CN102817075A - Master alloy production method by using polycrystalline foundry furnace - Google Patents
Master alloy production method by using polycrystalline foundry furnace Download PDFInfo
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Abstract
A master alloy production method by using a polycrystalline foundry furnace relates to the technical field of photovoltaic manufacturing. The method comprises the following steps: a. material selection: selecting a silicon material; b. calculating the amount of a dopant required; c. adding the dopant into sorted silicon material, loading the material and feeding into an ingot furnace; and d. using a polycrystalline silicon foundry method by successively carrying out steps comprising vacuumizing, heating, melting, growing crystal, annealing and cooling on the silicon material and the dopant, so as to produce a master alloy silicon ingot. The invention has beneficial effects of increasing the production yield as well as reducing the production cost. According to the invention, an optimal dose range of the dopant to be added can be calculated according to segregation state of the dopant in silicon; and an optimal range of the dopant is determined by the amount of master alloy produced in each furnace and the electrical resistivity of the required master alloy. The method can produce optimized master alloy through calculation, and reduce the production cost of enterprise to the maximum degree.
Description
Technical field
The present invention relates to photovoltaic manufacturing technology field, utilize the polycrystalline foundry furnace to carry out novel mother alloy working method, the single crystal pulling method that breaks traditions, especially a kind of through control to the doping agent consumption, produce the castmethod of the mother alloy of optimal resistivity.
Background technology
So-called " mother alloy " is exactly the alloy of impurity element and silicon in the photovoltaic industry; Mainly refer to the borosilicate alloy; The effect of mother alloy is mixed to raw material exactly; Purpose mainly is the impurity concentration that is used for changing donor impurity in the silicon melt (like phosphorus) or acceptor impurity (like boron), makes its monocrystalline that grows or polycrystalline resistivity reach the requirement of regulation.
Traditional mother alloy method for manufacturing all is to be drawn by single crystal growing furnace to form, and its defective is: yield poorly, the single crystal rod weight that traditional single crystal growing furnace one stove is pulled out is about 100kg; And level of automation is relatively low; The operation more complicated, the single crystal growing furnace volume is little, and the pulled crystal rod receives the influence of length and diameter; Production capacity is little, and cost of manufacture is high.
And adopt the method for casting, and make unrestrictedly, only depend on the size of heat size device; The every furnace output of polycrystalline ingot furnace can reach more than the 450kg at present; Even can throw into 800kg, and level of automation is very high, and yield rate is also than higher; Better large-scale production, the cost aspect can be controlled better.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing the polycrystalline foundry furnace to produce mother alloy, be intended to utilize the polycrystalline foundry furnace to produce mother alloy, thereby improve production output, reduce production costs.Especially through control, produce the mother alloy of required optimal resistivity to the doping agent consumption.
In polycrystalline Foundry Production mother alloy process, the consumption of controlled doping agent is crucial.Just can cast out the mother alloy of required optimal resistivity.The doping agent consumption is big, and the mother alloy resistivity that can cause producing is too low, in batching, is not easy to control consumption.The doping agent consumption is little, and the consumption of required mother alloy can increase in the time of batching, will increase some unnecessary costs.Therefore, the accurate consumption of calculation control doping agent has become bottleneck of the present invention.The present invention calculates the doping agent optimum amount scope that institute will throw in through the fractional condensation situation of doping agent in silicon, and what and required mother alloy resistivity that the optimum range of doping agent is produced mother alloy according to every stove are confirmed.
The objective of the invention is to realize through following scheme:
Utilize the polycrystalline foundry furnace to produce the method for mother alloy, it is characterized in that adopting successively following steps: a selects materials, and promptly selects used silicon material; B calculates the amount of required doping agent; C adds doping agent with well-graded silicon material, and ingot furnace is thrown in normal charging back; D adopts the method for polysilicon casting, to silicon material and doping agent vacuumize successively, heat, melt, long brilliant, anneal, cool off link, produce the mother alloy silicon ingot.
Further:
Used silicon material requires: P type/N type resistivity requires greater than 1 Ω .cm, and purity is more than 6N; Can be the quality that improves mother alloy so on the one hand, in theory is calculated, can ignore N type doping agent P, AS etc./P type doping agent B, the fractional condensation situation of AL etc. on the one hand in addition.
