CN106087047A - A kind of preparation method of foundry alloy - Google Patents
A kind of preparation method of foundry alloy Download PDFInfo
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- CN106087047A CN106087047A CN201610694945.7A CN201610694945A CN106087047A CN 106087047 A CN106087047 A CN 106087047A CN 201610694945 A CN201610694945 A CN 201610694945A CN 106087047 A CN106087047 A CN 106087047A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The invention discloses the preparation method of a kind of foundry alloy, including step: one, prepared by crucible bottom coating, and process is as follows: 101, coating spraying liquid preparation；102, the quantity for spray of coating spraying liquid determines: according to preparing the concentration of boron impurities in mother alloy ingot, and combines the charge of crucible, is determined the quantity for spray of coating spraying liquid；103, spraying: use spraying equipment by coating spraying liquid even application to the inner bottom surface of crucible；104, dry: use drying plant to dry, it is thus achieved that base coat；Two, foundry alloy founding: utilize the crucible of band base coat, carries out founding to preparing mother alloy ingot.The inventive method step is simple, reasonable in design and realization is easy, using effect is good, by coating one layer of base coat with boron nitride as primary raw material in crucible bottom, can effectively reduce crucible bottom oxygen content, and energy is easy, be rapidly completed foundry alloy preparation process, improves the quality of mother alloy ingot.
Description
Technical field
The invention belongs to foundry alloy preparing technical field, especially relate to the preparation method of a kind of foundry alloy.
Background technology
Foundry alloy is exactly the alloy of impurity element and silicon, and conventional foundry alloy has silicon phosphorus and silicon boron two kinds, and impurity concentration is
-2 powers of 10 and-3 powers of 10.Use foundry alloy doping can be made to be easily controlled as adulterant, more accurate, and female close
The purpose of gold doping is used to change donor impurity (such as phosphorus) or the impurity concentration of acceptor impurity (such as boron) in silicon melt so that it is raw
The monocrystalline resistivity grown reaches the requirement of regulation.Silicon material and impurity raw material when producing, need to be loaded stone by the actual foundry alloy that carries out
After English crucible more preheated, fusing (also referred to as melt), crystallize, anneal, the step such as cooling, common vacuum both can have been used to melt
Furnace is processed, it would however also be possible to employ polycrystalline silicon ingot or purifying furnace is processed.But the bottom of the institute of foundry alloy processing at present employing crucible
Sprayed coating is with Si3N4Material is as sprayed on material, because of Si3N4The features such as the heat conductivility of material itself is poor, unstability, make casting
Easily form the oxygen content bottom Hard Inclusion, and ingot casting finished product during ingot higher, the quality of mother alloy ingot product is had
The biggest impact.It addition, Si3N4Although material can be effectively isolated silicon liquid and crucible reaction, but Si3N4React with silicon liquid
Rear formation red sector, is easily introduced impurity Si3N4And form Hard Inclusion, the quality of mother alloy ingot finished product is affected the biggest.
Summary of the invention
The technical problem to be solved is for above-mentioned deficiency of the prior art, it is provided that a kind of foundry alloy
Preparation method, its method step is simple, reasonable in design and realization is easy, using effect is good, by coating one layer in crucible bottom
Base coat with boron nitride as primary raw material, can effectively reduce crucible bottom oxygen content, and energy is easy, be rapidly completed foundry alloy
Preparation process, improves the quality of mother alloy ingot.
For solving above-mentioned technical problem, the technical solution used in the present invention is: the preparation method of a kind of foundry alloy, its feature
Being, the method comprises the following steps:
Prepared by step one, crucible bottom coating, process is as follows:
Step 101, coating spraying liquid are prepared: by organic cementing agent, deionized water and boron nitride by 1: (2～2.5): (0.8
～1.2) mass ratio uniformly mix, obtain coating spraying liquid；
Step 102, the quantity for spray of coating spraying liquid determine: according to preparing the concentration of boron impurities in mother alloy ingot, and
In conjunction with the charge of crucible, the quantity for spray of coating spraying liquid described in step 101 is determined；
Step 103, spraying: according to quantity for spray determined by step 102, use spraying equipment by described in step 101
Coating spraying liquid even application is in the inner bottom surface of crucible；
Described crucible is silica crucible；
Step 104, drying: crucible described in step 103 is placed horizontally in drying plant, and uses described drying to set
Standby and under 80 DEG C～100 DEG C of temperature conditionss, the described coating spraying liquid being sprayed in crucible inner bottom surface is dried, obtain
Obtain base coat；
Step 2, foundry alloy founding: use polycrystalline silicon ingot or purifying furnace or casting furnace, and utilize band base coat in step one
Described need are prepared mother alloy ingot and are carried out founding by crucible.
The preparation method of above-mentioned a kind of foundry alloy, is characterized in that: organic binder bond described in step 101 is phenolic aldehyde-neoprene
Rubber based adhesives, epoxy adhesive, Instant adhesive, acrylic acid adhesive, polyvinyl alcohol adhesive, polyvinyl acetate are gluing
Agent, AE SGA, butvar adhesive stick or glass cement；
Described boron nitride is hexagonal boron nitride.
The preparation method of above-mentioned a kind of foundry alloy, is characterized in that: before step 2 carries out foundry alloy founding, first by founding institute
State and need to prepare the silicon material of mother alloy ingot and load in step one in the crucible of band base coat, then crucible is loaded described polycrystalline
Silicon ingot furnace or described casting furnace；
The charge of crucible described in step 102 is the interior charge loading silicon material of crucible；
Needing to prepare the concentration of boron impurities in mother alloy ingot in step 102 is the mass concentration of boron impurities；To described coating
When the quantity for spray of spray coating liquor is determined, according to preparing the concentration of boron impurities in mother alloy ingot, and combine described need preparation
The quality of mother alloy ingot, is carried out really respectively to needing the quality preparing the silicon material of mother alloy ingot and boron impurities described in founding
Fixed；Need to prepare the quality of mother alloy ingot boron impurities described in founding determined by further according to, and be coated with described in integrating step 101
Organic cementing agent, deionized water and the mass ratio of boron nitride in layer spray coating liquor, to needing described in founding to prepare mother alloy ingot
The quality of described boron nitride is determined；Need to prepare the described boron nitride of mother alloy ingot described in founding determined by further according to
Quality, the quantity for spray of described coating spraying liquid is determined.
