CN102220108A - Silicon liquid leakage preventing plugging agent for use in field of production of polycrystalline silicon - Google Patents
Silicon liquid leakage preventing plugging agent for use in field of production of polycrystalline silicon Download PDFInfo
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- CN102220108A CN102220108A CN2011100050878A CN201110005087A CN102220108A CN 102220108 A CN102220108 A CN 102220108A CN 2011100050878 A CN2011100050878 A CN 2011100050878A CN 201110005087 A CN201110005087 A CN 201110005087A CN 102220108 A CN102220108 A CN 102220108A
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Abstract
The invention relates to a silicon liquid leakage preventing plugging agent for use in the field of production of polycrystalline silicon, which belongs to the field of solar photovoltaics. The silicon liquid leakage preventing plugging agent for use in the field of production of polycrystalline silicon can well solve the technical problem of silicon liquid leakage. The silicon liquid leakage preventing plugging agent for use in the field of production of polycrystalline silicon, which can quickly react with molten silicon to form a high-temperature ceramic material. When used on a combined graphite crucible, the plugging agent provided by the invention can directly plug the silicon liquid in a graphite side wall in situ to prevent the silicon liquid from flowing out and prevent a silicon material from losing, the heat field of polycrystalline silicon ingot production furnace is not damaged and safety hazards are eliminated radically.
Description
Technical field
The present invention relates to the photovoltaic field a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent.
Background technology
In the technology of polycrystalline silicon ingot casting, quartz crucible is used to splendid attire silicon material, and the silicon material is finished thawing, solidified long brilliant whole process in quartz crucible.Because quartz crucible begins to soften after temperature surpasses about 1200 ℃, need usually quartz crucible to be fixed with other material.Adopt a graphite base plate to hold the quartz crucible bottom at present, and with several graphite backplates protect quartz crucible around, in the fusing of silicon raw material, crystalline silicon crystallisation process, because a variety of causes, such as the quality of crucible own there is the free time, or charging is too tight, may cause that all crucible breaks, thereby cause silicon liquid to spill quartz crucible.Because the crucible tray done of conventional graphite is put together by several sheet materials, therefore can only prevent the quartz crucible excessive deformation that is heated, can not prevent that silicon liquid from revealing from the gap.
In a single day silicon liquid leak, and the thermal field in not only silicon material loss, and the polycrystalline ingot furnace damages huge, as heat-insulation cage, well heater and body of heater.Serious meeting causes body of heater by burn through, makes the water coolant of cooled furnace wall contact with high temperature silicon liquid, produces a large amount of water vapour and hydrogen, the moment increase of body of heater pressure, thus cause blast, even personal injury takes place.
From the angle of anti-leakage current, it is optimal adding a monoblock type graphite crucible again in the quartz crucible outside, but the polysilicon weight that field of polysilicon production relates to can reach hundreds of kilograms, thereby it needs supporting plumbago crucible bulky.Graphite material that can splendid attire silicon liquid needs high-density graphite, and this raw material is because the restriction of complete processing, and its size is subjected to certain restriction.Incorporate in addition graphite need be emptied from a huge graphite block with mechanical means and form, and tooling cost is high.Thereby can only make the several piece graphite sheet usually and be spliced into the graphite subassembly again.Because the slit between the graphite cake, when crucible lost efficacy, silicon liquid can flow out from the slit between the graphite cake, thereby destroys thermal field, caused the consume of silicon material, structure deteriorate.Therefore the graphite subassembly of being made up of graphite cake can not stop silicon hydrorrhea stream.
