CN107523868A - Boron foundry alloy preparation method - Google Patents
Boron foundry alloy preparation method Download PDFInfo
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- CN107523868A CN107523868A CN201710592840.5A CN201710592840A CN107523868A CN 107523868 A CN107523868 A CN 107523868A CN 201710592840 A CN201710592840 A CN 201710592840A CN 107523868 A CN107523868 A CN 107523868A
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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
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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Abstract
A kind of boron foundry alloy preparation method, including：The selection industrial silicon raw material same or like with boron element concentration in target boron foundry alloy rod, and the summation of metallic element concentration is not higher than 1000ppmw in the industrial silicon raw material；The industrial silicon raw material is prepared into boron foundry alloy rod using vertical pulling method；Clip shouldering part and the epilog portion of the boron foundry alloy rod, the resistivity of the remaining boron foundry alloy rod is divided into by multiple gears according to fractional condensation principle, and the boron foundry alloy rod is cut into by bulk according to resistivity gear, obtain the boron foundry alloy block of multiple resistivity gears；Measure the actual resistivity of the boron foundry alloy block of each resistivity gear；The boron foundry alloy block of each resistivity gear is broken into graininess respectively, and separately packed according to resistivity gear.
Description
Technical field
The present invention relates to photovoltaic material prepared technology field, more particularly to a kind of boron foundry alloy preparation method.
Background technology
With developing rapidly for new energy technology, the research and development of photovoltaic cell are increasingly valued by people.Monocrystal silicon
Or polycrystal silicon ingot is the important component in photovoltaic cell.P-type polysilicon, standard (class) monocrystalline silicon used in photovoltaic cell is being cast
Need to carry out resistivity compensation deals to silicon material in ingot or pulling process, make casting polycrystal silicon ingot, standard (class) monocrystal silicon resistance
Rate control makes photovoltaic cell in 0.5 Ω cm to 6 Ω cm with suitable.
Foundry alloy is a kind of by refining, and composition is accurately used for the alloy material cast.It is as the mother metal cast, tool
There is a very strong hereditary property, many characteristics of foundry alloy, such as grain size, microcosmic mirror image tissue, or even including mechanics, electric property
Characteristic etc. many influence casting product qualities can entail casting after being poured into a mould by remelting, and in photovoltaic industry, boron is female to be closed
Gold is widely used in the control of polycrystal silicon ingot, standard (class) monocrystal silicon resistivity.Select the dopant of suitable resistivity can be with
Improve the debugging speed of resistivity in silicon ingot manufacturing process.Such as the silicon ingot of solar level is made, the resistivity of dopant is general
From the boron foundry alloy of low-resistivity.
Existing boron foundry alloy mainly draws boron foundry alloy by single crystal growing furnace, and its synthesis material selected is more than 6N level
HIGH-PURITY SILICON and high purity boron powder, material purity is high, and cost is high.And draw obtained boron foundry alloy rod and directly carry out broken packing
Dopant as silicon ingot uses, and influences the debugging efficiency of silicon ingot resistivity.
The content of the invention
In view of above-mentioned condition, it is necessary to in the prior art by single crystal growing furnace draw boron foundry alloy rod cost it is high and
A kind of the problem of debugging efficiency of the directly broken influence silicon ingot resistivity of boron foundry alloy rod, there is provided boron foundry alloy preparation method.
A kind of boron foundry alloy preparation method, including：
The selection industrial silicon raw material same or like with boron element concentration in target boron foundry alloy rod, and the industrial silicon raw material
The summation of middle metallic element concentration is not higher than 1000ppmw；
The industrial silicon raw material is pre-processed, the pretreated industrial silicon raw material is loaded to the stone of monocrystalline equipment
Material is carried out in English crucible, when the industrial silicon raw material in silica crucible is melted to Φ 200mm~Φ 300mm, is dropped
Temperature, and carry slag；When the liquid level after carrying slag starts crystallization, it is scaling-off to carry out secondary crystallization；Described in after secondary crystallization is scaling-off
Industrial silicon raw material obtains boron foundry alloy rod after seeding, shouldering, isometrical, ending process；
Shouldering part and the epilog portion of the boron foundry alloy rod are clipped, is closed the remaining boron mother according to fractional condensation principle
The resistivity of golden rod is divided into multiple gears, and the boron foundry alloy rod is cut into bulk according to resistivity gear, obtains multiple
The boron foundry alloy block of resistivity gear；
Measure the actual resistivity of the boron foundry alloy block of each resistivity gear；
The boron foundry alloy block of each resistivity gear is broken into graininess respectively, and separately carried out according to resistivity gear
Packing.
