CN103603039A - Purification method for polycrystalline silicon ingot leftovers - Google Patents
Purification method for polycrystalline silicon ingot leftovers Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 95
- 238000000746 purification Methods 0.000 title claims abstract description 66
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 34
- 235000021190 leftovers Nutrition 0.000 title abstract 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 250
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 250
- 239000010703 silicon Substances 0.000 claims abstract description 250
- 230000012010 growth Effects 0.000 claims abstract description 206
- 230000008569 process Effects 0.000 claims abstract description 57
- 238000001816 cooling Methods 0.000 claims abstract description 53
- 238000000137 annealing Methods 0.000 claims abstract description 29
- 238000009413 insulation Methods 0.000 claims description 188
- 238000002844 melting Methods 0.000 abstract description 32
- 230000008018 melting Effects 0.000 abstract description 32
- 239000012535 impurity Substances 0.000 abstract description 15
- 239000002210 silicon-based material Substances 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 11
- 238000010438 heat treatment Methods 0.000 abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 56
- 239000013078 crystal Substances 0.000 description 52
- 239000007789 gas Substances 0.000 description 30
- 229910052786 argon Inorganic materials 0.000 description 28
- 238000010309 melting process Methods 0.000 description 26
- 239000000203 mixture Substances 0.000 description 26
- 229920005591 polysilicon Polymers 0.000 description 19
- 230000003698 anagen phase Effects 0.000 description 18
- 238000011084 recovery Methods 0.000 description 15
- 238000005303 weighing Methods 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 12
- 239000000155 melt Substances 0.000 description 12
- 238000010792 warming Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention provides a purification method for polycrystalline silicon ingot leftovers. The method comprises the following steps: successively heating, melting, growing, annealing and cooling the polycrystalline silicon ingot leftovers, and completing purification of the polycrystalline silicon ingot leftovers. According to the growth process, the growth is divided into first stage growth, second stage growth, third stage growth, fourth stage growth, fifth stage growth, sixth stage growth and seventh stage growth; the first stage growth and the second stage growth are earlier period growth, and the forth growth, the fifth stage growth and the sixth stage growth are later period growth; the earlier period growth temperature is lower than the later period growth temperature. The purification method provided by the invention improves the directional impurity removal effect of the silicon ingots, thereby improving the recyclable silicon material proportion.
Description
Technical field
The present invention relates to field of polysilicon production, relate in particular to a kind of method of purification of polycrystal silicon ingot tankage.
Background technology
Solar energy resources is abundant, both can freely use, and again without transportation, to environment, without any pollution, be a kind of novel renewable energy source.Utilizing the best mode of sun power to utilize exactly photovoltaic material to change solar energy converting by photovoltaic is electric energy.Photovoltaic material conventional in prior art mainly comprises polysilicon, silicon single crystal and non-crystalline silicon etc.Polysilicon is a kind of form of elemental silicon, when the elemental silicon of melting solidifies under crossing cool condition, Siliciumatom is arranged in many nucleus with diamond lattice form, as these nucleus grow up to the different crystal grain of high preferred orientation, these crystal grain combine, and just crystallize into polysilicon.Polysilicon cost is low, saves power consumption, and photoelectric transformation efficiency is high, adopts polysilicon to become main development trend as photovoltaic material.
Polycrystal silicon ingot in use can meet through cutting the needs of actual production conventionally; polycrystal silicon ingot can produce many tankage as rim charge, corner material, liftout and bed material after cutting; these silicon material are understood some and are contained more impurity after cleaning, and do not meet the standard of use.In order to realize the recycling to these tankage, prior art often adopts the production technique of polysilicon to purify to it, makes the impurity that wherein most of impurity is discharged or made to be retained in wherein concentrate distribution, improves the proportion of recyclable silicon material.
Prior art need to be through heating to the purification of silicon material, fusing, growth, annealing and cooling five processes, first polycrystalline silicon material is packed in cated crucible and is placed on oriented solidified blocks, after closing burner hearth, vacuumize, heat, then through 12～13 hours, silicon material is melted completely, silicon material starts to carry out the growth of polysilicon after melting completely, in process of growth, silicon ingot adopts the method growth of directional freeze, be crystal by the bottom oriented growth that makes progress, process of growth is divided into 7 stages, the first growth phase time was 0.5 hour, controlling temperature is 1432 ℃, heat-insulation cage height is 8cm, the second growth phase time was 2.5 hours, and controlling temperature is 1432 ℃, and heat-insulation cage height is 12cm, the 3rd growth phases-time is 6 hours, and controlling temperature is 1432 ℃, and heat-insulation cage height is 14cm, the 4th growth phase time was 1 hour, and controlling temperature is 1430 ℃, and heat-insulation cage height is 15cm, the 5th growth phase time was 5 hours, and controlling temperature is 1426 ℃, and heat-insulation cage height is 16cm, the 6th growth phase time was 9 hours, and controlling temperature is 1420 ℃, and heat-insulation cage height is 16cm, the 7th growth phase time was 2.5 hours, and controlling temperature is 1416 ℃, and heat-insulation cage height is 16cm.Silicon ingot, after these seven growth periods complete, is finally annealed, cooling coming out of the stove.The directed impurities removal effect of the silicon ingot arriving of purifying by prior art is poor, and impurity comparatively disperses is distributed in silicon ingot top, and recyclable silicon material proportion is reduced.