The preparation method of above-mentioned a kind of foundry alloy, is characterized in that: crucible described in step one is casting furnace crucible；
When step 2 carries out foundry alloy founding, use described casting furnace, and utilize the earthenware of band base coat in step one
Described need are prepared mother alloy ingot and are carried out founding by crucible；
Described casting furnace is vacuum casting furnace, utilizes the crucible of band base coat in step one that prepared by described need foundry alloy
When ingot casting carries out founding, carry out founding according to the casting method of conventional mother alloy ingot.
The preparation method of above-mentioned a kind of foundry alloy, is characterized in that: crucible described in step one is polycrystalline silicon ingot or purifying furnace crucible；
When step 2 carries out foundry alloy founding, use described polycrystalline silicon ingot or purifying furnace, and utilize painting bottom band in step one
Described need are prepared mother alloy ingot and are carried out founding by the crucible of layer；Mother alloy ingot is prepared by described need when carrying out founding, according to
Conventional polycrystalline silicon ingot casting method carries out founding.
The preparation method of above-mentioned a kind of foundry alloy, is characterized in that: when carrying out foundry alloy founding in step 2, and process is as follows:
Step 201, charging: in step one, in the crucible of band base coat, load silicon material；
Step 202, preheating: use described polycrystalline silicon ingot or purifying furnace that the silicon material being loaded in crucible is preheated, and by described
The heating-up temperature of polycrystalline silicon ingot or purifying furnace steps up to T1；Preheating time is 4h～6h, wherein T1=1125 DEG C～1285 DEG C；
Step 203, fusing: use described polycrystalline silicon ingot or purifying furnace that the silicon material being loaded in crucible is melted, fusion temperature
For T1～T2；Wherein T2=1540 DEG C～1560 DEG C；
After the silicon material in crucible all melts, by the heating and temperature control of described polycrystalline silicon ingot or purifying furnace at T2, institute afterwards
The heating power stating polycrystalline silicon ingot or purifying furnace begins to decline, when the heating power of described polycrystalline silicon ingot or purifying furnace stops declining and continuing
Between after t, fusion process completes；Wherein t=20min～40min；
Step 204, long crystalline substance: be oriented solidifying after the heating-up temperature of described polycrystalline silicon ingot or purifying furnace is gradually decreased to T3 by T2
Gu, until completing long brilliant process；Wherein T3 is polysilicon crystal temperature and T3=1420 DEG C～1440 DEG C；
Step 205, anneal and cool down: after long brilliant process completes in step 205, anneal and cool down, and obtaining processing
The mother alloy ingot of molding.
The preparation method of above-mentioned a kind of foundry alloy, is characterized in that: in step 202 in warm, is cast by described polysilicon
The heating power of ingot stove is stepped up to P1, wherein P1=50kW～100kW；Described in step 203, the silicon material in crucible is whole
After fusing, the heating power situation of change of described polycrystalline silicon ingot or purifying furnace is observed, treats the heating of described polycrystalline silicon ingot or purifying furnace
Power drop is to P2, and keeps P2 constant and after persistent period t, and melt process completes；Wherein, P2=25kW～45kW.
The preparation method of above-mentioned a kind of foundry alloy, is characterized in that: spraying equipment described in step 103 is liquid spray gun, step
Drying plant described in rapid 104 is baking oven.
The preparation method of above-mentioned a kind of foundry alloy, is characterized in that: crucible described in step 102 is cube crucible；Step
Crucible described in 104 and described baking oven are all laid in level；
Described baking oven includes that casing, the bottom heater being laid in crucible bottom and four are laid in four of crucible respectively
The side heater of side-wall outer side, four described side heater are respectively positioned on above bottom heater, described bottom heater in
Level is laid, four described side heater all in vertically to laying；It is provided with on described bottom heater for crucible placement
Graphite cushion block.
The preparation method of above-mentioned a kind of foundry alloy, is characterized in that: when drying in step 104, first uses described drying
Crucible is heated to 80 DEG C～100 DEG C by equipment, then carries out being incubated until the described coating spraying that is sprayed in crucible inner bottom surface
Till liquid is dried.
The present invention compared with prior art has the advantage that
1, method step is simple, reasonable in design and realizes conveniently, it is easy to grasping, input cost is relatively low.
2, the coating material used is by organic cementing agent, deionized water and boron nitride, and cost is relatively low and preparation is easy.
3, the coating material used, using boron nitride as primary raw material, can effectively increase crucible bottom heat-conducting effect, and
Can reduce crucible bottom oxygen content, Simultaneous Stabilization is good, is not easily formed Hard Inclusion during ingot casting, and foundry alloy casting can be effectively ensured
The quality of ingot finished product.
4, the coating material used can effectively reduce the cost of polycrystalline silicon ingot casting, during due to boron originally as mother alloy ingot
A kind of adulterant used, but the cost of pure boron is at a relatively high；And prepare after using the coating material coating disclosed in the present invention
During polysilicon ingot crucible base coat, the doping of pure boron can be reduced, even avoid adding pure boron, it is thus possible to effectively drop
Low mother alloy ingot cost.
5, the painting method used is reasonable in design and realization is easy, using effect is good, can be easy, quickly in crucible bottom
Making one layer of base coat, and the base coat quality made is good, coating procedure is easily controllable.Meanwhile, the baking used
Stem structure is reasonable in design and cost is relatively low, using effect goods, and energy is easy, be rapidly completed the drying course of crucible bottom coating, and
And heats is good, crucible bottom uniform coating thickness and quality that machine-shaping can be effectively ensured are good.
6, mother alloy ingot method is simple and employing well known to a person skilled in the art mother alloy ingot method, it is easy to
Grasp.
7, use during polycrystalline silicon ingot or purifying furnace carries out mother alloy ingot, actual when melting, treat the silicon material in crucible
All after fusing, the heating-up temperature controlling ingot furnace keeps constant, and the time dependent curve of heating power to ingot furnace
(i.e. power curve) is observed；Wherein, after the silicon material in crucible all melts, the power curve of ingot furnace begins to decline,
After the power curve of ingot furnace declines and walks flat 20min～40min, melt process completes, and carries out crystal growing stage afterwards.Actual
In operating process, just can accurately be determined the time point that melt process completes by observed power curve, i.e. be switched by the melting stage
Point switching time to crystal growing stage.Practical operation is easy, and realizes conveniently, can be switched to long crystalline substance by the melting stage by accurate assurance
The switching time in stage.It is to say, the present invention stablizes ingot casting melt curve by extending the melt time, treat that power curve is walked flat
Cut crystal growing stage after 20min～40min again, thus can accurately be melted to the switching time of crystal growing stage, stopped simultaneously by
The problems such as the mother alloy ingot Quality Down that causes in melt deficiency of time or melt overlong time, cost increase.Further, use
After the present invention carries out accurate assurance to melt during mother alloy ingot to long brilliant switching time, can ensure that long brilliant quality and
It is finally made the conversion efficiency of cell piece；Meanwhile, crystal growth quality can be effectively improved, reduce viscous crucible rate, and finished product can be effectively improved
Rate.