Above-mentioned boron foundry alloy preparation method, wherein, it is described that the pretreated industrial silicon raw material is loaded into monocrystalline equipment
Silica crucible in carry out material, when the industrial silicon raw material in silica crucible is melted to Φ 200mm~Φ 300mm, enter
Row cooling, and carry slag；When the liquid level after carrying slag starts crystallization, carrying out the scaling-off step of secondary crystallization includes：
Pretreated industrial silicon raw material is fitted into the silica crucible of monocrystalline equipment, vacuumizes and detects leakage rate, stove
Interior vacuum is 5~8pa, and leakage rate is no more than 5pa/5min；Heater, power is improved once for every 8~12 minutes, from
Initial power 15kw is gradually risen to 90-95kw, the temperature of industrial silicon raw material is reached 1500~1600 DEG C, and start to melt；
When the industrial silicon raw material in silica crucible is melted to Φ 200mm~Φ 300mm, heater power is down to 20~30kw, entered
Row once carries slag；When liquid level starts crystallization, heater power is increased to 70~75kw, it is scaling-off to carry out secondary crystallization.
Above-mentioned boron foundry alloy preparation method, wherein, described the step of being pre-processed to the industrial silicon raw material, includes：
Industrial silicon raw material is pre-processed, pure water cleaning is crossed after cleaning 0.5~2min with nitration mixture, then by being cleaned by ultrasonic
After dry.
Above-mentioned boron foundry alloy preparation method, wherein, during preparing the boron foundry alloy rod, furnace pressure is kept in single crystal growing furnace
8-15T, 30-60slpm of argon flow amount, brilliant turn of 6-12rpm/min, crucible turn 4-10rpm/rpm, 6-9 cun of crystalline size.
Above-mentioned boron foundry alloy preparation method, wherein, according to fractional condensation principle by the institute after clipping shouldering part and epilog portion
The resistivity for stating boron foundry alloy rod is divided into 12~16 gears, the length of the boron foundry alloy block of each resistivity gear for 20~
200mm。
Above-mentioned boron foundry alloy preparation method, wherein, the model of the ratio of the resistivity of the boron foundry alloy club head and afterbody
Enclose for 1.5~3.
Above-mentioned boron foundry alloy preparation method, wherein, it is described to be respectively broken into the boron foundry alloy block of each resistivity gear
Granular step includes：
The boron foundry alloy block of each resistivity gear is broken into less than 30*30mm particles.
Above-mentioned boron foundry alloy preparation method, wherein, the position of blocking of the shouldering part is the boron foundry alloy club head
Just starting isometrical position, the epilog portion blocks position in the upward 50mm of boron foundry alloy rod epilog portion position
Put.
The embodiment of the present invention directly prepares boron mother's synthetic rod with industrial silicon raw material, reduces production cost, and according to fractional condensation
The resistivity of boron foundry alloy rod is divided into multiple gears by raw material, and will make obtained boron foundry alloy rod sanction according to resistivity gear
Multiple boron foundry alloy blocks are cut into, and measure the actual resistivity of the boron foundry alloy block of each electronics rate gear.It is each by what is cut
The boron foundry alloy block of resistivity gear is broken for boron foundry alloy particle and packed.Suitable resistivity is selected when needing to prepare silicon ingot
Boron foundry alloy particle used as dopant, desired value is quickly transferred to the resistivity of silicon ingot.
Brief description of the drawings
Fig. 1 is the flow chart of the boron foundry alloy preparation method in the embodiment of the present invention one；
Fig. 2 is the schematic diagram of boron foundry alloy rod；
Fig. 3 is the schematic diagram of the Resistivity testing point of boron foundry alloy block.
Embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings, wherein from beginning to end
Same or similar label represents same or similar element or the element with same or like function.Below with reference to attached
The embodiment of figure description is exemplary, is only used for explaining the present invention, and is not considered as limiting the invention.
With reference to following description and accompanying drawing, it will be clear that these and other aspects of embodiments of the invention.In these descriptions
In accompanying drawing, some particular implementations in embodiments of the invention are specifically disclosed, to represent to implement the implementation of the present invention
Some modes of the principle of example, but it is to be understood that the scope of embodiments of the invention is not limited.On the contrary, the present invention
Embodiment includes all changes, modification and the equivalent fallen into the range of the spirit and intension of attached claims.
Embodiment one
Fig. 1 is referred to as the kind boron foundry alloy preparation method in the embodiment of the present invention, including step S1~S6.
Step S11, the selection industrial silicon raw material same or like with boron element concentration in target boron foundry alloy, and the industry
The summation of metallic element concentration is not higher than 1000ppmw in silicon raw material.
The industrial silicon raw material same or like with boron element concentration in target boron foundry alloy rod is used in the present embodiment, and should
The summation of metallic element concentration is not higher than 1000ppmw in industrial silicon raw material, and cost is low.The industrial silicon raw material selected in the present invention
It is required that the single impurity content ＜ 10 such as impurity element gallium, phosphorus, arsenic3atoms/cm3.
The concentration of boron element in target boron foundry alloy rod can be calculated according to following formula：
Wherein, ρ is resistivity, and Ω .cm, N are boron element concentration, cm-3。
, it is necessary to the boron foundry alloy rod of production, i.e., the electricity of the head of boron foundry alloy rod and afterbody described in target in the present embodiment
The scope of the ratio of resistance rate is 1.5~3.When the boron element concentration in the industrial silicon raw material is less than the target boron foundry alloy rod
, can appropriate boron make-up powder during middle boron element concentration.According to the resistivity of the industrial silicon raw material and the mesh of target boron foundry alloy rod
Mark resistivity calculates the weight for the boron powder that need to be supplemented, and target foundry alloy resistivity is the resistivity of boron foundry alloy club head.It is sharp again
The mixture of the industrial silicon raw material and the boron powder of the weight is prepared into boron foundry alloy rod with vertical pulling method.
Step S12, boron foundry alloy rod is prepared using the industrial silicon raw material.Mainly comprise the following steps：To the industry
Silicon raw material is pre-processed, and the pretreated industrial silicon raw material is fitted into the silica crucible of monocrystalline equipment and carries out material,
When the industrial silicon raw material in silica crucible is melted to Φ 200mm~Φ 300mm, cooled, and carry slag；After slag is carried
Liquid level start crystallization when, carry out secondary crystallization it is scaling-off；The industrial silicon raw material after secondary crystallization is scaling-off by seeding,
Boron foundry alloy rod is obtained after shouldering, isometrical, ending process.
Vertical pulling method draws boron foundry alloy rod and carried out typically in single crystal growing furnace, and vertical pulling hair of the prior art mainly includes changing
Material, seeding, shouldering, turn shoulder, be isometrical, blowing out, taking this 7 big process of rod, realizing the self-produced of boron foundry alloy.Certainly in the previous of material
As need furnace chamber and polysilicon, alloy, seed crystal and silica crucible of single crystal growing furnace etc. carry out cleaning treatment.
In the present embodiment, boron foundry alloy rod is directly drawn in single crystal growing furnace using industrial silicon raw material, is drawing boron foundry alloy
Purification processes are carried out to industrial silicon raw material during rod, specific steps include：
Industrial silicon raw material is pre-processed, pure water cleaning is crossed after cleaning 0.5~2min with nitration mixture, then successively by ultrasound
Dried after cleaning；Pretreated industrial silicon raw material is fitted into the silica crucible of monocrystalline equipment, monocrystalline fire door is closed, vacuumizes
And leakage rate is detected, vacuum is 5~8pa in stove, and leakage rate is no more than 5pa/5min；Heater, by power every 8~12
Minute improves once, is gradually risen from initial power 15kw to 90-95kw, the temperature of industrial silicon raw material is reached 1500~1600
DEG C, and start to melt；When the industrial silicon raw material in silica crucible is melted to Φ 200mm~Φ 300mm, heater power is dropped
To 20~30kw, slag is once carried；When liquid level starts crystallization, heater power is increased to 70~75KW, carried out secondary
Crystallize scaling-off；Industrial silicon raw material after secondary crystallization is scaling-off by seeding, shouldering, turn the process such as shoulder, isometrical after obtain boron
Foundry alloy rod.