The patent No. is CN101169308, patent name is a kind of crucible tray, a kind of crucible tray that adopts carbon/carbon composite to be processed into is disclosed, it comprises base plate, side plate is installed on the base plate, fixedly connected between the adjacent biside plate, it is characterized in that base plate, side plate is processed into by carbon/carbon composite, because carbon/carbon composite inside has accurate three-dimensional structure, the crucible tray of being processed into has good heat conduction and resistance and high temperature resistance property, not only reduced the weight (product density is less than 1.8g/cm3) of crucible tray significantly, and strengthened the mechanical property of crucible tray, make it to be not easy under the effect of external force, to break, and brought up to 300 day or more by original more than 90 day work-ing life, and because adjacent biside plate adopts even tenon structure, product is easy for installation, handling ease, percentage of A-class goods height.But just strengthened the work-ing life of crucible tray, still do not solved the generation of silicon liquid leakage current phenomenon, still do not had the effect of good anti-silicon liquid leakage current.
For on silicon liquid leakage current sfgd., mainly adopt Metal Melting fracture of wire resist technology at present.Be meant that specifically warming plate is all around around the fixing metal fusible link below quartz crucible, when silicon liquid leakage current, the silicon drop is attached to above the fusible link, wire fusing is produced report to the police, thereby remind the user to take measures.Yet in the practical application, there are numerous unreliable factors in this resist technology: at first, the Metal Melting circuit wire position that is laid on bottom of furnace body exists is moved the home position in deviation or the life-time service and is not repaired, and when silicon liquid leakage current, can not guarantee that silicon liquid accurately and timely drops in above the fusible link; Next is when quartz crucible breaks the occurrence of large-area leakage current, the Metal Melting fracture of wire even silicon liquid has fused, but top silicon liquid meeting leakage current is to the various graphite and the metal parts of stove inner bottom part, can be when serious with the water-cooled stainless steel furnace wall burn through of bottom, with the recirculated water generation vigorous reaction in the interlayer of furnace wall, badly damaged ingot furnace, and major safety risks are arranged.And the warning behind the silicon liquid leakage current just takes place in Metal Melting fracture of wire resist technology, thereby reminds the user to adopt measure to remedy, and it can not play and prevent to leak the plumbago crucible holder that several plates that silicon liquid is made from graphite material form.
In recent years; more existing technical literature reports for solution silicon liquid leakage current problem; patent publication No. is CN101423219; patent name is the silicon liquid leakage defense device of a kind of polysilicon purification or ingot furnace; the silicon liquid leakage defense device of a kind of polysilicon purification or ingot furnace is provided; comprise crucible and platform; crucible is located at above the platform; it is characterized in that: also comprise chamfering and coagulating pan; described platform upper surface has a plurality of radially diversion trenchs and a plurality of broadwise diversion trench; described chamfering is located at the periphery of platform bottom; described coagulating pan is located at the following of platform and around one week of platform; the inside of being located at chamfering interior week of described coagulating pan; periphery extends to the outside of platform, and when silicon liquid took place to leak, silicon liquid can flow into by the diversion trench on the platform in the coagulating pan; thereby realize preventing the generation of structure deteriorate and blast, protection flushing and casting workman's personnel safety.
Patent publication No. is CN101158549; patent name is the silicon liquid leakage current securing system of polycrystalline silicon ingot or purifying furnace; the design and the manufacturing technology field that belong to polycrystalline silicon ingot or purifying furnace; main body of heater by bottom band rock wool; place the Thermal insulation cage body of body of heater inner bottom part band insulation base plate; place the heat exchange platform of being with quartz crucible and plumbago crucible in the Thermal insulation cage body; place the central sheath and the boss sleeve pipe at rock wool middle part; be opened in the curb on both sides, plumbago crucible bottom; be opened in the pod apertures on insulation base plate both sides; place on the rock wool of bottom of furnace body the silicon liquid leakage current bearing container with the pod apertures correspondence position, place the formations such as Metal Melting fracture of wire of tape-controller in the silicon liquid leakage current bearing container.The damage of silicon liquid to body of heater avoided in the effect of the flow guide system that confluxes that constitutes by the silicon liquid leakage current bearing container by curb, pod apertures, band Metal Melting fracture of wire.