8, practical, it is simple to batch production.
In sum, the inventive method step is simple, reasonable in design and realization is easy, using effect is good, by crucible
One layer of base coat with boron nitride as primary raw material of bottom coating, can effectively reduce crucible bottom oxygen content, and can be easy, fast
Speed completes foundry alloy preparation process, improves the quality of mother alloy ingot.
Below by drawings and Examples, technical scheme is described in further detail.
Accompanying drawing explanation
Fig. 1 is the method flow block diagram of the present invention.
Fig. 2 is the structural representation of the crucible of band base coat of the present invention.
Fig. 3 is the structural representation of baking oven of the present invention.
Fig. 4 is the preparation method FB(flow block) of crucible bottom coating of the present invention.
Temperature when Fig. 5 is to use the present invention to melt and power.
Description of reference numerals:
1 crucible；2 base coat；3 bottom heaters；
4 side heater；5 graphite cushion blocks.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of foundry alloy as shown in Figure 1, comprises the following steps:
Prepared by step one, crucible bottom coating, process is as follows:
Step 101, coating spraying liquid prepare: by organic cementing agent, deionized water and boron nitride by 1: 2～2.5: 0.8～
The mass ratio of 1.2 uniformly mixes, and obtains coating spraying liquid；
Step 102, the quantity for spray of coating spraying liquid determine: according to preparing the concentration of boron impurities in mother alloy ingot, and
In conjunction with the charge of crucible 1, the quantity for spray of coating spraying liquid described in step 101 is determined；
Step 103, spraying: according to quantity for spray determined by step 102, use spraying equipment by described in step 101
Coating spraying liquid even application is in the inner bottom surface of crucible 1；
Described crucible 1 is silica crucible；
Step 104, drying: crucible 1 described in step 103 is placed horizontally in drying plant, and uses described drying
Equipment and under 80 DEG C～100 DEG C of temperature conditionss, the described coating spraying liquid being sprayed in crucible 1 inner bottom surface being dried,
Obtain base coat 2, refer to Fig. 2 and Fig. 4；
Step 2, foundry alloy founding: use polycrystalline silicon ingot or purifying furnace or casting furnace, and utilize band base coat 2 in step one
Crucible 1 described need prepared mother alloy ingot carry out founding.
Time actually used, can according to specific needs, to cementing agent organic in coating spraying liquid described in step 101, go from
The mass ratio of sub-water and boron nitride adjusts accordingly.
In the present embodiment, described organic cementing agent is phenolic aldehyde-neoprene adhesive.
Wherein, the kind of phenolic aldehyde-neoprene adhesive is more, mainly include anchor 801 seccotine, hundred glue, JX-
15-1 glue, FN-303 glue, CX-401 glue, XY-401 glue, CH-406 glue etc..Above-mentioned phenolic aldehyde-neoprene adhesive is commercially available
Commodity, can directly obtain.
Time actually used, described organic cementing agent can also be organic silicon adhesive, epoxy adhesive, Instant adhesive,
Acrylic acid adhesive, polyvinyl alcohol adhesive, Polyvinyl acetate adhesive, AE SGA, butvar adhesive are viscous
Agent or glass cement.
Wherein, organic silicon adhesive (also referred to as organosilicon adhesive) point one pack system, bi-component, room temperature vulcanization and heating sulfur
Change etc. multiple, the major product trade mark of room temperature vulcanized has 703,704, FS-203, GD-400 etc..According to solidification temperature, organic
Silica gel stick can be divided into hot setting, low-temperature setting and cold curing three class.Organic silicon adhesive of the present invention is low
Temperature curing organic silicon adhesive.
Epoxy adhesive is Vinylidene Chloride epoxy adhesive or furan modified epoxy adhesive.
Instant adhesive is also referred to as instant glue, and conventional is ethyl α-cyanoacrylate, product designation 502 glue；Medical
Alpha-cyanoacrylate butyl ester, product designation 504 glue.
Acrylic acid adhesive, commercially available kind has SA-200, AB glue, J-39, J-50, SGA-404, SGA etc..
In the present embodiment, described boron nitride is boron nitride powder.
In the present embodiment, described boron nitride is hexagonal boron nitride.
In the present embodiment, spraying equipment described in step 103 is liquid spray gun.
Time actually used, spraying equipment described in step 103 can also be other type of liquid spraying equipment.
In the present embodiment, drying plant described in step 104 is baking oven.
As it is shown on figure 3, crucible 1 described in step 103 is cube crucible；Crucible 1 described in step 104 and described baking oven
All lay in level；
Described baking oven includes casing, be laid in the bottom heater 3 bottom crucible 1 and four be laid in crucible 1 respectively
The side heater 4 of four side-wall outer side, four described side heater 4 are respectively positioned on above bottom heater 3, and described bottom adds
Hot device 3 is laid in level, four described side heater 4 all in vertically to laying；It is provided with on described bottom heater 3 for earthenware
The graphite cushion block 5 that crucible 1 is placed.
In the present embodiment, when step 104 is dried, first use described drying plant that crucible 1 is heated to 90 DEG C, then
Carry out being incubated till the described coating spraying liquid being sprayed in crucible 1 inner bottom surface is dried.
Actual when drying, can adjust accordingly drying temperature according to specific needs.
It is good etc. that boron nitride owing to containing in described base coat has good heat conductivity, good stability, resistance to elevated temperatures
Advantage, can effectively strengthen the heat-conducting effect bottom crucible 1, can be effectively improved melting efficiency, and being difficult to of crucible 1 bottom gas
Get rid of, can effectively reduce the oxygen content bottom crucible 1, make the oxygen content bottom ingot casting finished product reduce.Meanwhile, boron nitride and oxygen exist
Under high temperature, reaction generates B2O3And nitrogen dioxide gas (NO2) etc., the oxygen content bottom crucible 1 can be reduced further, and raw
The B become2O3Compare Si3N4Stable, it is not easily formed Hard Inclusion during ingot casting, thus can effectively reduce the Hard Inclusion of ingot casting finished product, with
Time can be effectively improved the minority carrier life time of ingot casting finished product, the quality of ingot casting finished product can be effectively improved.