Industrial silicon raw material after secondary crystallization is scaling-off meets that the quality of boron foundry alloy rod is asked, then by seeding, shouldering,
Stove is closed down after the processes such as isometrical, ending to cool down to obtain boron foundry alloy rod.Wherein, it is when in silica crucible that primary crystallization, which carries slag,
Industrial silicon raw material is filtered when melting to Φ 200mm~Φ 300mm, removes filter residue, retains filtrate.Secondary crystallization is scaling-off to be referred to
After solution crystallization, filtered, remove filtrate.
Seeding is also referred to as welding or kind is brilliant, is that seed crystal is contacted with the industrial silicon raw material melted in silica crucible and is connected into one
Body.Shouldering be in order to increase pull out boron foundry alloy rod diameter, if not shouldering, the diameter very little of the boron foundry alloy rod of pull-out,
It can not use.It is isometrical, i.e., formal crystal pulling process, isodiametric growth of crystal is controlled to the length needed according to melt and single crystal growing furnace situation
Degree.Ending, is that boron foundry alloy rod tail diameter is gradually reduced, leaves melt.
During preparing boron foundry alloy rod using vertical pulling method, control draw conditions, in single crystal growing furnace furnace pressure keep 8-15T,
30-60slpm of argon flow amount, brilliant turn of 6-12rpm/min, crucible turn 4-10rpm/rpm, 6-9 cun of crystalline size, to obtain height
The boron foundry alloy rod of quality.
The present embodiment is once carried slag to the industrial silicon raw material during material before seeding and secondary crystallization is scaling-off,
Remove the impurity in industrial silicon raw material.Scaling-off number is crystallized when it is implemented, can suitably increase according to the amount of impurity, to protect
Demonstrate,prove the quality of drawn product.When the present embodiment draws boron foundry alloy rod in single crystal growing furnace, directly by industrial silicon raw material in single crystal growing furnace
In purified, without extra purification step, simplify technological process, improve production efficiency.
Step S13, shouldering part and the epilog portion of the boron foundry alloy rod are clipped, according to fractional condensation principle by remaining institute
The resistivity for stating boron foundry alloy rod is divided into multiple gears, and the boron foundry alloy rod is cut into bulk according to resistivity gear,
Obtain the boron foundry alloy block of multiple resistivity gears.
The boron element made in the industrial silicon raw material of boron foundry alloy rod is identical with the boron element concentration of target boron foundry alloy rod
Or it is alternate, therefore the resistivity for the boron foundry alloy rod for drawing to obtain by the industrial silicon raw material and the resistance of target boron foundry alloy rod
Rate scope is essentially identical.According to fractional condensation principle, will slowly be solidified again after fusing containing boron industry silicon raw material, then each portion in solid
The impurity concentration divided differs, therefore the resistivity of obtained boron foundry alloy rod various pieces differs.In the present embodiment, according to
The resistivity of the boron foundry alloy rod after clipping shouldering part and epilog portion is divided into 12~16 gears by fractional condensation principle, often
The length of the boron foundry alloy block of individual resistivity gear is 20~200mm.Since the bottom of boron foundry alloy rod, the boron of each gear
The resistivity of foundry alloy block gradually increases.The interval of the resistivity value of each gear is of substantially equal.