The method of said adding doping agent is: according to the fractional condensation situation of doping agent in silicon, come to calculate accurately the doping agent consumption that will throw in; In the computation process, carry out following steps successively:
A is according to formula one: N=1.33*power (10; 16)/ρ 1+1.082*power (10; 17)/ρ 1 [1+power (54.56 ρ 1,1.105)] (theoretical calculation formula sees that the GB/T13389-1992 boron-doping mixes phosphorus single crystal silicon resistivity and doping content conversion article, calculates the doping content value by boron-doped silicon monocrystalline resistivity); Calculate by the B atomic percent in the silicon material of resistivity stepping, calculate atom number wherein through concentration then.
B is according to formula two: n1=(M1*2.33/10.84*6.02*power (10,23)+2.33*M)
/ (M*1000) * 0.75*power (1-(H*2.33*83*83)/(M*1000);-0.25) (theoretical formula is seen the photovoltaic material books of being correlated with: the doping content of different positions is by the segregation coefficient decision of doping agent itself); Calculate the fractional condensation concentration of dopant atom different positions in silicon solution in silicon material and the doping agent, wherein the atom number of doping agent is by how many decisions of doping agent consumption;
C is according to formula three: ρ 2=1.305*power (10; 16)/N+1.133*power (10; 17)/(N+N*power (2.58*power (10 ,-19) * N ,-0.737)) (theoretical calculation formula sees that the GB/T13389-1992 boron-doping mixes phosphorus single crystal silicon resistivity and doping content conversion article; Calculate boron-doping silicon wafer resistivity by doping content), calculate the resistivity of silicon ingot different positions; The calculated resistance rate is to produce in order better to be used for, because can use the mother alloy of different resistivity scope in the actual production;
How many doping agents D confirms to add according to the requirement of resistivity.
Described doping agent refers to boron or phosphorus.
The alphabetical implication that above-mentioned formula relates to: N is a doping content, and ρ is a silicon wafer resistivity, and wherein, ρ 1 is the silicon material resistivity of throwing the actual different gear resistivity that record in stokehold, ρ 2 be according to calculate come out of the stove after the resistivity of silicon material; N1 is a fractional condensation concentration, and M1 is a boron opaque amount, and M is the silicon ingot quality, and H is the silicon ingot height.
Adopt the method for polysilicon casting in the said d step, specifically: A vacuumizes: vacuumize and be evacuated to below the 0.01mbar, begin to connect the well heater operation; B heating: during heating, power is increased to 90% from 0%, when Heating temperature levels off to 1175 ℃ of power control and temperature controlled conversion temps, and slowly lower again (dropping to 50%-60%), the heat-processed of execution 4-5h under vacuum state; The C fusing: the fs still is in vacuum state to extract the gas in crucible and the silicon material in the melting process; Feed argon gas afterwards, make pressure maintain 500-700mbar, the melting process top temperature is between 1535-1560, and melting process continues about 10-14h; D is long brilliant: fusing need to finish artificially to confirm that the back gets into the long brilliant stage, in long first brilliant stage, temperature reaches long brilliant design temperature, opens heat-insulation cage with cooling DS-block, reach long brilliant temperature after silicon ingot long brilliant from the bottom to the top; Long brilliant process continues 22-26h, and long brilliant pressure process still maintains between the 500-700mbar; E annealing: during annealing, close heat-insulation cage, temperature drops to annealing temperature and is incubated the temperature more than two hours, makes in the silicon ingot temperature everywhere identical; The F cooling: accomplish the annealing back and get into colling stages, open heat-insulation cage and feed argon gas to quicken cooling, colling stages is more than 10h; Cooling the last stage, the TC2 temperature drops to below 450 ℃, and heat-insulation cage is opened fully; Pressure is charged to 940-960mbar, goes out ingot afterwards.
