solution high-purity material purification process, the shortcoming that purifying velocity is slow, utilize the purification principle, the method innovation invention that district noted earlier is molten is coagulated the purification technique scheme for a kind of district of different designs, mainly be that electromagnetic induction heating and resistance heated comprehensively are one, be applied on the new-type same directional solidification furnace, promptly be in purification furnace, material to molten state passes through the cooling directional solidification, making this cooling zone coagulate the zone slowly moves by certain orientation, utilize the difference of impurity equilibrium concentration segregation coefficient between solid phase and liquid phase, solidify repeatedly with fusion process in impurity just segregate in solid phase or the liquid phase and redistributed, thereby reach the purpose of removing impurity, but because the more raw material of the method single treatment, thereby can improve output greatly, principle and method have been designed a kind of convenient production according to this, output is big, speed is fast, cheap purification furnace.
The present invention is achieved through the following technical solutions:
A kind of novel directional solidification and purification stove of the present utility model, wherein: directional solidification and purification stove is that double-layer plate is formed outer furnace shell inner lining as thermal insulation material and refractory material is formed the vertical body of heater of whole airtight straight bucket, in body of heater, some vertical uniform the hanging of resistance heater in the stove upper inside wall, induction heater is arranged on the bottom of resistance heater, be positioned at and be provided with water-cooled assembly, graphite heating piece, graphite crucible on the hydraulic elevation type underframe on the body of heater axis successively, graphite crucible and resistance heater are contour.
A kind of novel directional solidification and purification stove described in the utility model, wherein: described induction heater is to be arranged on furnace wall, resistance heater bottom cold induction coil of stainless steel water and anti-oxidation fire resistant heat preserving ring layer all around to form, corresponding with the height and position of graphite heating piece, produce the cold induction coil of stainless steel water of certain frequency alternating magnetic field and the graphite heating piece of generation inductive loop by energising, formation is rapidly heated to the induction heating apparatus of graphite crucible bottom heating the graphite heating piece.
A kind of novel directional solidification and purification stove described in the utility model, wherein: described some the resistance heaters of vertically hanging on the stove inwall are resistance heaters that Si-Mo rod is formed.
A kind of novel directional solidification and purification stove described in the utility model, wherein: described some the resistance heaters of vertically hanging on the stove inwall are resistance heaters that Elema is formed.
A kind of novel directional solidification and purification stove described in the utility model, wherein: described some the resistance heaters of vertically hanging on the stove inwall are resistance heaters that graphite heater is formed.
A kind of novel directional solidification and purification stove described in the utility model, wherein: described water-cooled assembly comprises the water-cooled tray salver and is incubated diathermanous material layer, water-cooled tray salver and to be incubated the size of diathermanous material layer consistent and greater than furnace bottom furnace chamber size, slide up and down the fitting-type sealing by sealing ring and the furnace bottom furnace chamber formation that is provided with on the water-cooled tray salver, the cooling water that suitable flow is arranged in the described water-cooled tray salver, the diathermanous material layer of described insulation are stacked piece or the monoblock formations of being set to of the diathermanous material layer of high-temperature-resistant thermal-insulation of several layers.
A kind of novel directional solidification and purification stove described in the utility model, wherein: the thickness of described graphite heating piece is not less than 80mm.
A kind of novel directional solidification and purification stove described in the utility model, wherein: described body of heater top is provided with can open and the middle bell that is embedded with cast gate, and semiconductor fusing feed liquid to be purified pours into behind the graphite crucible with sealing device gate seal by cast gate.
A kind of novel directional solidification and purification stove described in the utility model, wherein: the described slotting device for runner that is encapsulated in the cast gate place is the seal bar with certain radian termination.
A kind of novel directional solidification and purification stove described in the utility model, wherein: described furnace roof cast gate place is provided with can stretch into blowing argon gas in the stove, catch up with most air to make is in the movable tunger tube of argon shield state in the stove.