In the present embodiment, crucible 1 described in step one is casting furnace crucible；
In the present embodiment, when step 2 carries out foundry alloy founding, use described casting furnace, and utilize in step one at the bottom of band
Described need are prepared mother alloy ingot and are carried out founding by the crucible 1 of portion's coating 2；
Described casting furnace is vacuum casting furnace, utilizes the crucible 1 of band base coat 2 in step one need to prepare female conjunction to described
When gold ingot casting carries out founding, carry out founding according to the casting method of conventional mother alloy ingot.
Further, described vacuum casting furnace is vaccum sensitive stove.
In the present embodiment, before step 2 carries out foundry alloy founding, first prepare mother alloy ingot by needing described in founding
Silicon material loads in step one in the crucible 1 of band base coat 2, then crucible 1 is loaded described casting furnace.
In the present embodiment, the charge of crucible 1 described in step 102 is the interior charge loading silicon material of crucible 1；
Needing to prepare the concentration of boron impurities in mother alloy ingot in step 102 is the mass concentration of boron impurities；To described coating
When the quantity for spray of spray coating liquor is determined, according to preparing the concentration of boron impurities in mother alloy ingot, and combine described need preparation
The quality of mother alloy ingot, is carried out really respectively to needing the quality preparing the silicon material of mother alloy ingot and boron impurities described in founding
Fixed；Need to prepare the quality of mother alloy ingot boron impurities described in founding determined by further according to, and be coated with described in integrating step 101
Organic cementing agent, deionized water and the mass ratio of boron nitride in layer spray coating liquor, to needing described in founding to prepare mother alloy ingot
The quality of described boron nitride is determined；Need to prepare the described boron nitride of mother alloy ingot described in founding determined by further according to
Quality, the quantity for spray of described coating spraying liquid is determined.Wherein,
In the present embodiment, described silicon material is silica flour.
In the present embodiment, compared with conventional crucible, the surface free from admixture of machine-shaping foundry alloy finished product, without viscous crucible phenomenon,
Bottom ingot casting, oxygen content reduces by more than 60%, and minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate is
75%.
Embodiment 2
In the present embodiment, as different from Example 1: crucible 1 described in step one is polycrystalline silicon ingot or purifying furnace crucible；
When step 2 carries out foundry alloy founding, use described polycrystalline silicon ingot or purifying furnace, and utilize painting bottom band in step one
Described need are prepared mother alloy ingot and are carried out founding by the crucible 1 of layer 2；Mother alloy ingot is prepared by described need when carrying out founding, presses
The polycrystalline silicon ingot casting method of more solito carries out founding.
At present, polycrystalline silicon ingot casting method mainly has half casting process and fine melt ingot casting method two kinds, and half casting process is also referred to as
There is seed crystal ingot casting polycrystalline silicon process, refer to use grade silicon material to carry out epitaxial growth as nucleating center, cast low defect Gao Pin
The polycrystalline silicon ingot casting of matter；Fine melt ingot casting method is also referred to as without seed crystal ingot casting polycrystalline silicon process or without seed crystal efficient polycrystalline silicon technology, refers to
Non-silicon material is used to prepare shaggy heterogeneous forming core layer in crucible bottom, during by the roughness of control forming core layer with forming core
Degree of supercooling obtains bigger nucleation rate, casts low defect high-quality polycrystalline silicon ingot casting.At present, polycrystalline silicon ingot casting method is cast with fine melt
Ingot method is main.
Thus, step 2 uses polycrystalline silicon ingot or purifying furnace, and utilizes the crucible 1 of band base coat 2 to carry out ingot casting.And
And, the polycrystalline silicon ingot casting method used is conventional polycrystalline silicon ingot casting method, specially fine melt polycrystalline silicon ingot casting method.
In the present embodiment, before step 2 carries out foundry alloy founding, first prepare mother alloy ingot by needing described in founding
Silicon material loads in step one in the crucible 1 of band base coat 2, then crucible 1 is loaded described polycrystalline silicon ingot or purifying furnace.
In the present embodiment, remaining method step and technological parameter are the most same as in Example 1.
In the present embodiment, compared with conventional crucible, the surface free from admixture of machine-shaping foundry alloy finished product, without viscous crucible phenomenon,
Bottom ingot casting, oxygen content reduces by more than 62%, and minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate is
78%.
Embodiment 3
In the present embodiment, as different from Example 2: when carrying out mother alloy ingot in step 2, process is as follows:
Step 201, charging: in step one, in the crucible 1 of band base coat 2, load silicon material；
Step 202, preheating: use described polycrystalline silicon ingot or purifying furnace that the silicon material being loaded in crucible 1 is preheated, and by described
The heating-up temperature of polycrystalline silicon ingot or purifying furnace steps up to T1；Preheating time is 5h, wherein T1=1200 DEG C；
Step 203, fusing: use described polycrystalline silicon ingot or purifying furnace that the silicon material being loaded in crucible 1 is melted, fusion temperature
For T1～T2；Wherein T2=1550 DEG C；
After the silicon material in crucible 1 all melts, by the heating and temperature control of described polycrystalline silicon ingot or purifying furnace at T2, institute afterwards
The heating power stating polycrystalline silicon ingot or purifying furnace begins to decline, when the heating power of described polycrystalline silicon ingot or purifying furnace stops declining and continuing
Between after t, fusion process completes；Wherein t=30min；
Step 204, long crystalline substance: be oriented solidifying after the heating-up temperature of described polycrystalline silicon ingot or purifying furnace is gradually decreased to T3 by T2
Gu, until completing long brilliant process；Wherein T3 is polysilicon crystal temperature and T3=1430 DEG C；
Step 205, anneal and cool down: after long brilliant process completes in step 205, anneal and cool down, and obtaining processing
The described mother alloy ingot of molding.
In the present embodiment, when step 205 being annealed and cool down, according to the annealing in conventional polysilicon casting ingot method and
Cooling means is annealed and cools down.Further, conventional polysilicon casting ingot method is polysilicon fine melt ingot casting method.
In the present embodiment, described polycrystalline silicon ingot or purifying furnace is G5 type ingot furnace.Further, described polycrystalline silicon ingot or purifying furnace is specially Zhejiang
The G5 type ingot furnace that Jiang Jingsheng electromechanics limited company produces.Described crucible be silica crucible and its be G5 crucible, and raw
The polycrystalline silicon ingot casting that output is come is G5 ingot.