The invention has the beneficial effects as follows: adopt the method for invention casting to produce mother alloy,, produce the mother alloy of required optimal resistivity especially through control to the doping agent consumption.Its advantage is: 1, level of automation is high, and technology is simple, is convenient to control.2, improve output, reduced production cost; Because manufacturing is unrestricted, only depend on the size of heat size device, the every furnace output of polycrystalline ingot furnace can reach more than the 450kg at present, even can throw into 800kg, has therefore realized the large-scale production of mother alloy, and output is obviously promoted.And yield rate is higher, has reduced production cost effectively.3, can pass through the calculation control production cost, help the lifting of enterprise profit.Can produce optimized mother alloy castmethod through calculating, farthest reduce the production cost of enterprise.Producing the mother alloy of required optimal resistivity, is vital to the requirement of resistivity, must know the requirement to mother alloy resistivity before throwing stove production, need weigh the advantages and disadvantages.Such as the mother alloy of producing 0.0025 Ω .cm resistivity, in the production of carrying out polycrystal silicon ingot, throwing the used mother alloy amount of stove amount about every stove 450kg is about 80g.And produce the mother alloy of 0.0013 Ω .cm resistivity, the throwing stove amount of every stove is about 40g.Throw the stove amount although can reduce, but also can increase some risks, resistivity is low more, will accurately control more the assurance of throwing the stove amount.Therefore, produce the mother alloy of which scope resistivity, need in actual production, grasp flexibly.Adopt the present invention, can come better control production cost, improve enterprise profit through in good time cost analysis.
Embodiment
In order to make those skilled in the art person understand the present invention program better, and make above-mentioned purpose of the present invention, feature and advantage can be more obviously understandable, below in conjunction with embodiment the present invention done further detailed explanation.
Embodiment 1:
Produce P type doping agent, doping agent is the boron powder.
With the silicon material of the P type 1.5 Ω .cm of the well-graded 450kg of a stove, purity is more than 6N, and producing 1cm place, silicon ingot bottom resistivity is the mother alloy of 0.0025 Ω .cm.The weight that can accurately calculate required boron powder is 202.44g; Calculate by formula one (see before and state) that boron atom number is 1.81882E+21 in the silicon material; The doping content of being calculated 1cm place, silicon ingot bottom by formula two (see before and state) is 4.40638E+19; The resistivity of calculating 1cm place, silicon ingot bottom according to the segregation coefficient of boron in silicon by formula three (see before and state) is P type 0.002500036 Ω .cm, can be good at satisfying the production demand.Can be 0.001375611 Ω .cm through the resistivity P type that formula three accurately calculates silicon ingot 26cm place this moment also.Through calculating the boron powder that adds 202.44g in can feeding normally, throw behind the stove through vacuumizing, heating, fusing, long brilliant, annealing is cooled off six links and just can be produced satisfactory mother alloy silicon ingot.Vacuumize and be evacuated to below the 0.01mbar; Begin to connect the well heater operation; During heating; Power is increased to 90% by certain change curve from 0%, when Heating temperature levels off to 1175 ℃ of power control and temperature controlled conversion temps, slowly lowers the heat-processed of all 4-5h of execution under vacuum state again.The fs still is in vacuum state to extract the gas in crucible and the silicon material in the melting process.Feed argon gas afterwards, make pressure maintain 500-700mbar, the melting process top temperature is between 1535-1560, and melting process continues about 12h.Fusing finish to need artificially to confirm that the back gets into the long brilliant stage, in long first brilliant stage, temperature reaches long brilliant design temperature, opens heat-insulation cage with cooling DS-block, reach long brilliant temperature after silicon ingot long brilliant from the bottom to the top.Long brilliant process is about 24h, and long brilliant pressure process still maintains between the 500-700mbar.During annealing, close heat-insulation cage afterwards, temperature drops to annealing temperature and is incubated temperature more than two hours makes in the silicon ingot temperature everywhere identical.Accomplish the back of annealing and get into colling stages, open heat-insulation cage and feed argon gas to quicken cooling, colling stages cools off the last stage more than 10h, and the TC2 temperature drops to below 450 ℃, and heat-insulation cage is opened fully, and pressure is charged to 950mbar, prepares out ingot.
Can carry out evolution to silicon ingot normally afterwards, block thin slice, be divided into 0.0010-0.0015 Ω .cm by mother alloy resistivity into 1-2cm, 0.0016-0.0020 Ω .cm, 0.0021-0.0025 Ω .cm third gear is applied to actual production.
Embodiment 2:
Produce N type doping agent, doping agent is a phosphorus.
Embodiment is with last identical, and above-mentioned three formula need to calculate according to the doping content of N type doping agent and the conversion between the resistivity, do not give unnecessary details in detail at this.
