CN101906659A - Doping method of monocrystalline silicon for photovoltaics - Google Patents
Doping method of monocrystalline silicon for photovoltaics Download PDFInfo
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Abstract
The invention relates to a doping method of monocrystalline silicon for photovoltaics. The doping method ensures the doping accuracy by adopting a supplementary doping method and completes the formula computation and the spreadsheet making by utilizing Excel software, therefore, the work originally completed by specific people on a computer can be conveniently completed by workers through checking printed spreadsheets.
Description
Technical field
The present invention relates to a kind of adulterating method of monocrystalline silicon for photovoltaics, especially a kind of doping up method of silicon single crystal.
Background technology
The rise of green energy resource has promoted the development of photovoltaic with the silicon single-crystal industry, and the various types of silicon raw material all makes the best use of everything, and a lot of feed particles are very little and can't test.Adulterated purpose: the client provides the electrical resistivity range requirement, monocrystalline resistivity is by descend in order from the beginning to the end (being because the boron concentration of decision resistivity increases successively owing to dephlegmation), by the resistivity (abbreviation target resistivity) of control monocrystalline head, thereby the resistivity that makes whole monocrystalline is in acceptability limit.Adulterated principle: boron conservation, boron only come from raw material and mother alloy.After the high temperature liquefaction, boron is thorough mixing under effects such as thermal convection, mechanical stirring, and distributes according to the fractional condensation principle.The fractional condensation principle: solid silicon monocrystalline and liquid silicon monocrystalline are as the different solubility of different media to the boron atom, and its ratio is called segregation coefficient K, is 0.8 herein, and solid is lower slightly to the solubleness of boron.Resistivity and boron concentration relationship (the resistivity unit resistance is Ω .cm, omits for style of writing makes things convenient for resistivity unit): resistivity and boron concentration have certain mutual transformational relation, calculating formula following (this relational expression is seen GB GB/T13389-92):
N=(1.33E+16/ ρ)+1.082E+17/ ρ * [1+ (54.56 * ρ) ^1.105)] formula 1;
ρ=(1.305E+16/N)+1.133 * E+17/{N * [1+ (^-0.737 of 2.58 * 10E+-19 * N)] } formula 1 ';
E wherein is a scientific notation.
Originally the adulterating method of Shi Yonging is commonly referred in advance and mixes, and gets the boron content that intermediate value is calculated raw material according to resistivity of raw materials, in the time of shove charge, packs in the lump calculating good mother alloy.Advantage, centre need not blow-ons, save time, and parts are also had certain benefit work-ing life; When shortcoming was exactly the boron content that calculates in the raw material, resistivity was calculated and is got intermediate value (from the relational expression and the nonlinear relationship of resistivity and concentration, getting intermediate value also is caving-in bash); Even if it is feasible to get intermediate value, if 0.5-3, be on earth inclined to one side 0.5 still be more inclined to one side 3 many, this is very uncertain, error is more, takes care of the pence, and tends to occur than large deviation it would, of course, also be possible to " two negatives make a positive ".
The method of calculation of mixing in advance suppose to have 5 kinds of raw materials, and resistivity (getting intermediate value), quality are respectively ρ 1, G1, and ρ 2, G2 ..., ρ 5, G5;
1, at first calculate corresponding concentration N1 according to resistrivity meter, N2 ..., N5;
2, calculate boron content N1 * G1+N2 * G2+....+N5 * G5 in the raw material;
3, set the target resistivity of a head, calculate the aimed concn Nm (the boron concentration of target resistivity silicon single crystal correspondence) of head;
4, calculate the concentration Nx of mother alloy according to the resistivity specification of mother alloy;
Above-mentioned all is known parameters, and these parameters also can change.Unknown parameter only is mother alloy weight Gx, and unit is g, and the density of silicon is 2.33g/cm
3Gx is generally g, and charging capacity is kg, and charging capacity can be ignored mother alloy weight during calculating.
The fractional condensation effect that produces during 5, according to boron conservation and crystallization:
Head aimed concn * charging capacity=(existing boron content+mother alloy boron content in the raw material) * segregation coefficient
According to above-mentioned thinking: the corresponding substitution that concerns, wherein K is a constant 0.8, has only Gx in the formula for treating evaluation:
Nm * (G1+G2...+G5)=[(N1 * G1+N2 * G2.......+N5 * G5)+(Gx ÷ 1000 ÷ 2.33) * Nx] * K formula 2 '
Here have only a unknown number Gx, these operation relations are converted into the formula of Excel, make form and be used for producing.In general this evaluation work of mixing in advance needs special personnel to finish on computers.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of adulterating method of monocrystalline silicon for photovoltaics is provided, the used mother alloy quality of calculated single crystal silicon doping accurately.