Time actually used, the charge of described silica crucible is about 600kg.
In the present embodiment, the charge of described silica crucible is 560kg.During actually used, can be according to concrete need
Want, the charge of described silica crucible is adjusted accordingly.
Time actually used, in step 203 in fusion process, in described polycrystalline silicon ingot or purifying furnace, it is filled with noble gas and by institute
State polycrystalline silicon ingot or purifying furnace internal gas pressure and be maintained at Q1, wherein Q1=550mbar～650mbar.In the present embodiment, Q1=600mbar.
Actual when melting, can according to specific needs the value size of Q1, T2 and t be adjusted accordingly.
Meanwhile, in step 202 in warm, the heating power of described ingot furnace is stepped up to P1, wherein P1=
50kW～100kW；After the silicon material in crucible all melts described in step 203, the heating power of described ingot furnace is changed feelings
Condition is observed, and treats that the heating power of described ingot furnace drops to P2, and keeps P2 constant and after persistent period t, melt process
Complete；Wherein, P2=25kW～45kW.
Further, when melting in step 203, process is as follows:
1st step, insulation: by the heating and temperature control of described polycrystalline silicon ingot or purifying furnace at T1, and be incubated 0.4h～0.6h；
2nd step to the 5th step, heat up and pressurize: by first to rear point of four step by the heating-up temperature of described polycrystalline silicon ingot or purifying furnace by
T1 is gradually promoted to T4, and the heating-up time is 0.4h～0.6h；Temperature-rise period is filled with indifferent gas in described polycrystalline silicon ingot or purifying furnace
The air pressure of described polycrystalline silicon ingot or purifying furnace is also stepped up to Q1 by body；Wherein, T4=1190 DEG C～1325 DEG C；
6th step, heat up and pressurize for the first time: the heating-up temperature of described polycrystalline silicon ingot or purifying furnace is gradually promoted to by T2 T5 and
Heating-up time is 3.5h～4.5h, and polycrystalline silicon ingot or purifying furnace internal gas pressure described in temperature-rise period is maintained at Q1；Wherein, T5=1440 DEG C
～1460 DEG C；
7th step: second time heat up and pressurize: the heating-up temperature of described polycrystalline silicon ingot or purifying furnace is gradually promoted to by T3 T6 and
Heating-up time is 3.5h～4.5h, and polycrystalline silicon ingot or purifying furnace internal gas pressure described in temperature-rise period is maintained at Q1；Wherein, T6=1490 DEG C
～1510 DEG C；
8th step, third time heat up and pressurize: the heating-up temperature of described polycrystalline silicon ingot or purifying furnace is gradually promoted to by T4 T2 and
Heating-up time is 3.5h～4.5h, and polycrystalline silicon ingot or purifying furnace internal gas pressure described in temperature-rise period is maintained at Q1；Wherein, T2=1540 DEG C
～1560 DEG C；
9th step, insulation: by the heating and temperature control of described polycrystalline silicon ingot or purifying furnace at T2, and be incubated 3.5h～4.5h；Insulation
During, described polycrystalline silicon ingot or purifying furnace internal gas pressure is maintained at Q1；
10th step, persistently insulation: by the heating and temperature control of described polycrystalline silicon ingot or purifying furnace at T2, and be incubated 4h～8h, directly
Silicon material to crucible all melts；In insulating process, described polycrystalline silicon ingot or purifying furnace internal gas pressure is maintained at Q1.
In the present embodiment, the 6th step is carried out heat up for the first time and carry out in pressure maintaining period, in the 7th step second time heat up and
Carry out third time in pressure maintaining period, in the 8th step heat up and pressure maintaining period neutralization the 9th step carries out in insulating process, be both needed to institute
The heating power situation of change stating polycrystalline silicon ingot or purifying furnace is observed, and guarantees the heating power change of described polycrystalline silicon ingot or purifying furnace
Steadily.
Meanwhile, by rear point of four steps by the heating-up temperature of described polycrystalline silicon ingot or purifying furnace by T1 the most gradually in the 2nd step to the 5th step
When being promoted to T3, each step promotes temperature 5 DEG C～8 DEG C, and each step promotes and is both needed to 5min～10min.
Further, in step 202, preheating time is 5h；In warm, by the heating power of described polycrystalline silicon ingot or purifying furnace with
The rate of rise of 10kW/h～15kW/hkW/h steps up to P1.
In the present embodiment, in step 202 in warm, the heating power of described polycrystalline silicon ingot or purifying furnace is stepped up to
P1, wherein P1=75kW.
Actual when preheating, can according to specific needs, to the growth speed of heating power in preheating time, warm
The value size of rate and T1 and P1 adjusts accordingly.
In the present embodiment, after the silicon material in crucible all melts, by the heating and temperature control of described polycrystalline silicon ingot or purifying furnace
At T2, and the time dependent curve of heating power (i.e. power curve) of described polycrystalline silicon ingot or purifying furnace is observed, refers to
Fig. 5.In Fig. 5, fine line is the time dependent curve of heating power of described polycrystalline silicon ingot or purifying furnace, and needing solid line is described polycrystalline
The time dependent curve of heating-up temperature of silicon ingot furnace, vertical line is alarming line when all melting of the silicon material in crucible.By Fig. 5
It can be seen that after the silicon material in crucible all melts, the power curve of described polycrystalline silicon ingot or purifying furnace begins to decline, treat described many
After the power curve of crystal silicon ingot furnace declines and walks flat 30min, melt process completes, and enters crystal growing stage afterwards；In i.e. Fig. 5
The time point that A point completes for melt process.
In actual mechanical process, just can accurately be determined the time point that melt process completes by observed power curve, i.e. by
Melting stage is switched to some switching time of crystal growing stage.Practical operation is easy, and realizes conveniently, and energy accurate assurance is by melting rank
Section is switched to the switching time of crystal growing stage.
In the present embodiment, after described in step 203, the silicon material in crucible all melts, described polycrystalline silicon ingot or purifying furnace is added
Thermal power situation of change is observed, and treats that the heating power of described polycrystalline silicon ingot or purifying furnace drops to P2, and keeps P2 constant and hold
After continuous time t, melt process completes；Wherein, P2=35kW.
Actual when melting, according to the difference of charge in described crucible, the size of P2 is accordingly at 25kW～45kW model
It is adjusted in enclosing.