The above; Be merely embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is in the technical scope that the present invention discloses; The variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (5)
1. utilize the polycrystalline foundry furnace to produce the method for mother alloy, it is characterized in that adopting successively following steps: a selects materials, and promptly selects used silicon material; B calculates the amount of required doping agent; C adds doping agent with well-graded silicon material, and ingot furnace is thrown in normal charging back; D adopts the method for polysilicon casting, to silicon material and doping agent vacuumize successively, heat, melt, long brilliant, anneal, cool off link, produce the mother alloy silicon ingot.
2. the method for utilizing the polycrystalline foundry furnace to produce mother alloy according to claim 1, it is characterized in that used silicon material requires: P type/N type resistivity requires greater than 1 Ω .cm, and purity is more than 6N.
3. the method for utilizing the polycrystalline foundry furnace to produce mother alloy according to claim 1 and 2 is characterized in that the method that adds doping agent is: according to the fractional condensation situation of doping agent in silicon, come to calculate accurately the doping agent consumption that will throw in; In the computation process, carry out following steps successively:
A is according to formula one: N=1.33*power (10,16)/ρ 1+1.082*power (10,17)
/ ρ 1 [1+power (54.56 ρ 1,1.105)] calculates by the B atomic percent in the silicon material of resistivity stepping;
(M1*2.33/10.84*6.02*power (10 according to formula two: n1=for B; 23) * 0.75*power (1-(H*2.33*83*83)/(M*1000)+2.33*M)/(M*1000);-0.25); Calculate the fractional condensation concentration of dopant atom different positions in silicon solution in silicon material and the doping agent, wherein the atom number of doping agent is by how many decisions of doping agent consumption;
C is according to formula three: ρ 2=1.305*power (10,16)/N+1.133*power (10,17)
The resistivity of silicon ingot different positions is calculated in/(N+N*power (2.58*power (10 ,-19) * N ,-0.737));
How many doping agents D confirms to add according to the requirement of resistivity.
4. the method for utilizing the polycrystalline foundry furnace to produce mother alloy according to claim 3, it is characterized in that: doping agent refers to boron or phosphorus.
5. want the 1 described method of utilizing the polycrystalline foundry furnace to produce mother alloy according to right, it is characterized in that: adopt the method for polysilicon casting in the d step, specifically: A vacuumizes: vacuumize and be evacuated to below the 0.01mbar, begin to connect the well heater operation; B heating: during heating, power is increased to 90% from 0%, when Heating temperature levels off to 1175 ℃ of power control and temperature controlled conversion temps, slowly lowers the heat-processed of execution 4-5h under vacuum state again; The C fusing: the fs still is in vacuum state to extract the gas in crucible and the silicon material in the melting process; Feed argon gas afterwards, make pressure maintain 500-700mbar, the melting process top temperature is between 1535-1560, and melting process continues about 10-14h; D is long brilliant: fusing need to finish artificially to confirm that the back gets into the long brilliant stage, in long first brilliant stage, temperature reaches long brilliant design temperature, opens heat-insulation cage with cooling DS-block, reach long brilliant temperature after silicon ingot long brilliant from the bottom to the top; Long brilliant process continues 22-26h, and long brilliant pressure process still maintains between the 500-700mbar; E annealing: during annealing, close heat-insulation cage, temperature drops to annealing temperature and is incubated the temperature more than two hours, makes in the silicon ingot temperature everywhere identical; The F cooling: accomplish the annealing back and get into colling stages, open heat-insulation cage and feed argon gas to quicken cooling, colling stages is more than 10h; Cooling the last stage, the TC2 temperature drops to below 450 ℃, and heat-insulation cage is opened fully; Pressure is charged to 940-960mbar, goes out ingot afterwards.
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| CN103361724A (en) * | 2013-06-21 | 2013-10-23 | 东海晶澳太阳能科技有限公司 | Boron-gallium co-doped efficient polycrystalline silicon and preparation method thereof |
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| CN104178809A (en) * | 2014-09-01 | 2014-12-03 | 大连理工大学 | Method for preparing low metal boron master alloy by use of metallurgy method |
| CN104195638A (en) * | 2014-09-01 | 2014-12-10 | 大连理工大学 | Method for preparing boron master alloy by using metallurgy method |
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| CN112251805A (en) * | 2019-07-22 | 2021-01-22 | 洛阳阿特斯光伏科技有限公司 | Nitrogen-doped P-type silicon master alloy and preparation method thereof, nitrogen-doped polycrystalline silicon ingot and preparation method thereof |
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Application publication date: 20121212 |