Summary of the invention
The object of the invention is to provide a kind of method of purification of polycrystal silicon ingot tankage.Method provided by the invention can improve the directed impurities removal effect of polycrystal silicon ingot tankage, improves recyclable silicon material proportion.
The method of purification that the invention provides a kind of polycrystal silicon ingot tankage, comprises the following steps:
By polycrystal silicon ingot tankage heat successively, fusing, growth, annealing and cooling, complete the purification to described polycrystal silicon ingot tankage;
According to the process of described growth, described growth be divided into the growth of first stage, the growth of the growth of subordinate phase, phase III, the growth of the growth of fourth stage, five-stage, the growth in the 6th stage and the growth in the 7th stage;
The growth of described first stage and subordinate phase be grown to early growth, the growth of described fourth stage, the growth of five-stage and the 6th stage be grown to late growing stage; The temperature of described early growth is lower than the temperature of described late growing stage.
Preferably, described purification is carried out in polycrystalline silicon ingot or purifying furnace;
Described early growth, in polycrystalline silicon ingot or purifying furnace, heat insulation device height is 7～19cm.
Preferably, the temperature of described early growth is 1405～1415 ℃.
Preferably, described purification is carried out in polycrystalline silicon ingot or purifying furnace;
Described late growing stage, in polycrystalline silicon ingot or purifying furnace, heat insulation device height is 15～23cm.
Preferably, the temperature of described late growing stage is 1409～1425 ℃.
Preferably, the time of described early growth is 2～4 hours.
Preferably, the time of described late growing stage is 10～18 hours.
Preferably, the temperature of the growth of described phase III is 1408～1418 ℃.
Preferably, the temperature of the growth in described the 7th stage is 1410～1420 ℃.
The method of purification that the invention provides a kind of polycrystal silicon ingot tankage, comprises the following steps: by polycrystal silicon ingot tankage heat successively, fusing, growth, annealing and cooling, complete the purification to described polycrystal silicon ingot tankage; According to the process of described growth, described growth be divided into the growth of first stage, the growth of the growth of subordinate phase, phase III, the growth of the growth of fourth stage, five-stage, the growth in the 6th stage and the growth in the 7th stage; The growth of described first stage and subordinate phase be grown to early growth, the growth of described fourth stage, the growth of five-stage and the 6th stage be grown to late growing stage; The temperature of described early growth is lower than the temperature of described late growing stage.Method of purification provided by the invention is by reducing its growth temperature when the early growth of polycrystal silicon ingot tankage, and the brilliant speed of length in polycrystal silicon ingot tankage early stages is improved; When polycrystal silicon ingot tankage late growing stage, improve its growth temperature, the brilliant rate reduction of length in later stage makes to grow, thereby improved the directed impurities removal effect of polycrystal silicon ingot tankage in process of growth, make impurity more concentrated be distributed in silicon ingot top, improved the proportion of recyclable silicon material.Experimental result shows, the silicon ingot that the method for purification by polycrystal silicon ingot tankage provided by the invention obtains reclaims proportion and can reach 81%.
In addition, method of purification provided by the invention has improved the brilliant speed of length in polycrystal silicon ingot tankage early stages, has reduced the brilliant speed of length in later stage, is improving the time that does not extend the cycle of operation of purifying technique when silicon material reclaims proportion.
Embodiment
The method of purification that the invention provides a kind of polycrystal silicon ingot tankage, comprises the following steps:
By polycrystal silicon ingot tankage heat successively, fusing, growth, annealing and cooling, complete the purification to described polycrystal silicon ingot tankage;
According to the process of described growth, described growth be divided into the growth of first stage, the growth of the growth of subordinate phase, phase III, the growth of the growth of fourth stage, five-stage, the growth in the 6th stage and the growth in the 7th stage;
The growth of described first stage and subordinate phase be grown to early growth, the growth of described fourth stage, the growth of five-stage and the 6th stage be grown to late growing stage;
The temperature of described early growth is lower than the temperature of described late growing stage.