Main feature of the present invention is to rely on the bigger graphite material in bottom by the more heat energy of eddy-current heating deposit, thereby form uniform thermal field in the assurance furnace chamber, simultaneously, last furnace chamber has Si-Mo rod or other resistive heater heats, guaranteed that the crucible wall heat does not does not scatter and disappear laterally, and can only be by the bottom graphite block and by corresponding power supply intermodulation power, simultaneously by cooling water and water-cooled tray salver guarantee with heat from the bottom unidirectional shedding, form unidirectional orientation coagulation mechanism process, thereby reach semiconductor silicon, the directional solidification effect and the refining effect of other semi-conducting material and specific alloy material.The present invention has following remarkable advantage:
1, the present invention combines eddy-current heating and resistance class (Si-Mo rod, silicon carbon rod, graphite heater, resistance wire etc.) mode of heating.
2, this patent product is based on independent research fully, can use conventional industrial silicon raw material, and is with low cost, wide material sources.
3, every equipment price deficiency of this patent product is 1,000,000 yuans, substitutes import equipment and material fully.
4, this patent product is broken the restriction that existing device adopts vacuum to purify, and does not need vacuum technique, and is with low cost, simple, and existing home made materials all can be produced.
5, this patent product melts the melting melt simultaneously very big extendable room, can adjust the size of output according to the batch size of the market demand.
6, the melting ingot casting cycle of external silicon ingot furnace reached more than 48 hours, and this patent product ingot casting purification cycle is no more than 18 hours, has improved production efficiency, energy savings greatly.
7, this patent product is based on independent research to China's development photovoltaic industry, and very far-reaching and realistic meanings are arranged.
Description of drawings:
Fig. 1: represent that a kind of region of no pressure of the present invention coagulates purification furnace example structure schematic diagram.
The specific embodiment:
The invention will be described further below in conjunction with the drawings and specific embodiments, but not as a limitation of the invention.
As shown in Figure 1, a kind of novel directional solidification and purification stove, this directional solidification and purification stove is that double-layer plate is formed outer furnace shell 15 inner lining as thermal insulation material and refractory material is formed the vertical body of heater of whole airtight straight bucket, in body of heater, some resistance heater 4 vertical uniform hanging in the stove upper inside wall, induction heater is arranged on the bottom of resistance heater 4, be positioned at and be provided with water-cooled assembly, graphite heating piece 6, graphite crucible 5 on the hydraulic elevation type underframe 12 on the body of heater axis successively, graphite crucible 5 is contour with resistance heater 4.Described induction heater is to be arranged on furnace wall, resistance heater 4 bottom cold induction coil 8 of stainless steel water and anti-oxidation fire resistant heat preserving ring layer 7 all around to form, and corresponding with the height and position of graphite heating piece 6, the thickness of described graphite heating piece 6 is not less than 80mm.Described anti-oxidation fire resistant heat preserving ring layer 7 has certain thickness, cold induction coil 8 energisings of stainless steel water produce the alternating magnetic field of certain frequency, make graphite heating piece 6 produce inductive loop, graphite heating piece 6 is rapidly heated to the eddy-current heating of graphite crucible 5 bottoms heating thereby constitute.Described water-cooled assembly comprises water-cooled tray salver 11 and is incubated diathermanous material layer 10, water-cooled tray salver 11 and to be incubated the size of diathermanous material layer 10 consistent and greater than furnace bottom furnace chamber size constitutes by sealing ring 13 and the furnace bottom furnace chamber that is provided with on the water-cooled tray salver 11 to slide up and down the fitting-type sealing.The cooling water that suitable flow is arranged in the described water-cooled tray salver 11, the stacked piece that is set to of the diathermanous material layer of high-temperature-resistant thermal-insulation that the diathermanous material layer 10 of described insulation is several layers constitutes, and also can be that a monoblock high-temperature-resistant thermal-insulation heat-insulating material constitutes.Described body of heater top is provided with can open and the middle bell 2 that is embedded with cast gate 1, described bell 2 is fire resistant heat preserving water cooled covers, semiconductor fusing feed liquid to be purified pours into graphite crucible 5 backs by cast gate 1 and uses sealing device 18 with gate seal, and the described slotting device for runner 18 at cast gate place that is encapsulated in is for having the seal bar of certain radian termination.Described furnace roof cast gate 1 place is provided with movable tunger tube and stretches into blowing argon gas in the stove, catches up with most air to make and is in the argon shield state in the stove.Vertically hang the resistance heater that the resistance heating body 4 that is used for heating cavity on the stove inwall can be the Si-Mo rod composition for described some.It can also be the resistance heater that Elema is formed.It also can be the resistance heater that graphite heater is formed.Whole purification furnace places on the melt pit pedestal 9 by concrete casting by bottom reinforcement 14.