Having both at home and abroad takes some technical schemes to be used for preventing the potential safety hazard that silicon liquid leakage current causes, especially at home, over 2007, applied for nearly 10 about preventing the patent of silicon liquid leakage current, but they all have a common feature: adopt complicated drainage system with the silicon liquid drainage to holding groove or directly silicon liquid holding groove is set in the lower end, both sides of polycrystalline silicon ingot or purifying furnace graphite base plate DS-Block, implement inconvenient, complex process, be unfavorable for applying aborning, and because temperature contrast, silicon liquid may solidify in the drainage process, cause drainage channel to stop up, in case the serious leakage that quartz crucible breaks and causes takes place, guide arrangement can only local drainage part silicon liquid, and most of silicon liquid still can be revealed along the gap between the graphite backplate of splicing, and not only the loss of silicon material is big, the silicon liquid of leakage current damages huge to the thermal field in the polycrystalline ingot furnace, and potential safety hazard exists all the time.
Therefore, the best approach that solves silicon liquid leakage current problem is exactly with silicon liquid original position splendid attire, neither can cause the loss of silicon material, also can not the more important thing is the thorough potential safety hazard of having eliminated to damaging the thermal field in the polycrystalline ingot furnace.
So seek a kind of cheap for manufacturing costly, be easy to apply aborning, and can prevent effectively absolutely that the method for silicon liquid leakage current or device have quite substantial meaning for whole polycrystalline silicon ingot casting field.
Summary of the invention
The present invention proposes a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, can be good at solving the technical problem of existing silicon liquid leakage current.
Technical scheme of the present invention is:
A kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: the generation high temperature ceramic material takes place to react rapidly with molten silicon liquid.
A kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent comprises that reagent and additive form, and the weight proportion between reagent and the additive is: reagent 10-100 part, additive 0-90 part; Wherein reagent is any one or two kinds in Mo powder or the C powder, and additive is Si
3N
4, SiC, aluminum oxide or magnesian any one or wherein two kinds mixing.Additive can strengthen the mechanical property of plugging agent.
A kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: can be powdery, also can be packaged into strip.
A kind of be used for field of polysilicon production prevent silicon liquid leakage current with plugging agent in the application of built-up type plumbago crucible, wherein: a kind of combined type copple, comprise sidewall and base plate, wherein: base plate is provided with groove, the tenon of the groove on the base plate and sidewall bottom adopts the chase mortise fixed mode that cooperatively interacts to splice, sidewall around be distributed in base plate around; Sidewall and base plate surround a cavity jointly, are filled with plugging agent in the slit between base plate and the sidewall.
Principle of work of the present invention: when silicon liquid leakage current, liquid-state silicon and plugging agent react the generation high temperature ceramic material rapidly and solidify, and have stoped silicon liquid to flow out.Plugging agent can be powdered, also can be packaged into strip, is convenient to construct and keep certain contractility, and the high temperature that can alleviate backplate expands, and can repeatedly use.Use Mo powder or C powder+silicon nitride powder to be configured to plugging agent according to a certain percentage in the experiment.
Adopt the Mo powder as plugging agent, when silicon liquid generation leakage current, the rapid self-propagating reaction of Mo powder and silicon liquid generates MoSi
2
Mo+2Si(l)=?MoSi
2
Adopt the C powder as plugging agent, when silicon liquid generation leakage current, the rapid self-propagating reaction of C powder and silicon liquid generates SiC.
C+Si(l)=?SiC
This reaction is the process of volumetric expansion, thereby the slit is blocked, and has stoped silicon liquid to the graphite side wall external leakage.
Principle: slotting on graphite base plate and the graphite side wall is to fill plugging agent in order to allow in the splicing slit of plugging agent between base plate and backplate, plugging agent and silicon liquid react the generation high temperature ceramic material rapidly, to splice the slit and fill, play the effect of anti-silicon liquid leakage current.If use the graphite base plate and the graphite side wall of existing structure, in the splicing slit, fill plugging agent because folk prescription is to stressed, can be with the slit support bigger, can not play the effect of anti-silicon liquid leakage current.