Method of purification provided by the invention is by reducing temperature when the early growth of polycrystal silicon ingot tankage, when polycrystal silicon ingot tankage late growing stage, improve temperature, make the brilliant speed raising of length in early stage of polycrystal silicon ingot tankage, the brilliant rate reduction of length in later stage, thereby improved the directed impurities removal effect of polycrystal silicon ingot tankage, make impurity more concentrated be distributed in silicon ingot top, improved the proportion of recyclable silicon material.
The present invention by polycrystal silicon ingot tankage heat successively, fusing, growth, annealing and cooling, complete the purification to described polycrystal silicon ingot tankage.The present invention does not have special restriction to the source of described polycrystal silicon ingot tankage, adopts rim charge, corner material, liftout and bed material that in normal productive process well known to those skilled in the art, silicon ingot produces through cutting.
The present invention does not have special restriction to the method for described heating, adopts the technical scheme heating in polycrystal silicon ingot preparation process well known to those skilled in the art.In the present invention, the temperature of described heating is preferably 20～1300 ℃, more preferably 25～1200 ℃; The time of described heating is preferably 13～16 hours, more preferably 14～15 hours; The present invention preferably heats polycrystal silicon ingot tankage in vacuum environment, and the vacuum tightness in described heat-processed is preferably 0～100Pa, and more preferably 20～80Pa, most preferably is 50Pa.In the process that the present invention preferably heats at described polysilicon tankage, be incubated, the present invention preferably heats described polycrystal silicon ingot tankage in heat insulation device, to realize the insulation to described heat-processed, the present invention does not have special restriction to the kind of described heat insulation device, can bring into play heat insulation effect, in the present invention, described heat insulation device is preferably heat-insulation cage.Described heat insulation device is preferably airtight, to realize the insulation completely to heat-processed.
Complete after described heating, the present invention, by the polysilicon tankage fusing after heating, obtains the polysilicon tankage of melting.The present invention does not have special restriction to described fusing, adopts the technical scheme of preparing the fusing in polysilicon ingot process well known to those skilled in the art.The present invention preferably, under the atmosphere of shielding gas, is melted the polysilicon tankage after described heating; In the present invention, described shielding gas is preferably rare gas element, more preferably argon gas.In the present invention, the pressure of described shielding gas is preferably 0.04～0.07MPa, and in an embodiment of the present invention, the pressure of described shielding gas can be specially 0.04MPa, 0.05MPa, 0.06MPa or 0.07MPa.In the present invention, the temperature of described fusing is preferably 1100～1650 ℃, more preferably 1200～1550 ℃; The time of described fusing is preferably 4～7 hours, more preferably 5～6 hours.The present invention is preferably incubated described polysilicon tankage in the process of fusing, the present invention is preferably melted described polycrystal silicon ingot tankage in heat insulation device, to realize the insulation to described heat-processed, the present invention does not have special restriction to the kind of described heat insulation device, can bring into play heat insulation effect.In the present invention, described heat insulation device is preferably heat-insulation cage, and described heat insulation device is preferably airtight, to realize the insulation completely to melting process.
Obtain after the polycrystal silicon ingot tankage of described melting, the present invention carries out the polycrystal silicon ingot tankage of described melting the growth of crystal, obtains polycrystal silicon ingot crystal.The present invention is preferably dispelled the heat in the polysilicon tankage of described melting carry out the process of crystal growth, and the height that the present invention preferably raises the heat insulation device described in above-mentioned heating and melting technical scheme, dispels the heat to described heat-processed to realize.
According to the process of described growth, described growth be divided into the growth of first stage, the growth of the growth of subordinate phase, phase III, the growth of the growth of fourth stage, five-stage, the growth in the 6th stage and the growth in the 7th stage.In the present invention, the growth of described first stage and subordinate phase be grown to early growth, the time of described early growth is preferably 1～4 hour, more preferably 2～3 hours, most preferably is 2.5 hours; The temperature of described early growth is preferably 1405～1415 ℃, more preferably 1408～1413 ℃, most preferably is 1410 ℃; In described early growth process, described heat insulation device height is preferably 7～19cm, and more preferably 9～18cm, most preferably is 10～16cm.