This device belongs to semiconductor metallurgy purification category, is eddy-current heating and resistance class (Si-Mo rod, silicon carbon rod, graphite heater, resistance wire etc.) mode of heating are combined.First half heating is made up of Si-Mo rod, and the bottom is an eddy-current heating.Concrete enforcement is that heating cavity is made up of two parts, and promptly resistance heater 4 and the bottom at the heating of graphite crucible 5 sidewalls is made up of some the Si-Mo rods of vertically hanging of furnace chamber top graphite heating piece 6 and the cold induction coil 8 of stainless steel water that graphite crucible 5 bottoms are heated formed.By graphite heating piece 6 outer attached certain thickness anti-oxidation fire resistant heat preserving ring layers 7; mainly be to prevent to heat of the heat radiation of the high temperature of graphite heating piece 6 to the cold induction coil 8 of stainless steel water; be to protect the cold induction coil 8 of stainless steel water; place the water-cooled tray salver 11 that stainless steel is manufactured on the required hydraulic elevation type underframe 12 of input and output material; on water-cooled tray salver 11, place the diathermanous material layer 10 of several layers or certain thickness insulation again; water-cooled tray salver 11 and be incubated the consistent size of diathermanous material layer 10 but be slightly larger than furnace bottom furnace chamber size; thereby, play secluding air and prevent the effect that thermal convection current produces so that insulation diathermanous material layer 10 in rise back seals the furnace chamber bottom in the furnace chamber bottom closely connected.On the diathermanous material layer 10 of its certain thickness insulation, place again by graphite heating piece 6, on the plane, top of graphite heating piece 6, place again with its peripheral dimension mutually one to graphite crucible 5, and graphite crucible 5 bottoms are entirely closely connected with graphite heating piece 6.
The course of work: at first hydraulic elevation type underframe 12 is reduced to certain position, cold induction coil 8 of stainless steel water and outer attached certain thickness anti-oxidation fire resistant heat preserving ring layer 7 in the Si-Mo rod on furnace chamber top heating original paper and the lower heating chamber is fixed at this moment, the just diathermanous material layer 10 of certain thickness insulation and the graphite heating piece 6 on stainless steel water cold dish box 11 tops fallen thereupon, at this moment, graphite crucible 5 carefully is put on this graphite heating piece 6, opening hydraulic elevation type underframe 12 slowly rises, graphite crucible 5 and graphite heating piece 6 are sent into furnace chamber, and make the diathermanous material layer 10 of certain thickness insulation on the stainless steel water cold dish box 11 be closely attached at the bottom of the furnace chamber mouth periphery and its sealing.Feed the cooling water of suitable flow simultaneously in the water-cooled tray salver 11.By furnace roof cast gate 1 the tunger tube (not shown) is stretched into Argon the former air of depositing in the stove is caught up with to the greatest extent, make to be in the argon shield state in its stove.And the seal bar 18 that will have the certain radian termination is inserted and is encapsulated in cast gate with gate seal.Adopt the energising of certain order and power, the induction heater of furnace chamber Si-Mo rod heater and lower furnace chamber in the unlatching, because graphite heating piece 6 materials of lower furnace chamber mainly are graphite, and graphite is the good conductor of electricity, and the alternating magnetic field that produces certain frequency by the cold induction coil 8 of stainless steel water produces inductive loop simultaneously and makes its heating graphite crucible 5 bottoms that are rapidly heated in graphite heating piece 6.Because graphite heating piece 6 is selected the bigger graphite block of volume for use, when being heated to uniform temperature, will lay in big thermal energy, thereby the uniformity coefficient that guarantees graphite crucible 5 bottoms and furnace chamber temperature field has been played great role.When treating that the interior temperature of graphite crucible 5 and furnace chamber reaches requirement, open the seal bar 18 of furnace roof cast gate, with fusing treat that purified silicon liquid or other semiconductor to be purified fusing feed liquid pours into graphite crucible 5 by cast gate 1 after, with seal bar 18 cast gate 1 is sealed, stablize behind the certain hour that induction heating power with the cold induction coil 8 of stainless steel water reduces or outage stops heating, and top Si-Mo rod heater continues with certain power heat tracing to be carried out in graphite crucible 5 sides, the heat of graphite crucible 5 systems scatters and disappears and can only pass through graphite crucible 5 bottoms at this moment, and the graphite heating piece 6 that originally heated graphite crucible 5 bottoms