The test contrast:
Prior art 1: adopt the apertured design of splicing, assembly unit.
Prior art 2: adopt the apertured design of splicing, assembly unit.Increase complicated accessory silicon hydrorrhea stream, leakage current guiding take-off equipment.CN101158549 for example
Effect A: anti-silicon liquid leakage current effect
Effect B: silicon liquid leakage current is to the thermal field damage intensity of polycrystalline silicon ingot or purifying furnace
Table 1 the present invention is applied to the built-up type plumbago crucible compared with the prior art
The implementation result of table 2 different technologies scheme of the present invention relatively
Can find out that from table 2 it is 50 parts in Mo powder that plugging agent of the present invention adopts proportioning, Si
3N
450 parts, the best results of anti-silicon liquid leakage current.
Advantage of the present invention and effect: plugging agent of the present invention is applied to silicon liquid direct in-situ to be got lodged in the graphite side wall behind the built-up type plumbago crucible, silicon liquid can't flow out, can not cause the loss of silicon material, and can not cause damage, thoroughly eliminate potential safety hazard the thermal field of polycrystalline silicon ingot or purifying furnace.
Reference numeral
Accompanying drawing 1 is the structural representation of existing base plate;
Accompanying drawing 2 is structural representations of existing side plate splicing;
Accompanying drawing 3 is structural representations that existing base plate is connected with side plate;
Accompanying drawing 4 is structural representations of a kind of embodiment base plate among the present invention;
Accompanying drawing 5 is structural representations of a kind of embodiment side plate splicing among the present invention;
Accompanying drawing 6 is structural representations that a kind of embodiment base plate among the present invention is connected with side plate;
Accompanying drawing 7 is structural representations of the another kind of embodiment base plate among the present invention;
Accompanying drawing 8 is structural representations of the another kind of embodiment side plate splicing among the present invention;
Accompanying drawing 9 is structural representations that the another kind of embodiment base plate among the present invention is connected with side plate;
Description of drawings: groove 1, tenon 2, base plate 3, sidewall 4, plugging agent 5.
Embodiment
Embodiment 6, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 80 parts of reagents, 20 parts of additives; Wherein reagent is the C powder, and additive is SiC.All the other are with embodiment 2.
Embodiment 7, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 70 parts of reagents, 30 parts of additives; Wherein reagent is the Mo powder, and additive is an aluminum oxide.All the other are with embodiment 2.
Embodiment 8, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 65 parts of reagents, 35 parts of additives; Wherein reagent is the C powder, and additive is a magnesium oxide.All the other are with embodiment 2.
Embodiment 9, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 60 parts of reagents, 40 parts of additives; Wherein reagent is the Mo powder, and additive is Si
3N
4All the other are with embodiment 2.
Embodiment 10, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 55 parts of reagents, 45 parts of additives; Wherein reagent is the C powder, and additive is SiC.All the other are with embodiment 2.
Embodiment 11, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 50 parts of reagents, 50 parts of additives; Wherein reagent is the Mo powder, and additive is Si
3N
4All the other are with embodiment 2.
Embodiment 12, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 45 parts of reagents, 55 parts of additives; Wherein reagent is the Mo powder, and additive is an aluminum oxide.All the other are with embodiment 2.
Embodiment 13, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 40 parts of reagents, 60 parts of additives; Wherein reagent is the C powder, and additive is a magnesium oxide.All the other are with embodiment 2.
Embodiment 14, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 60 parts of reagents, 40 parts of additives; Wherein reagent is the C powder, and additive is Si
3N
4With mixing of SiC.All the other are with embodiment 2.
Embodiment 15, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 55 parts of reagents, 45 parts of additives; Wherein reagent is the Mo powder, and additive is that SiC mixes with magnesian.All the other are with embodiment 2.
Embodiment 16, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 50 parts of reagents, 50 parts of additives; Wherein reagent is the mixing of C powder and Mo powder, and additive is a magnesium oxide and the mixing of aluminum oxide.All the other are with embodiment 2.