During vertical pulling method, boron foundry alloy rod part containing shouldering and epilog portion, this two-part surface irregularity, electricity
Resistance rate detector, such as the probes of KDY-1 tetra-, this two-part resistivity can not accurately be detected.And the ending of afterbody
The change of partial ohmic rate is fast, has an impact to follow-up dispensing resistivity management and control, so to be blocked to it.The shouldering part cut out
Can be as the raw material of secondary making foundry alloy rod with epilog portion.As shown in Fig. 2 the position of blocking of general shouldering part 110 is
The head of boron foundry alloy rod 100 just start isometrical position or its near, epilog portion 120 block position epilog portion to
The position of upper 50mm positions or fractional condensation 94%.
Step S14, measure the actual resistivity of the boron foundry alloy block of each resistivity gear.
The resistivity of boron foundry alloy block based on fractional condensation principle is estimate, it is necessary to be obtained accurately after accurate measurement again
Actual resistivity.KDY-1 resistivity testers can be used in the Resistivity testing of boron foundry alloy block, and reading requirement is accurate to 0.0001
Ω cm, four probe directions must be parallel with cutting lines during test, first carries out an inspection with mark block, mother is detected again after point inspection is qualified
The resistivity of alloy block.
As shown in figure 3,20 points of end surface measurement of each foundry alloy block 200, measurement position is in place for the institute of roundlet in figure 210
Put, record reading after stable reading is constant.The resistivity of the detection in each section calculates average value after removing maximum and small value, takes
The average value being calculated is section resistivity.The section resistivity for two sections of the actual resistivity of each boron foundry alloy block
Average value.The difference of the section resistivity of two sections and the ratio of the average value of two-section surface resistivity will be controlled within 5%.
Step S15, the boron foundry alloy block of each resistivity gear is broken into graininess respectively, and according to resistivity gear
Separately packed.
Boron foundry alloy can be crushed by Mechanical Crushing or stress, for example, Mechanical Crushing can use disintegrating machine to carry out boron mother
Alloy block crushes.For resistivity distributing homogeneity, boron foundry alloy block crushes size and is less than 30*30mm.Boron foundry alloy is broken
Must separately be crushed according to different resistivity gear when broken, and it is broken after peace gear carry out packing as mixing agent and use, can not
Packed so that different stalls are mixed into broken or mixing.
The boron foundry alloy particle of different resistivity gear is used in the foundry alloy doping of silicon ingot, the electricity of the silicon ingot of different purposes
Resistance rate requires different, such as in photovoltaic cell, casting polycrystal silicon ingot, the control of standard (class) monocrystal silicon resistivity are in 0.5 Ω cm
To 6 Ω cm.Agent (boron foundry alloy particle) is mixed according to what the target resistivity of ingot casting selected suitable resistivity gear, and according to
Target resistivity and the resistivity gear for mixing agent used calculate the weight for the foundry alloy particle for needing to add.It is for example, general
Solar level original silicon material is doped using low-resistance borosilicate foundry alloy as dopant, boron foundry alloy dopant resistivity is general
Control is in 0.0001 Ω cm to 0.01 Ω cm.
The present embodiment directly prepares boron mother's synthetic rod with industrial silicon raw material, and according to fractional condensation raw material by the electricity of boron foundry alloy rod
Resistance rate is divided into multiple gears, and the boron foundry alloy rod that making obtains is cut into multiple boron foundry alloy blocks according to resistivity gear,
And measure the actual resistivity of the boron foundry alloy block of each electronics rate gear.By the boron foundry alloy of each resistivity gear cut
Block is broken for boron foundry alloy particle and packed.Select the boron foundry alloy particle of suitable resistivity to be used as when needing to prepare silicon ingot to mix
Miscellaneous dose of use, to adjust the resistivity of silicon ingot.
Embodiment two
Step S21, the selection industrial silicon raw material 130kg same or like with boron element concentration in target boron foundry alloy, and
The summation of metallic element concentration is not higher than 1000ppmw in the industrial silicon raw material.