this moment is because outage, and the stainless steel water cold dish box 11 below it becomes cooling system, and can cool off generation upwards passing of solid liquid interface comparatively stably by graphite crucible 5 bottoms to the silicon liquid in the graphite crucible 5 uniformly, thereby with the impurity in the silicon liquid owing to above the difference of the segregation coefficient in the solid-liquid two-phase drains into, finish the directional solidification process, reach the effect of purification removal of impurities.Suitable reduce to suitable temperature after, hydraulic elevation type underframe 12 begins to drop to certain position, takes out graphite crucible 5 and changes another graphite crucible 5 and carry out next furnace operating.Will specify to adopt two kinds of mode of heatings why in same stove at this: this is because the solid-liquid freezing interface in the graphite crucible 5 is very responsive to electromagnetic stirr in the directional solidification process, and taboo electromagnetic agitation, Si-Mo rod on the contrary does not only help raw material forms steady solid-liquid freezing interface in graphite crucible 5 for resistance heated does not produce electromagnetic agitation, the reason of two kinds of different heating modes of employing that Here it is in this directional solidification furnace.
Claims (10)
1. novel directional solidification and purification stove, it is characterized in that: directional solidification and purification stove is that double-layer plate is formed outer furnace shell (15) inner lining as thermal insulation material and refractory material is formed the vertical body of heater of whole airtight straight bucket, in body of heater, vertical uniform the hanging of some resistance heaters (4) in the stove upper inside wall, induction heater is arranged on the bottom of resistance heater (4), be positioned at and be provided with water-cooled assembly, graphite heating piece (6), graphite crucible (5) on the hydraulic elevation type underframe (12) on the body of heater axis successively, graphite crucible (5) is contour with resistance heater (4).
2. a kind of novel directional solidification and purification stove according to claim 1, it is characterized in that: described induction heater is for being arranged on cold induction coil of stainless steel water (8) and anti-oxidation fire resistant heat preserving ring layer (7) composition around resistance heater (4) furnace wall, bottom, corresponding with the height and position of graphite heating piece (6), produce the cold induction coil of stainless steel water (8) of frequency alternating magnetic field and the graphite heating piece (6) of generation inductive loop by energising, formation is rapidly heated to the induction heating apparatus of graphite crucible (5) bottom heating graphite heating piece (6).
3. a kind of novel directional solidification and purification stove according to claim 1 is characterized in that: described some the resistance heaters of vertically hanging on the stove inwall (4) are the resistance heaters that Si-Mo rod is formed.
4. a kind of novel directional solidification and purification stove according to claim 1 is characterized in that: described some the resistance heaters of vertically hanging on the stove inwall (4) are the resistance heaters that Elema is formed.
5. a kind of novel directional solidification and purification stove according to claim 1 is characterized in that: described some the resistance heaters of vertically hanging on the stove inwall (4) are the resistance heaters that graphite heater is formed.
6. a kind of novel directional solidification and purification stove according to claim 2, it is characterized in that: described water-cooled assembly comprises water-cooled tray salver (11) and is incubated diathermanous material layer (10), water-cooled tray salver (11) and to be incubated the size of diathermanous material layer (10) consistent and greater than furnace bottom furnace chamber size, go up the sealing ring (13) that is provided with by water-cooled tray salver (11) and slide up and down the fitting-type sealing with furnace bottom furnace chamber formation, the cooling water that suitable flow is arranged in the described water-cooled tray salver (11), the diathermanous material layer of described insulation (10) are stacked piece or the monoblock formations of being set to of the diathermanous material layer of high-temperature-resistant thermal-insulation of several layers.
7. a kind of novel directional solidification and purification stove according to claim 6 is characterized in that: the thickness of described graphite heating piece (6) is not less than 80mm.
8. a kind of novel directional solidification and purification stove according to claim 7, it is characterized in that: described body of heater top is provided with can open and the centre is embedded with the bell (2) of cast gate (1), and semiconductor fusing feed liquid to be purified pours into graphite crucible (5) back usefulness sealing device (18) with gate seal by cast gate (1).