Concrete, in the present invention, the time of the growth of described first stage is preferably 0.3～1 hour, more preferably 0.4～0.7 hour, most preferably is 0.5 hour; The temperature of the growth of described first stage is preferably 1405～1415 ℃, more preferably 1408～1412 ℃, most preferably is 1410 ℃; In the process of growth of described first stage, the height of described heat insulation device is preferably 7～13cm, and more preferably 8～12cm, most preferably is 10cm;
Complete after the growth of first stage the growth that grows into subordinate phase of polycrystal silicon ingot tankage.In the present invention, the time of the growth of described subordinate phase is preferably 1.7～3 hours, more preferably 1.9～2.5 hours, most preferably be 2 hours, the temperature of the growth of described subordinate phase is preferably 1405～1415 ℃, more preferably 1408～1412 ℃, most preferably is 1410 ℃; In the process of growth of described subordinate phase, the height of described heat insulation device is preferably 13～19cm, and more preferably 15～18cm, most preferably is 16cm;
Complete after the growth of subordinate phase the growth that grows into the phase III of polycrystal silicon ingot tankage.In the present invention, the time of the growth of described phase III is preferably 5～7 hours, more preferably 5.5～6.5 hours, most preferably be 6 hours, the temperature of the growth of described phase III is preferably 1408～1418 ℃, more preferably 1410～1415 ℃, most preferably is 1413 ℃; In the process of growth of described phase III, described heat insulation device height is preferably 13～19cm, and more preferably 15～17cm, most preferably is 16cm;
Complete after the growth of phase III the growth that grows into fourth stage of polycrystal silicon ingot tankage.In the present invention, the growth of described fourth stage, the growth of five-stage and the 6th stage be grown to late growing stage, the time of described late growing stage is preferably 10～18 hours, more preferably 12～16 hours, most preferably is 13 hours.In the present invention, the temperature of described early growth is lower than the temperature of described late growing stage, and the temperature of described late growing stage is preferably 1409～1425 ℃, more preferably 1412～1422 ℃, most preferably is 1414～1420 ℃; In the process of described late growing stage, described heat insulation device height is preferably 15～23cm, and more preferably 17～22cm, most preferably is 18～20cm.
Concrete, in the present invention, the time of the growth of described fourth stage is preferably 0.5～2 hour, more preferably 0.7～1.5 hour, most preferably be 1 hour, the temperature of the growth of described fourth stage is preferably 1409～1419 ℃, more preferably 1410～1418 ℃, most preferably be 1414 ℃; In the process of growth of described fourth stage, the height of described heat insulation device is preferably 15～21cm, and more preferably 16～19cm, most preferably is 18cm;
Complete after the growth of fourth stage the growth that grows into five-stage of polycrystal silicon ingot tankage.In the present invention, the time of the growth of described five-stage is preferably 2～6 hours, more preferably 3～5 hours, most preferably be 4 hours, the temperature of the growth of described five-stage is preferably 1415～1425 ℃, more preferably 1418～1423 ℃, most preferably is 1420 ℃; In the process of growth of described five-stage, the height of described heat insulation device is preferably 17～23cm, and more preferably 18～21cm, most preferably is 20cm;
Complete after the growth of five-stage the growth that grew into for the 6th stage of polycrystal silicon ingot tankage.In the present invention, the time of the growth in described the 6th stage is preferably 7.5～10 hours, more preferably 7.8～9 hours, most preferably be 8 hours, the temperature of the growth in described the 6th stage is preferably 1415～1425 ℃, more preferably 1418～1423 ℃, most preferably is 1420 ℃; In the process of growth in described the 6th stage, the height of described heat insulation device is preferably 17～23cm, and more preferably 18～21cm, most preferably is 20cm;
Complete after the growth in the 6th stage, the growth that grew into for the 7th stage of polycrystal silicon ingot tankage, in the present invention, the time of the growth in described the 7th stage is preferably 2～3 hours, more preferably 2.3～2.8 hours, most preferably be 2.5 hours, the temperature of the growth in described the 7th stage is preferably 1410～1420 ℃, more preferably 1412～1418 ℃, most preferably be 1415 ℃; In the process of growth in described the 7th stage, the height of described heat insulation device is preferably 13～19cm, and more preferably 15～18cm, most preferably is 16cm.
In the present invention, described growth is preferably carried out under shielding gas atmosphere, and described shielding gas is preferably rare gas element, more preferably argon gas.
Complete after the growth of polysilicon tankage, the polycrystal silicon ingot crystal that the present invention obtains growth is annealed.The present invention does not have special restriction to described annealing, adopts the annealing technology scheme of preparing in polysilicon ingot process well known to those skilled in the art.In the present invention, described annealing is preferably carried out under shielding gas atmosphere, and described shielding gas is preferably rare gas element, more preferably argon gas.In the present invention, the temperature of described annealing is preferably 1400～1000 ℃, more preferably 1370～950 ℃; The time of described annealing is preferably 2～10 hours, more preferably 2.5～4 hours, most preferably is 3 hours.