Step S22, industrial silicon raw material is pre-processed, pure water cleaning is crossed after cleaning 0.5min with nitration mixture, then by super
Dried after sound cleaning；Pretreated industrial silicon raw material is fitted into the silica crucible of monocrystalline equipment, closes monocrystalline fire door, is taken out true
Sky simultaneously detects leakage rate, and vacuum is 5pa, leakage rate 3pa/5min in stove；Heater, power is improved for every 8 minutes
Once, gradually risen from initial power 15kw to 90kw, the temperature of industrial silicon raw material is reached 1500 DEG C, and start to melt；When
When industrial silicon raw material in silica crucible is melted to Φ 200mm, heater power is down to 20kw, is once carried slag；Work as liquid
When face starts crystallization, heater power is increased to 70kw, it is scaling-off to carry out secondary crystallization；Industry after secondary crystallization is scaling-off
Silicon raw material obtains boron foundry alloy rod after seeding, shouldering, isometrical, ending process.Wherein, seeding, shouldering, isometrical, ending lamp
The principle of process is with reference to embodiment one or of the prior art, and it will not go into details again.
Step S23, the size (length, weight, diameter) of the boron foundry alloy rod to coming out of the stove detect, and it is female to clip the boron
The shouldering part of alloy bar and epilog portion, the position for the shouldering part clipped start for the boron foundry alloy club head just
The position in footpath, that clips epilog portion blocks position in the upward 50mm of boron foundry alloy rod epilog portion position.
Step S24, the resistivity of the remaining boron foundry alloy rod is divided into by 12 gears according to fractional condensation principle, and according to electricity
The boron foundry alloy rod is cut into bulk by resistance rate gear, obtains the boron foundry alloy block of 12 resistivity gears, and foundry alloy rod is pressed
Blocked according to elder generation (not including epilog portion and shouldering part) from afterbody length be followed successively by 50mm, 20mm, 30mm, 40mm, 50mm,
60mm, 70mm, 80mm, 90mm, 100mm, 110mm and 136mm.
Step S25, measure the actual resistivity of the boron foundry alloy block of each resistivity gear.The boron foundry alloy of each gear
Actual resistivity measuring method and with reference in embodiment one, will not be described here.
Step S26, the boron foundry alloy block of each resistivity gear is broken into particle of the particle diameter less than 30*30mm respectively,
And separately packed according to resistivity gear.
Embodiment three
Step S31, the selection industrial silicon raw material 150kg same or like with boron element concentration in target boron foundry alloy rod,
And the summation of metallic element concentration is not higher than 1000ppmw in the industrial silicon raw material.
Step S32, industrial silicon raw material is pre-processed, pure water cleaning is crossed after cleaning 2min with nitration mixture, then by ultrasound
Dried after cleaning；Pretreated industrial silicon raw material is fitted into the silica crucible of monocrystalline equipment, monocrystalline fire door is closed, vacuumizes
And leakage rate is detected, vacuum is 8pa, leakage rate 5pa/5min in stove；Heater, power is improved one in every 10 minutes
It is secondary, gradually risen from initial power 15kw to 95kw, the temperature of industrial silicon raw material is reached 1550 DEG C, and start to melt；Work as stone
When industrial silicon raw material in English crucible is melted to Φ 250mm, heater power is down to 25kw, is once carried slag；Work as liquid level
When starting crystallization, heater power is increased to 75kw, it is scaling-off to carry out secondary crystallization；Industrial silicon after secondary crystallization is scaling-off
Raw material obtains boron foundry alloy rod after seeding, shouldering, isometrical, ending process.
Step S33, the size (length, weight, diameter) of the boron foundry alloy rod to coming out of the stove detect, and it is female to clip the boron
The shouldering part of alloy bar and epilog portion, the position for the shouldering part clipped start for the boron foundry alloy club head just
The position in footpath, that clips epilog portion blocks position in the upward 50mm of boron foundry alloy rod epilog portion position；
Step S34, the resistivity of the remaining boron foundry alloy rod is divided into by 14 gears according to fractional condensation principle, and according to electricity
The boron foundry alloy rod is cut into bulk by resistance rate gear, obtains the boron foundry alloy block of 14 resistivity gears, and foundry alloy rod is pressed
Blocked according to elder generation (not including epilog portion and shouldering part) from afterbody length be followed successively by 50mm, 20mm, 30mm, 40mm, 50mm,
60mm, 70mm, 80mm, 90mm, 100mm, 110mm and 120mm, 140mm, 182mm.