In the present embodiment, the 1st step is incubated 0.5h；
The heating-up temperature of described polycrystalline silicon ingot or purifying furnace is gradually promoted by T1 by the 2nd step to the 5th step by elder generation to rear point of four steps
To T4, the heating-up time is 0.5h (total time of the i.e. the 2nd step to the 5th step is 0.5h)；To described polycrystalline silicon ingot casting in temperature-rise period
It is filled with noble gas in stove and the air pressure of described polycrystalline silicon ingot or purifying furnace is stepped up to Q1；Wherein, T4=1250 DEG C；
The heating-up temperature of described polycrystalline silicon ingot or purifying furnace is gradually promoted by T1 by the 2nd step to the 5th step by elder generation to rear point of four steps
During to T4, each step promotes temperature 5 DEG C～8 DEG C, and each step promotes and is both needed to 5min～10min；
Carrying out in 6th step heating up for the first time and during pressurize, the heating-up time is 4h, T5=1450 DEG C；
Carrying out second time in 7th step to heat up and during pressurize, the heating-up time is 4h, T6=1500 DEG C.
Carrying out third time in 8th step to heat up and during pressurize, the heating-up time is 4h；
When 9th step is incubated, it is incubated 4h；
When 10th step is persistently incubated, it is incubated 6h, until the silicon material in crucible all melts.
In the present embodiment, the 6th step is carried out heat up for the first time and carry out in pressure maintaining period, in the 7th step second time heat up and
Carry out third time in pressure maintaining period, in the 8th step heat up and pressure maintaining period neutralization the 9th step carries out in insulating process, be both needed to institute
The heating power situation of change stating polycrystalline silicon ingot or purifying furnace is observed, and guarantees the heating power change of described polycrystalline silicon ingot or purifying furnace
Steadily.
During it is to say, the 6th step to the 9th step melts, it is necessary to make power curve steadily advance, it is impossible to occur more
Significantly sags and crests, so can bring increasing of Hard Inclusion.
In the present embodiment, when heating up and pressurize in the 2nd step to the 5th step, process is as follows:
2nd step, the first step promote: by 1200 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1220 DEG C, and heat up
Time is 7min.
3rd step, second step promote: by 1220 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1235 DEG C, and heat up
Time is 8min.
4th step, the 3rd step promote: by 1235 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1242 DEG C, and heat up
Time is 5min.
5th step, the 4th step promote: by 1242 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1250 DEG C, and heat up
Time is 5min.
In the present embodiment, the 10th step being treated, the silicon material in crucible all melts and described polycrystalline silicon ingot or purifying furnace sends " fusing
Complete to report to the police " after, need manual intervention, the decline situation of power curve is observed, treats the power of described polycrystalline silicon ingot or purifying furnace
After curve declines and walks flat 30min, melt process completes, and manual intervention afterwards will be cut into crystal growing stage the melting stage.
In the present embodiment, described noble gas is argon.
In the present embodiment, remaining method step and technological parameter are the most same as in Example 2.
In the present embodiment, compared with conventional crucible, the surface free from admixture of machine-shaping mother alloy ingot finished product, existing without viscous crucible
As, oxygen content reduction by more than 64%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate bottom ingot casting
It is 78%.
Embodiment 4
In the present embodiment, as different from Example 3: in step 202, preheating time is 4h and T1=1285 DEG C, P1=
100kW；In step 203 T2=1560 DEG C, t=20min, P2=45kW, Q1=650mbar；In 1st step, temperature retention time is
0.4h；In 2nd step to the 5th step T4=1325 DEG C, the heating-up time is 0.4h；In 6th step, T5=1460 DEG C and heating-up time are
3.5h；In 7th step, T6=1510 DEG C and heating-up time are 3.5h；In 8th step, the heating-up time is 3.5h；Temperature retention time in 9th step
For 3.5h；In 10th step, temperature retention time is 4h.
In the present embodiment, when heating up and pressurize in the 2nd step to the 5th step, process is as follows:
2nd step, the first step promote: by 1285 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1290 DEG C, and heat up
Time is 5min.
3rd step, second step promote: by 1290 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1295 DEG C, and heat up
Time is 5min.
4th step, the 3rd step promote: by 1295 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1315 DEG C, and heat up
Time is 9min.
5th step, the 4th step promote: by 1315 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1325 DEG C, and heat up
Time is 5min.
In the present embodiment, remaining method step and technological parameter are the most same as in Example 3.
In the present embodiment, compared with conventional crucible, the surface free from admixture of machine-shaping mother alloy ingot finished product, existing without viscous crucible
As, oxygen content reduction by more than 60%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate bottom ingot casting
It is 72%.
Embodiment 5
In the present embodiment, as different from Example 3: in step 202, preheating time is 6h and T1=1125 DEG C, P1=
50kW；In step 203 T2=1540 DEG C, t=40min, P2=25kW, Q1=550mbar；In 1st step, temperature retention time is 0.6h；
In 2nd step to the 5th step T4=1190 DEG C, the heating-up time is 0.6h；In 6th step, T5=1440 DEG C and heating-up time are 4.5h；7th
In step, T6=1490 DEG C and heating-up time are 4.5h；In 8th step, the heating-up time is 4.5h；In 9th step, temperature retention time is 4.5h；The
In 10 steps, temperature retention time is 8h.
In the present embodiment, when heating up and pressurize in the 2nd step to the 5th step, process is as follows:
2nd step, the first step promote: by 1125 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1140 DEG C, and heat up
Time is 9min.
3rd step, second step promote: by 1140 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1155 DEG C, and heat up
Time is 8min.
4th step, the 3rd step promote: by 1155 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1175 DEG C, and heat up
Time is 10min.
5th step, the 4th step promote: by 1175 DEG C, the heating-up temperature of polycrystalline silicon ingot or purifying furnace is promoted to 1190 DEG C, and heat up
Time is 9min.
In the present embodiment, remaining method step and technological parameter are the most same as in Example 3.
In the present embodiment, compared with conventional crucible, the surface free from admixture of machine-shaping mother alloy ingot finished product, existing without viscous crucible
As, oxygen content reduction by more than 65%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate bottom ingot casting
It is 70%.