9. a kind of novel directional solidification and purification stove according to claim 8 is characterized in that: the described device for runner (18) that is encapsulated in the cast gate place of inserting is to have the seal bar of certain radian termination.
10. a kind of novel directional solidification and purification stove according to claim 9 is characterized in that: described furnace roof cast gate (1) is located to be provided with and can be stretched into the movable tunger tube that blows out argon gas in the stove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101454425A CN101173838A (en) | 2007-07-06 | 2007-09-12 | Novel directional solidification and purification stove |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710118497 | 2007-07-06 | ||
| CN200710118497.7 | 2007-07-06 | ||
| CNA2007101454425A CN101173838A (en) | 2007-07-06 | 2007-09-12 | Novel directional solidification and purification stove |
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| CN101173838A true CN101173838A (en) | 2008-05-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2007101454425A Pending CN101173838A (en) | 2007-07-06 | 2007-09-12 | Novel directional solidification and purification stove |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071455A (en) * | 2010-12-15 | 2011-05-25 | 哈尔滨工业大学 | Water cooling device for directional solidification of polycrystalline silicon |
| CN102358952A (en) * | 2011-09-09 | 2012-02-22 | 宁波国钰光伏材料有限公司 | Fuel-gas-heating directional solidification furnace |
| CN109930023A (en) * | 2019-03-28 | 2019-06-25 | 西安交通大学 | Manufacturing method of large-tonnage chromium-zirconium-copper alloy |
| CN110749193A (en) * | 2019-10-29 | 2020-02-04 | 河南泰豪机电设备有限公司 | Closed heating furnace for smelting aluminum |
| CN113108595A (en) * | 2021-02-23 | 2021-07-13 | 昆明理工大学 | Industrial molten pool visualization system and method based on electromagnetic tomography technology |
| CN117287966A (en) * | 2023-11-27 | 2023-12-26 | 四川威纳尔特种电子材料有限公司 | Smelting device and method for efficiently forming and producing blank pup joint for bonding wire |
| CN117760150A (en) * | 2024-02-22 | 2024-03-26 | 福建福碳新材料科技有限公司 | Isostatic graphite processing cooling device for manufacturing large semiconductor silicon wafer |
-
2007
- 2007-09-12 CN CNA2007101454425A patent/CN101173838A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071455A (en) * | 2010-12-15 | 2011-05-25 | 哈尔滨工业大学 | Water cooling device for directional solidification of polycrystalline silicon |
| CN102071455B (en) * | 2010-12-15 | 2012-10-17 | 哈尔滨工业大学 | Water cooling device for directional solidification of polycrystalline silicon |
| CN102358952A (en) * | 2011-09-09 | 2012-02-22 | 宁波国钰光伏材料有限公司 | Fuel-gas-heating directional solidification furnace |
| CN102358952B (en) * | 2011-09-09 | 2014-01-15 | 宁波国钰光伏材料有限公司 | Fuel-gas-heating directional solidification furnace |
| CN109930023A (en) * | 2019-03-28 | 2019-06-25 | 西安交通大学 | Manufacturing method of large-tonnage chromium-zirconium-copper alloy |
| CN110749193A (en) * | 2019-10-29 | 2020-02-04 | 河南泰豪机电设备有限公司 | Closed heating furnace for smelting aluminum |
| CN113108595A (en) * | 2021-02-23 | 2021-07-13 | 昆明理工大学 | Industrial molten pool visualization system and method based on electromagnetic tomography technology |
| CN117287966A (en) * | 2023-11-27 | 2023-12-26 | 四川威纳尔特种电子材料有限公司 | Smelting device and method for efficiently forming and producing blank pup joint for bonding wire |
| CN117287966B (en) * | 2023-11-27 | 2024-01-23 | 四川威纳尔特种电子材料有限公司 | Smelting device and method for efficiently forming and producing blank pup joint for bonding wire |
| CN117760150A (en) * | 2024-02-22 | 2024-03-26 | 福建福碳新材料科技有限公司 | Isostatic graphite processing cooling device for manufacturing large semiconductor silicon wafer |
| CN117760150B (en) * | 2024-02-22 | 2024-05-03 | 福建福碳新材料科技有限公司 | Isostatic graphite processing cooling device for manufacturing large semiconductor silicon wafer |
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Open date: 20080507 |