The present invention preferably anneals polycrystal silicon ingot crystal in vacuum environment, and the vacuum tightness in described annealing process is preferably 0～100Pa, and more preferably 20～80Pa, most preferably is 30～60Pa; In the process that the present invention preferably anneals described polycrystal silicon ingot crystal, be incubated, the present invention preferably anneals described polycrystal silicon ingot crystal in heat insulation device, to realize the insulation to described annealing process; In crystal growing process described in technique scheme, on the basis of heat insulation device height, the present invention preferably reduces the height of described heat insulation device, makes it consistent with the height of heat insulation device in heating and melting process described in technique scheme.The present invention does not have special restriction to the kind of described heat insulation device, can bring into play heat insulation effect.In the present invention, described heat insulation device is preferably heat-insulation cage, and described heat insulation device is preferably airtight, to realize the insulation completely to annealing process.
Complete after the annealing of described polycrystal silicon ingot crystal, the present invention carries out the polycrystal silicon ingot crystal after annealing cooling, completes the purification to described polycrystal silicon ingot tankage.The present invention, to the described cooling special restriction that do not have, adopts the cooling technology scheme in purifying polycrystalline silicon ingot technique well known to those skilled in the art.In the present invention, described coolingly preferably carry out under shielding gas atmosphere, described shielding gas is preferably rare gas element, more preferably argon gas; Described cooling temperature is preferably 1000～400 ℃, more preferably 950～350 ℃; The described cooling time is preferably 8～15 hours, more preferably 10～13 hours, most preferably is 11～12 hours.
The present invention preferably carries out being incubated in cooling process at described polysilicon tankage, the present invention preferably carries out cooling by described polycrystal silicon ingot crystal in heat insulation device, to realize the insulation to described process of cooling, the present invention does not have special restriction to the kind of described heat insulation device, can bring into play heat insulation effect, in the present invention, described heat insulation device is preferably heat-insulation cage.Described heat insulation device is preferably airtight, to realize the insulation completely to process of cooling.
The equipment that the present invention adopts described polysilicon tankage purification does not have special restriction, adopts polycrystalline silicon ingot or purifying furnace well known to those skilled in the art; As adopted commercially available model, it is the GT450 type ingot furnace of GT450.
Method of purification provided by the invention is by reducing temperature when the early growth of polycrystal silicon ingot tankage, when polycrystal silicon ingot tankage late growing stage, improve temperature, make the brilliant speed raising of length in early stage of polycrystal silicon ingot tankage, the brilliant rate reduction of length in later stage, thereby improved the directed impurities removal effect of polycrystal silicon ingot tankage, make impurity more concentrated be distributed in silicon ingot top, improved the proportion of recyclable silicon material.
In order to further illustrate the present invention, below in conjunction with embodiment, the method for purification of polycrystal silicon ingot tankage provided by the invention is described in detail, but they can not be interpreted as to limiting the scope of the present invention.
Embodiment 1
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1410 ℃, and heat-insulation cage altitude mixture control, to 10cm, maintains 1410 ℃ by temperature after 0.5 hour, and heat-insulation cage height rises to 16cm, continued growth 2 hours; Then temperature is adjusted to 1413 ℃, heat-insulation cage height dimension is held in 16cm, after 6 hours, temperature is adjusted to 1414 ℃, regulate heat-insulation cage height value 18cm, maintain 1 hour, then temperature is adjusted to 1420 ℃, heat-insulation cage altitude mixture control is to 20cm, and continued growth 4 hours, maintains 1420 ℃ by temperature, heat-insulation cage height dimension is held in 20cm, after 8 hours, adjust the temperature to 1415 ℃, heat-insulation cage height is down to 16cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the present embodiment polycrystal silicon ingot tankage is 75.6%
Embodiment 2
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1405 ℃, and heat-insulation cage altitude mixture control, to 7cm, maintains 1405 ℃ by temperature after 0.3 hour, and heat-insulation cage height rises to 13cm, continued growth 1.7 hours; Then temperature is adjusted to 1413 ℃, heat-insulation cage height dimension is held in 16cm, after 6 hours, temperature is adjusted to 1414 ℃, regulate heat-insulation cage height value 18cm, maintain 1 hour, then temperature is adjusted to 1420 ℃, heat-insulation cage altitude mixture control is to 20cm, and continued growth 4 hours, maintains 1420 ℃ by temperature, heat-insulation cage height dimension is held in 20cm, after 8 hours, adjust the temperature to 1415 ℃, heat-insulation cage height is down to 16cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the present embodiment polycrystal silicon ingot tankage is 77.4%.