Embodiment 17, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 45 parts of reagents, 55 parts of additives; Wherein reagent is the mixing of Mo powder and C powder, and additive is SiC.All the other are with embodiment 2.
Embodiment 18, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 40 parts of reagents, 60 parts of additives; Wherein reagent is the C powder, and additive is aluminum oxide and Si
3N
4Mixing.All the other are with embodiment 2.
Embodiment 19, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 30 parts of reagents, 70 parts of additives; Wherein reagent is the Mo powder, and additive is Si
3N
4All the other are with embodiment 2.
Embodiment 20, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 20 parts of reagents, 80 parts of additives; Wherein reagent is the C powder, and additive is Si
3N
4All the other are with embodiment 2.
Embodiment 21, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 comprises that reagent and additive form, and the weight proportion between reagent and the additive is: 10 parts of reagents, 90 parts of additives; Wherein reagent is the Mo powder, and additive is a magnesium oxide.All the other are with embodiment 2.
Embodiment 22, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 is a powdery.All the other are with any one embodiment among the embodiment 1-21.
Embodiment 23, a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, wherein: plugging agent 5 is packaged into strip.All the other are with any one embodiment among the embodiment 1-21.
Embodiment 24, a kind of be used for field of polysilicon production prevent silicon liquid leakage current with plugging agent in the application of built-up type plumbago crucible, wherein: a kind of combined type copple, comprise sidewall 4 and base plate 3, it is characterized in that: base plate 3 is provided with groove 1, groove 1 on the base plate 3 adopts the chase mortise fixed mode that cooperatively interacts to splice with the tenon of sidewall 4 bottoms 2, sidewall 4 around be distributed in base plate 3 around; Sidewall 4 surrounds a cavity jointly with base plate 3, is filled with plugging agent 5 in the slit between base plate 3 and the sidewall 4.All the other are with any one embodiment among the embodiment 1-23.
Claims (4)
- One kind be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, it is characterized in that: with the molten silicon liquid generation high temperature ceramic material that reacts rapidly.
- 2. as claimed in claim 1 be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, it is characterized in that: plugging agent (5) comprises reagent and additive composition, weight proportion between reagent and the additive is: reagent 10-100 part, additive 0-90 part; Wherein reagent is any one or two kinds in Mo powder or the C powder, and additive is Si 3N 4, any one or wherein two kinds mixing in SiC, aluminum oxide or the magnesium oxide.
- 3. as claimed in claim 1 a kind of be used for field of polysilicon production prevent silicon liquid leakage current plugging agent, it is characterized in that: can be powdery, also can be packaged into strip.
- One kind be used for field of polysilicon production prevent silicon liquid leakage current with plugging agent in the application of built-up type plumbago crucible, it is characterized in that: a kind of combined type copple, comprise sidewall (4) and base plate (3), base plate (3) is provided with groove (1), the tenon (2) of the groove (1) on the base plate (3) and sidewall (4) bottom adopts the chase mortise fixed mode that cooperatively interacts to splice, sidewall (4) around be distributed in base plate (3) around; Sidewall (4) surrounds a cavity jointly with base plate (3), is filled with plugging agent (5) in the slit between base plate (3) and the sidewall (4).
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| CN2011100050878A CN102220108A (en) | 2011-01-12 | 2011-01-12 | Silicon liquid leakage preventing plugging agent for use in field of production of polycrystalline silicon |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112144118A (en) * | 2020-10-27 | 2020-12-29 | 宜兴市昱元能源装备技术开发有限公司 | Reusable graphite crucible in ingot casting monocrystalline silicon or polycrystalline silicon and use method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112144118A (en) * | 2020-10-27 | 2020-12-29 | 宜兴市昱元能源装备技术开发有限公司 | Reusable graphite crucible in ingot casting monocrystalline silicon or polycrystalline silicon and use method |
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Application publication date: 20111019 |