Step S35, measure the actual resistivity of the boron foundry alloy block of each resistivity gear.The boron foundry alloy of each gear
Actual resistivity measuring method and with reference in embodiment one, will not be described here.
Step S36, the boron foundry alloy block of each resistivity gear is broken into particle of the particle diameter less than 30*30mm respectively,
And separately packed according to resistivity gear.
Example IV
Step S41, the selection industrial silicon raw material 170kg same or like with boron element concentration in target boron foundry alloy rod,
And the summation of metallic element concentration is not higher than 1000ppmw in the industrial silicon raw material.
Step S42, industrial silicon raw material is pre-processed, pure water cleaning is crossed after cleaning 0.5min with nitration mixture, then by super
Dried after sound cleaning；Pretreated industrial silicon raw material is fitted into the silica crucible of monocrystalline equipment, closes monocrystalline fire door, is taken out true
Sky simultaneously detects leakage rate, and vacuum is 8pa, leakage rate 2pa/5min in stove；Heater, power is improved one in every 12 minutes
It is secondary, gradually risen from initial power 15kw to 95kw, the temperature of industrial silicon raw material is reached 1600 DEG C, and start to melt；Work as stone
When industrial silicon raw material in English crucible is melted to Φ 300mm, heater power is down to 30kw, is once carried slag；Work as liquid level
When starting crystallization, heater power is increased to 75kw, it is scaling-off to carry out secondary crystallization；Industrial silicon after secondary crystallization is scaling-off
Raw material obtains the boron foundry alloy rod after seeding, shouldering, isometrical, ending process.
Step S43, the size (length, weight, diameter) of the boron foundry alloy rod to coming out of the stove detect, and it is female to clip the boron
The shouldering part of alloy bar and epilog portion, the position for the shouldering part clipped start for the boron foundry alloy club head just
The position in footpath, that clips epilog portion blocks position in the upward 50mm of boron foundry alloy rod epilog portion position；
Step S44, the resistivity of the remaining boron foundry alloy rod is divided into by 16 gears according to fractional condensation principle, and according to electricity
The boron foundry alloy is cut into bulk by resistance rate gear, obtains the boron foundry alloy block of 16 resistivity gears, foundry alloy rod according to
First blocked from afterbody (not including epilog portion and shouldering part) length be followed successively by 50mm, 20mm, 30mm, 40mm, 50mm,
60mm, 70mm, 80mm, 90mm, 100mm, 110mm and 120mm, 140mm, 160mm, 180mm, 200mm.
During cutting, if final stage can be not required to block with part≤70mm, the last period is directly incorporated into, if final stage ＞
70mm, separately block.
Step S45, measure the actual resistivity of the boron foundry alloy block of each resistivity gear.The boron foundry alloy of each gear
Actual resistivity measuring method and with reference in embodiment one, will not be described here.
Step S46, the boron foundry alloy block of each resistivity gear is broken into particle of the particle diameter less than 30*30mm respectively,
And separately packed according to resistivity gear.
The embodiment of the present invention draws boron foundry alloy rod using industrial silicon raw material in single crystal growing furnace, reduces production cost.Industry
Silicon raw material is once carried slag in the material stage and secondary crystallization is scaling-off, and industrial silicon raw material is purified, and ensures boron foundry alloy
The quality of rod.Boron foundry alloy rod after drawing is divided into multiple gears according to resistivity, and is cut and crushed, packed.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description
Point is contained at least one embodiment or example of the present invention.In this manual, to the schematic representation of above-mentioned term not
Necessarily refer to identical embodiment or example.Moreover, specific features, structure, material or the feature of description can be any
One or more embodiments or example in combine in an appropriate manner.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (8)
- A kind of 1. boron foundry alloy preparation method, it is characterised in that including：The selection industrial silicon raw material same or like with boron element concentration in target boron foundry alloy rod, and it is golden in the industrial silicon raw material The summation of category concentration of element is not higher than 1000ppmw；The industrial silicon raw material is pre-processed, the pretreated industrial silicon raw material is loaded to the quartzy earthenware of monocrystalline equipment Material is carried out in crucible, when the industrial silicon raw material in silica crucible is melted to Φ 200mm~Φ 300mm, is cooled, and Carry slag；When the liquid level after carrying slag starts crystallization, it is scaling-off to carry out secondary crystallization；The industrial silicon after secondary crystallization is scaling-off Raw material obtains boron foundry alloy rod after seeding, shouldering, isometrical, ending process；Shouldering part and the epilog portion of the boron foundry alloy rod are clipped, according to fractional condensation principle by the remaining boron foundry alloy rod Resistivity be divided into multiple gears, and the boron foundry alloy rod is cut into by bulk according to resistivity gear, obtains multiple resistance The boron foundry alloy block of rate gear；Measure the actual resistivity of the boron foundry alloy block of each resistivity gear；The boron foundry alloy block of each resistivity gear is broken into graininess respectively, and separately beaten according to resistivity gear Bag.