Embodiment 6
In the present embodiment, as different from Example 3: organic cementing agent, deionized water and boron nitride are pressed by step 101
The mass ratio of 1: 2: 0.8 uniformly mixes, and obtains coating spraying liquid；Described organic cementing agent is organic silicon adhesive；In step 102
When spraying, 1m in described crucible 1 inner bottom surface2The quality of contained boron nitride in the described coating spraying liquid of spraying in region
For 100g；When step 103 is dried, use described drying plant and to being sprayed in crucible 1 under 80 DEG C of temperature conditionss
Described coating spraying liquid on bottom surface, portion is dried, and first uses described drying plant that crucible 1 is heated to 80 DEG C, then enters
Row insulation is till the described coating spraying liquid being sprayed in crucible 1 inner bottom surface is dried.
In the present embodiment, remaining method step and technological parameter are the most same as in Example 3.
In the present embodiment, compared with conventional crucible, the surface free from admixture of machine-shaping mother alloy ingot finished product, existing without viscous crucible
As, oxygen content reduction by more than 64%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate bottom ingot casting
It is 72%.
Embodiment 7
In the present embodiment, as different from Example 3: organic cementing agent, deionized water and boron nitride are pressed by step 101
The mass ratio of 1: 2.5: 0.8 uniformly mixes, and obtains coating spraying liquid；Described organic cementing agent is epoxy adhesive；In step 102
When spraying, 1m in described crucible 1 inner bottom surface2The quality of contained boron nitride in the described coating spraying liquid of spraying in region
For 130g；When step 103 is dried, use described drying plant and to being sprayed in crucible 1 under 100 DEG C of temperature conditionss
Described coating spraying liquid on bottom surface, portion is dried, and first uses described drying plant that crucible 1 is heated to 100 DEG C, then
Carry out being incubated till the described coating spraying liquid being sprayed in crucible 1 inner bottom surface is dried.
In the present embodiment, remaining method step and technological parameter are the most same as in Example 3.
In the present embodiment, compared with conventional crucible, the surface free from admixture of machine-shaping mother alloy ingot finished product, existing without viscous crucible
As, oxygen content reduction by more than 72%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate bottom ingot casting
It is 75%.
Embodiment 8
In the present embodiment, as different from Example 2: organic cementing agent, deionized water and boron nitride are pressed by step 101
The mass ratio of 1: 2.5: 1.2 uniformly mixes, and obtains coating spraying liquid；Described organic cementing agent is Instant adhesive；In step 102
When spraying, 1m in described crucible 1 inner bottom surface2The quality of contained boron nitride in the described coating spraying liquid of spraying in region
For 180g.
In the present embodiment, remaining method step and technological parameter are the most same as in Example 2.
In the present embodiment, compared with conventional crucible, the surface free from admixture of machine-shaping mother alloy ingot finished product, existing without viscous crucible
As, oxygen content reduction by more than 65%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate bottom ingot casting
It is 68%.
Embodiment 9
In the present embodiment, as different from Example 1: organic cementing agent, deionized water and boron nitride are pressed by step 101
The mass ratio of 1: 2: 1.2 uniformly mixes, and obtains coating spraying liquid；Described organic cementing agent is acrylic acid adhesive；In step 102
When spraying, 1m in described crucible 1 inner bottom surface2The quality of contained boron nitride in the described coating spraying liquid of spraying in region
For 200g.
In the present embodiment, remaining method step and technological parameter are the most same as in Example 1.
In the present embodiment, compared with conventional crucible, the surface free from admixture of machine-shaping mother alloy ingot finished product, existing without viscous crucible
As, oxygen content reduction by more than 60%, minority carrier life time ＞ 5.5us (microsecond), Hard Inclusion ratio ＜ 0.5%, yield rate bottom ingot casting
It is 65%.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention, every according to the present invention
Any simple modification, change and the equivalent structure change that above example is made by technical spirit, all still falls within skill of the present invention
In the protection domain of art scheme.
Claims (10)
1. the preparation method of a foundry alloy, it is characterised in that the method comprises the following steps:
Prepared by step one, crucible bottom coating, process is as follows:
Step 101, coating spraying liquid are prepared: by organic cementing agent, deionized water and boron nitride by 1: (2～2.5): (0.8～
1.2) mass ratio uniformly mixes, and obtains coating spraying liquid；
Step 102, the quantity for spray of coating spraying liquid determine: according to preparing the concentration of boron impurities in mother alloy ingot, and combine
The charge of crucible (1), is determined the quantity for spray of coating spraying liquid described in step 101；
Step 103, spraying: according to quantity for spray determined by step 102, use spraying equipment by coating described in step 101
Spray coating liquor even application is in the inner bottom surface of crucible (1)；
Described crucible (1) is silica crucible；
Step 104, drying: crucible described in step 103 (1) is placed horizontally in drying plant, and uses described drying to set
It is standby and under 80 DEG C～100 DEG C of temperature conditionss, the described coating spraying liquid being sprayed in crucible (1) inner bottom surface is dried,
Obtain base coat (2)；
Step 2, foundry alloy founding: use polycrystalline silicon ingot or purifying furnace or casting furnace, and utilize band base coat (2) in step one
Described need are prepared mother alloy ingot and are carried out founding by crucible (1).
2. according to the preparation method of a kind of foundry alloy described in claim 1, it is characterised in that: organic viscous described in step 101
Knot agent be phenolic aldehyde-neoprene adhesive, epoxy adhesive, Instant adhesive, acrylic acid adhesive, polyvinyl alcohol adhesive,
Polyvinyl acetate adhesive, AE SGA, butvar adhesive stick or glass cement；
Described boron nitride is hexagonal boron nitride.
3. according to the preparation method of a kind of foundry alloy described in claim 1 or 2, it is characterised in that: step 2 carries out foundry alloy
Before founding, first the silicon material preparing mother alloy ingot will be needed described in founding to load the crucible of band base coat (2) in step one
(1) in, then crucible (1) is loaded described polycrystalline silicon ingot or purifying furnace or described casting furnace；
The charge of crucible described in step 102 (1) is the interior charge loading silicon material of crucible (1)；
Needing to prepare the concentration of boron impurities in mother alloy ingot in step 102 is the mass concentration of boron impurities；To described coating spraying
When the quantity for spray of liquid is determined, according to preparing the concentration of boron impurities in mother alloy ingot, and combine and described need to prepare female conjunction
The quality of gold ingot casting, is determined respectively to needing the quality preparing the silicon material of mother alloy ingot and boron impurities described in founding；Again
Need to prepare the quality of mother alloy ingot boron impurities, and the spray of coating described in integrating step 101 described in founding determined by according to
The mass ratio of organic cementing agent, deionized water and boron nitride in masking liquid, to needing described in founding to prepare described in mother alloy ingot
The quality of boron nitride is determined；Need to prepare the matter of the described boron nitride of mother alloy ingot described in founding determined by further according to
Amount, is determined the quantity for spray of described coating spraying liquid.