Embodiment 3
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1415 ℃, and heat-insulation cage altitude mixture control, to 13cm, maintains 1415 ℃ by temperature after 1 hour, and heat-insulation cage height rises to 19cm, continued growth 3 hours; Then temperature is adjusted to 1413 ℃, heat-insulation cage height dimension is held in 16cm, after 6 hours, temperature is adjusted to 1414 ℃, regulate heat-insulation cage height value 18cm, maintain 1 hour, then temperature is adjusted to 1420 ℃, heat-insulation cage altitude mixture control is to 20cm, and continued growth 4 hours, maintains 1420 ℃ by temperature, heat-insulation cage height dimension is held in 20cm, after 8 hours, adjust the temperature to 1415 ℃, heat-insulation cage height is down to 16cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the present embodiment polycrystal silicon ingot tankage is 73.8%.
Embodiment 4
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1410 ℃, and heat-insulation cage altitude mixture control, to 10cm, maintains 1410 ℃ by temperature after 0.5 hour, and heat-insulation cage height rises to 16cm, continued growth 2 hours; Then temperature is adjusted to 1409 ℃, heat-insulation cage altitude mixture control, to 13cm, is adjusted to 1414 ℃ by temperature after 6 hours, regulate heat-insulation cage height value 18cm, maintain 0.5 hour, then temperature is adjusted to 1420 ℃, heat-insulation cage altitude mixture control is to 20cm, and continued growth 2 hours, maintains 1420 ℃ by temperature, heat-insulation cage height dimension is held in 20cm, after 7.5 hours, adjust the temperature to 1415 ℃, heat-insulation cage height is down to 16cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the present embodiment polycrystal silicon ingot tankage is 74.6%.
Embodiment 5
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1410 ℃, and heat-insulation cage altitude mixture control, to 10cm, maintains 1410 ℃ by temperature after 0.5 hour, and heat-insulation cage height rises to 16cm, continued growth 2 hours; Then temperature is adjusted to 1418 ℃, heat-insulation cage altitude mixture control, to 19cm, is adjusted to 1414 ℃ by temperature after 6 hours, regulate heat-insulation cage height value 18cm, maintain 2 hours, then temperature is adjusted to 1420 ℃, heat-insulation cage altitude mixture control is to 20cm, and continued growth 6 hours, maintains 1420 ℃ by temperature, heat-insulation cage height dimension is held in 20cm, after 10 hours, adjust the temperature to 1415 ℃, heat-insulation cage height is down to 16cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the present embodiment polycrystal silicon ingot tankage is 75.9%.
Embodiment 6
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1410 ℃, and heat-insulation cage altitude mixture control, to 10cm, maintains 1410 ℃ by temperature after 0.5 hour, and heat-insulation cage height rises to 16cm, continued growth 2 hours; Then temperature is adjusted to 1413 ℃, heat-insulation cage height dimension is held in 16cm, after 6 hours, temperature is adjusted to 1409 ℃, regulate heat-insulation cage height value 15cm, maintain 1 hour, then temperature is adjusted to 1420 ℃, heat-insulation cage altitude mixture control is to 20cm, and continued growth 4 hours, maintains 1420 ℃ by temperature, heat-insulation cage height dimension is held in 20cm, after 8 hours, adjust the temperature to 1415 ℃, heat-insulation cage height is down to 16cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the present embodiment polycrystal silicon ingot tankage is 76.7%.
Embodiment 7
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1410 ℃, and heat-insulation cage altitude mixture control, to 10cm, maintains 1410 ℃ by temperature after 0.5 hour, and heat-insulation cage height rises to 16cm, continued growth 2 hours; Then temperature is adjusted to 1413 ℃, heat-insulation cage height dimension is held in 16cm, after 6 hours, temperature is adjusted to 1419 ℃, regulate heat-insulation cage height value 21cm, maintain 1 hour, then temperature is adjusted to 1420 ℃, heat-insulation cage altitude mixture control is to 20cm, and continued growth 4 hours, maintains 1420 ℃ by temperature, heat-insulation cage height dimension is held in 20cm, after 8 hours, adjust the temperature to 1415 ℃, heat-insulation cage height is down to 16cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the present embodiment polycrystal silicon ingot tankage is 78.9%.
Embodiment 8
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1410 ℃, and heat-insulation cage altitude mixture control, to 10cm, maintains 1410 ℃ by temperature after 0.5 hour, and heat-insulation cage height rises to 16cm, continued growth 2 hours; Then temperature is adjusted to 1413 ℃, heat-insulation cage height dimension is held in 16cm, after 6 hours, temperature is adjusted to 1414 ℃, regulate heat-insulation cage height value 18cm, maintain 1 hour, then temperature is adjusted to 1415 ℃, heat-insulation cage altitude mixture control is to 17cm, and continued growth 4 hours, maintains 1415 ℃ by temperature, heat-insulation cage height dimension is held in 17cm, after 8 hours, adjust the temperature to 1415 ℃, heat-insulation cage height is down to 16cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the present embodiment polycrystal silicon ingot tankage is 79.6%.