- 2. boron foundry alloy preparation method as claimed in claim 1, it is characterised in that described by the pretreated industrial silicon Raw material, which is fitted into the silica crucible of monocrystalline equipment, carries out material, when the industrial silicon raw material in silica crucible is melted to Φ During 200mm~Φ 300mm, cooled, and carry slag；When the liquid level after carrying slag starts crystallization, it is scaling-off to carry out secondary crystallization Step includes：Pretreated industrial silicon raw material is fitted into the silica crucible of monocrystalline equipment, vacuumizes and detects leakage rate, it is true in stove Reciprocal of duty cycle is 5~8pa, and leakage rate is no more than 5pa/5min；Heater, power is improved once for every 8~12 minutes, from starting Power 15kw is gradually risen to 90-95kw, the temperature of industrial silicon raw material is reached 1500~1600 DEG C, and start to melt；Work as stone When industrial silicon raw material in English crucible is melted to Φ 200mm~Φ 300mm, heater power is down to 20~30kw, carries out one It is secondary to carry slag；When liquid level starts crystallization, heater power is increased to 70~75kw, it is scaling-off to carry out secondary crystallization.
- 3. boron foundry alloy preparation method as claimed in claim 1, it is characterised in that described to be carried out in advance to the industrial silicon raw material The step of processing, includes：Industrial silicon raw material is pre-processed, pure water cleaning is crossed after cleaning 0.5~2min with nitration mixture, then dried after ultrasonic cleaning It is dry.
- 4. boron foundry alloy preparation method as claimed in claim 1, it is characterised in that prepare the process of the boron foundry alloy rod In, furnace pressure keeps 8-15T, 30-60slpm of argon flow amount, brilliant turn of 6-12rpm/min, crucible to turn 4-10rpm/ in single crystal growing furnace 6-9 cun of rpm, crystalline size.
- 5. boron foundry alloy preparation method as claimed in claim 1, it is characterised in that shouldering part will be clipped according to fractional condensation principle It is divided into 12~16 gears, the boron foundry alloy of each resistivity gear with the resistivity of the boron foundry alloy rod after epilog portion The length of block is 20~200mm.
- 6. boron foundry alloy preparation method as claimed in claim 1, it is characterised in that the boron foundry alloy club head and afterbody The scope of the ratio of resistivity is 1.5~3.
- 7. boron foundry alloy preparation method as claimed in claim 1, it is characterised in that described respectively by each resistivity gear Boron foundry alloy block, which is broken into granular step, to be included：The boron foundry alloy block of each resistivity gear is broken into less than 30*30mm particles.
- 8. boron foundry alloy preparation method as claimed in claim 1, it is characterised in that position is blocked as institute in the shouldering part State boron foundry alloy club head and finished up in the boron foundry alloy rod just starting isometrical position, the position of blocking of the epilog portion The upward 50mm in part position.
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| CN111304743A (en) * | 2019-10-30 | 2020-06-19 | 弘元新材料(包头)有限公司 | Process for pulling single crystal furnace automatic system |
| CN113774474A (en) * | 2021-09-17 | 2021-12-10 | 青海高景太阳能科技有限公司 | Preparation method for improving single crystal RRV |
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