4. according to the preparation method of a kind of foundry alloy described in claim 1 or 2, it is characterised in that: crucible described in step one (1)
For casting furnace crucible；
When step 2 carries out foundry alloy founding, use described casting furnace, and utilize the crucible of band base coat (2) in step one
(1) described need are prepared mother alloy ingot and carry out founding；
Described casting furnace is vacuum casting furnace, utilizes the crucible (1) of band base coat (2) in step one need to prepare female conjunction to described
When gold ingot casting carries out founding, carry out founding according to the casting method of conventional mother alloy ingot.
5. according to the preparation method of a kind of foundry alloy described in claim 1 or 2, it is characterised in that: crucible described in step one (1)
For polycrystalline silicon ingot or purifying furnace crucible；
When step 2 carries out foundry alloy founding, use described polycrystalline silicon ingot or purifying furnace, and utilize band base coat (2) in step one
Crucible (1) described need prepared mother alloy ingot carry out founding；Mother alloy ingot is prepared by described need when carrying out founding, according to
Conventional polycrystalline silicon ingot casting method carries out founding.
6. according to the preparation method of a kind of foundry alloy described in claim 5, it is characterised in that: step 2 carries out foundry alloy and melts
During casting, process is as follows:
Step 201, charging: in step one, in the crucible (1) of band base coat (2), load silicon material；
Step 202, preheating: use described polycrystalline silicon ingot or purifying furnace that the silicon material being loaded in crucible (1) is preheated, and by described many
The heating-up temperature of crystal silicon ingot furnace steps up to T1；Preheating time is 4h～6h, wherein T1=1125 DEG C～1285 DEG C；
Step 203, fusing: using described polycrystalline silicon ingot or purifying furnace to melt the silicon material being loaded in crucible (1), fusion temperature is
T1～T2；Wherein T2=1540 DEG C～1560 DEG C；
After the silicon material in crucible (1) all melts, by the heating and temperature control of described polycrystalline silicon ingot or purifying furnace at T2, described afterwards
The heating power of polycrystalline silicon ingot or purifying furnace begins to decline, and treats that the heating power of described polycrystalline silicon ingot or purifying furnace stops declining and the persistent period
After t, fusion process completes；Wherein t=20min～40min；
Step 204, long crystalline substance: carry out directional solidification after the heating-up temperature of described polycrystalline silicon ingot or purifying furnace is gradually decreased to T3 by T2, directly
To completing long brilliant process；Wherein T3 is polysilicon crystal temperature and T3=1420 DEG C～1440 DEG C；
Step 205, anneal and cool down: after long brilliant process completes in step 205, anneal and cool down, and obtaining machine-shaping
Mother alloy ingot.
7. according to the preparation method of a kind of foundry alloy described in claim 6, it is characterised in that: in step 202 in warm,
The heating power of described polycrystalline silicon ingot or purifying furnace is stepped up to P1, wherein P1=50kW～100kW；Earthenware described in step 203
After silicon material in crucible (1) all melts, the heating power situation of change of described polycrystalline silicon ingot or purifying furnace is observed, treats described many
The heating power of crystal silicon ingot furnace drops to P2, and keeps P2 constant and after persistent period t, and melt process completes；Wherein, P2=
25kW～45kW.
8. according to the preparation method of a kind of foundry alloy described in claim 1 or 2, it is characterised in that: spray described in step 103
Equipment is liquid spray gun, and drying plant described in step 104 is baking oven.
9. according to the preparation method of a kind of foundry alloy described in claim 8, it is characterised in that: crucible described in step 102 (1)
For cube crucible；Crucible described in step 104 (1) and described baking oven are all laid in level；
Described baking oven includes that casing, the bottom heater (3) being laid in crucible (1) bottom and four are laid in crucible (1) respectively
The side heater (4) of four side-wall outer side, four described side heater (4) are respectively positioned on bottom heater (3) top, institute
State bottom heater (3) to lay in level, four described side heater (4) all in vertically to laying；Described bottom heater
(3) the graphite cushion block (5) placed for crucible (1) it is provided with on.
10. according to the preparation method of a kind of foundry alloy described in claim 1 or 2, it is characterised in that: step 104 is dried
Time dry, first use described drying plant that crucible (1) is heated to 80 DEG C～100 DEG C, then carry out being incubated until being sprayed into crucible (1)
Till described coating spraying liquid in inner bottom surface is dried.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112885549A (en) * | 2021-01-08 | 2021-06-01 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11189495A (en) * | 1997-12-26 | 1999-07-13 | Sumitomo Metal Ind Ltd | Silicon single crystal and its production |
| CN202881446U (en) * | 2012-07-16 | 2013-04-17 | 深圳市石金科技有限公司 | Thermal field structure for large-capacity polycrystalline silicon ingot furnace |
| CN103084325A (en) * | 2013-01-31 | 2013-05-08 | 天津英利新能源有限公司 | Crucible and coating method thereof |
| CN103741213A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Melting process for polycrystalline silicon cast ingots |
| CN103741216A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Ingot casting method for purification of silicon powder |
| CN103741215A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Ingot casting method of granular polysilicon |
| CN103741214A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Polycrystalline silicon ingot casting process |
-
2016
- 2016-08-19 CN CN201610694945.7A patent/CN106087047A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11189495A (en) * | 1997-12-26 | 1999-07-13 | Sumitomo Metal Ind Ltd | Silicon single crystal and its production |
| CN202881446U (en) * | 2012-07-16 | 2013-04-17 | 深圳市石金科技有限公司 | Thermal field structure for large-capacity polycrystalline silicon ingot furnace |
| CN103084325A (en) * | 2013-01-31 | 2013-05-08 | 天津英利新能源有限公司 | Crucible and coating method thereof |
| CN103741213A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Melting process for polycrystalline silicon cast ingots |
| CN103741216A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Ingot casting method for purification of silicon powder |
| CN103741215A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Ingot casting method of granular polysilicon |
| CN103741214A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Polycrystalline silicon ingot casting process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112885549A (en) * | 2021-01-08 | 2021-06-01 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
| CN112885549B (en) * | 2021-01-08 | 2022-09-20 | 哈尔滨工业大学 | Preparation method of magnetic phase change material of regenerator of magnetic refrigerator and magnetic refrigeration circulating system |
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Application publication date: 20161109 |