Embodiment 9
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1410 ℃, and heat-insulation cage altitude mixture control, to 10cm, maintains 1410 ℃ by temperature after 0.5 hour, and heat-insulation cage height rises to 16cm, continued growth 2 hours; Then temperature is adjusted to 1413 ℃, heat-insulation cage height dimension is held in 16cm, after 6 hours, temperature is adjusted to 1414 ℃, regulate heat-insulation cage height value 18cm, maintain 1 hour, then temperature is adjusted to 1425 ℃, heat-insulation cage altitude mixture control is to 23cm, and continued growth 4 hours, maintains 1425 ℃ by temperature, heat-insulation cage height dimension is held in 23cm, after 8 hours, adjust the temperature to 1415 ℃, heat-insulation cage height is down to 16cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the present embodiment polycrystal silicon ingot tankage is 80.5%.
Embodiment 10
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1410 ℃, and heat-insulation cage altitude mixture control, to 10cm, maintains 1410 ℃ by temperature after 0.5 hour, and heat-insulation cage height rises to 16cm, continued growth 2 hours; Then temperature is adjusted to 1413 ℃, heat-insulation cage height dimension is held in 16cm, after 6 hours, temperature is adjusted to 1414 ℃, regulate heat-insulation cage height value 18cm, maintain 1 hour, then temperature is adjusted to 1420 ℃, heat-insulation cage altitude mixture control is to 20cm, and continued growth 4 hours, maintains 1420 ℃ by temperature, heat-insulation cage height dimension is held in 20cm, after 8 hours, adjust the temperature to 1410 ℃, heat-insulation cage height is down to 13cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the polycrystal silicon ingot tankage of the present embodiment is 76.3%.
Embodiment 11
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1410 ℃, and heat-insulation cage altitude mixture control, to 10cm, maintains 1410 ℃ by temperature after 0.5 hour, and heat-insulation cage height rises to 16cm, continued growth 2 hours; Then temperature is adjusted to 1413 ℃, heat-insulation cage height dimension is held in 16cm, after 6 hours, temperature is adjusted to 1414 ℃, regulate heat-insulation cage height value 18cm, maintain 1 hour, then temperature is adjusted to 1420 ℃, heat-insulation cage altitude mixture control is to 20cm, and continued growth 4 hours, maintains 1420 ℃ by temperature, heat-insulation cage height dimension is held in 20cm, after 8 hours, adjust the temperature to 1420 ℃, heat-insulation cage height is down to 19cm, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal;
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the polycrystal silicon ingot tankage of the present embodiment is 75.7%.
Embodiment 12
Adopt with the technique polycrystal silicon ingot tankage of embodiment 1 same principle and purify, different, the present embodiment adopts GT800 type ingot furnace to replace the GT450 type ingot furnace in embodiment 1.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the polycrystal silicon ingot tankage of the present embodiment is 78.3%
Embodiment 13
Adopt with the technique of embodiment 1 same principle polycrystal silicon ingot tankage are purified, different, the present embodiment adopts smart merit 500N type ingot furnace to replace the GT450 type ingot furnace in embodiment 1.
The check of weighing of the polycrystal silicon ingot crystal of the present invention after to the purification obtaining, result shows, the recovery proportion of the polycrystal silicon ingot tankage of the present embodiment is 81%
Comparative example
After the polycrystal silicon ingot of normally producing is cut according to user demand, obtain polycrystal silicon ingot tankage.
420g polycrystal silicon ingot tankage are heated in GT450 type ingot furnace, vacuum tightness is 50Pa, temperature is 1200 ℃, and in heat-processed, heat-insulation cage is air-tight state, heats after 15 hours, polycrystal silicon ingot tankage start fusing, continue to be warming up to 1550 ℃, vacuum tightness is adjusted to 0.06MPa, melting process is incubated and passes into argon gas completely, melting process heat-insulation cage is air-tight state, melts the polycrystal silicon ingot tankage that obtain melting after 5 hours;
Obtain after the polycrystal silicon ingot tankage of melting, polycrystal silicon ingot tankage enter growth phase, cool the temperature to 1432 ℃, and heat-insulation cage altitude mixture control, to 8cm, rises to 12cm by heat-insulation cage height after 0.5 hour, temperature continued growth 2.5 hours; Then heat-insulation cage height is risen to 14cm, temperature maintains 1432 ℃, after 6 hours, temperature is adjusted to 1430 ℃, regulate heat-insulation cage height value 15cm, maintain 1 hour, then temperature is adjusted to 1426 ℃, heat-insulation cage altitude mixture control is to 16cm, and continued growth 5 hours, maintains heat-insulation cage height constant, cool the temperature to 1420 ℃, after 9 hours, adjust the temperature to 1416 ℃, heat-insulation cage height is constant, keeps 2.5 hours, complete the growth of polycrystal silicon ingot, obtain polycrystal silicon ingot crystal.
After growth, temperature is down to 1000 ℃ gradually; anneal; in annealing process, heat-insulation cage is air-tight state; vacuum tightness is 44Pa; anneal, after 3.5 hours, temperature is down to 400 ℃ gradually, the polycrystal silicon ingot growing into is carried out under argon shield cooling, in process of cooling, heat-insulation cage is air-tight state; after cooling 11.5 hours, complete the purification to polycrystal silicon ingot tankage, the polycrystal silicon ingot crystal after being purified.
The check of weighing of the polycrystal silicon ingot of the present invention after to the purification obtaining, result shows, the recovery proportion of the polycrystal silicon ingot tankage of this comparative example is 65.7%
By above embodiment and comparative example, can be found out, the method for purification technique of polycrystal silicon ingot tankage provided by the invention is simple.Adopt method of purification provided by the invention to purify to polycrystal silicon ingot tankage, the recovery proportion of polycrystal silicon ingot tankage has reached 81%, adopts prior art to purify to polycrystal silicon ingot tankage, and reclaiming proportion only has 65.7%.Method of purification provided by the invention has improved the directed impurities removal effect of silicon ingot, make impurity more concentrated be distributed in silicon ingot top, improved the proportion of recyclable silicon material.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (9)
1. a method of purification for polycrystal silicon ingot tankage, comprises the following steps: by polycrystal silicon ingot tankage heat successively, fusing, growth, annealing and cooling, complete the purification to described polycrystal silicon ingot tankage; According to the process of described growth, described growth be divided into the growth of first stage, the growth of the growth of subordinate phase, phase III, the growth of the growth of fourth stage, five-stage, the growth in the 6th stage and the growth in the 7th stage; The growth of described first stage and subordinate phase be grown to early growth, the growth of described fourth stage, the growth of five-stage and the 6th stage be grown to late growing stage; It is characterized in that,
The temperature of described early growth is lower than the temperature of described late growing stage.
2. method of purification according to claim 1, is characterized in that, described purification is carried out in polycrystalline silicon ingot or purifying furnace;
Described early growth, in polycrystalline silicon ingot or purifying furnace, heat insulation device height is 7～19cm.
3. method of purification according to claim 1, is characterized in that, the temperature of described early growth is 1405～1415 ℃.
4. method of purification according to claim 1, is characterized in that, described purification is carried out in polycrystalline silicon ingot or purifying furnace;
Described late growing stage, in polycrystalline silicon ingot or purifying furnace, heat insulation device height is 15～23cm.
5. method of purification according to claim 1, is characterized in that, the temperature of described late growing stage is 1409～1425 ℃.
6. method of purification according to claim 1, is characterized in that, the time of described early growth is 2～4 hours.
7. method of purification according to claim 1, is characterized in that, the time of described late growing stage is 10～18 hours.
8. method of purification according to claim 1, is characterized in that, the temperature of the growth of described phase III is 1408～1418 ℃.
9. method of purification according to claim 1, is characterized in that, the temperature of the growth in described the 7th stage is 1410～1420 ℃.
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| CN101545135A (en) * | 2009-05-11 | 2009-09-30 | 浙江碧晶科技有限公司 | Preparation and purification method of solar grade silicon crystal |
| CN102134075A (en) * | 2011-01-24 | 2011-07-27 | 云南乾元光能产业有限公司 | Novel method for producing solar-grade polysilicon |
| US20120164054A1 (en) * | 2009-01-08 | 2012-06-28 | Bp Corporation North America Inc. | Impurity Reducing Process and Purified Material |
| CN103014848A (en) * | 2011-09-22 | 2013-04-03 | 吴江亿泰光伏设备有限公司 | Polysilicon purification ingot casting furnace control system |
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| US20120164054A1 (en) * | 2009-01-08 | 2012-06-28 | Bp Corporation North America Inc. | Impurity Reducing Process and Purified Material |
| CN101545135A (en) * | 2009-05-11 | 2009-09-30 | 浙江碧晶科技有限公司 | Preparation and purification method of solar grade silicon crystal |
| CN102134075A (en) * | 2011-01-24 | 2011-07-27 | 云南乾元光能产业有限公司 | Novel method for producing solar-grade polysilicon |
| CN103014848A (en) * | 2011-09-22 | 2013-04-03 | 吴江亿泰光伏设备有限公司 | Polysilicon purification ingot casting furnace control system |
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| CN105887190A (en) * | 2016-04-20 | 2016-08-24 | 佳科太阳能硅(龙岩)有限公司 | Method for purifying and recovering gallium-doped ingot top materials |
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