According to technical scheme provided by the invention, the adulterating method step of described monocrystalline silicon for photovoltaics is as follows:
At first polycrystalline silicon raw material is put into single crystal growing furnace, melt in the protective atmosphere in the main chamber, seed crystal hangs from concubine insertion liquid silicon and gets sample, by isolating the major-minor chamber sample is taken out, and tests the electricalresistivity of sample then with four point probe
Little,
The boron concentration N of sample
Little, mother alloy boron concentration Nx, the boron concentration Nm of target resistivity silicon single crystal all calculates by formula 1
N=(1.33E+16/ ρ)+1.082E+17/ ρ * [1+ (54.56 * ρ) ^1.105)] formula 1
Promptly obtain boron concentration N by the electricalresistivity;
Need the mother alloy quality Gx that drops into to calculate by formula 2
Nm * G=N * G+ (Gx ÷ 1000 ÷ 2.33) * Nx * K formula 2
Wherein, G is total charging capacity of polycrystalline silicon raw material, and segregation coefficient K is a constant 0.8;
Utilize Microsoft Office Excel software to calculate automatically formula 1 and formula 2, input comprises: target resistivity, the Ω .cm of unit; Total charging capacity G, units; Mother alloy resistivity, the Ω .cm of unit; The electricalresistivity of sample
Little, the Ω .cm of unit; Work output is mother alloy quality Gx, the g of unit (following omission unit); Generate the sample electricalresistivity by Excel software
LittleWith the form of the respective value of mother alloy quality Gx, the workman is according to the sample electricalresistivity who measures
LittleTable look-up and needing to obtain the mother alloy quality Gx of input.
Advantage of the present invention is: in scale operation, because the silicon raw material is comparatively mixed and disorderly, the present invention adopts the method for doping up to guarantee adulterated accuracy, and the work that needs the special messenger to finish on computers originally, only need print form and table look-up and can conveniently solve for the workman.
Embodiment
Because the uncertainty of raw material and the improvement of monocrystalline equipment, we expect getting a fritter after the seed crystal insertion by concubine after changing material, and test resistance rate resistivity is as a whole carried out computing.After changing material and finishing, whole volatilization face is enough big, does not have oxygen alms giver (can play the retroaction of N type on resistivity) substantially, and resistivity that should the sample piece is the most correct.
The resistivity of sample piece is being used in the process of this account form as the single resistivity of this stove monocrystalline.Sample resistance ρ
LittleInput, weight is total charging capacity G=G1+G2...+G5; The weight of other four kinds of raw materials is made as 0, applies mechanically the formula of mixing in advance, and in use, usually crystal bar is lower than target value in annealing (eliminating " N type " effect of oxygen alms giver) back resistivity.Why can you mix many?
Under special circumstances, if head target resistance and sample resistance are all 2, using this calculating formula to show also needs to mix.If this obviously bigger deviation occurred with our cognition---do not get sample, the head of Here it is monocrystalline has reached target resistivity, should mix, and changes charging capacity, mother alloy specification etc. at this moment in reckoner, and doping all should be 0.
The present invention has proposed the account form of doping up and the difference of mixing in advance for the first time, has summed up difference between the two.And by corresponding design, under the situation of scale operation, charging capacity, the mother alloy specification, the target resistance of monocrystalline is a fixed, mother alloy uses also and determines under the situation that sample resistance is determined, the work that the professional must finish on computers, only need simple table look-up to get.
Through careful distinguishing, what may go wrong has two aspects: whether solid-liquid density difference is different consistent with the liquid sensistor with sample resistance.
Solid-liquid density is respectively 2.33 and 2.53, and difference is little, and finally exists with solid form, so get rid of.
Sample resistance and liquid sensistor: crystalline moment exists the effect of segregation, segregation coefficient 0.8.The resistance that is sample is 2, and its corresponding boron concentration is N
Little, the boron concentration of liquid silicon is N so
Little/ 0.8, the resistivity that goes out of concentration conversion is only the overall resistivity of silicon raw material (solid) thus again, use this resistivity with mix in advance formula calculate be only right.
So far also can explain original doubt: sample resistance ≠ liquid sensistor, (it is generally acknowledged: from homogeneous take off one on the whole, inevitable be identical with integral body, has ignored the difference of the solubleness of solid-liquid two relative boron here.) but be higher than the liquid sensistor, and certain mathematical relation is arranged.
From the another one angle, if whole stove resistivity of raw materials is very desirable, all be 2, to draw the head target resistivity so and be 2 monocrystalline, want on earth to mix?
Want obviously, because the resistance head height of boron-doping monocrystalline, afterbody low (corresponding boron concentration is exactly that head is low, afterbody is high), according to the boron conservation, if undope, so what Xia Mian boron come from if head resistance is 2? thereby verified that it is full of prunes that original way is used as whole silicon raw material resistance to sample resistance.
First kind of method of calculation is as follows:
1, sample electricalresistivity
LittleObtain sample boron concentration N
Little
2, sample boron concentration obtains liquid silicon boron concentration=N
Little/ 0.8
3, liquid silicon boron concentration can get the liquid silicon resistivity, uses the formula 1 ' of GB to obtain.
4, this resistivity is as the overall resistivity of raw material, and use is mixed method of calculation in advance and got final product.
Second kind of method of calculation is as follows:
With respect to mixing formula in advance:
Head aimed concn * charging capacity=(existing boron content+mother alloy boron content) * segregation coefficient;
The calculation formula of doping up:
Boron concentration * the charging capacity of head aimed concn * charging capacity=sample+mother alloy boron content * segregation coefficient;
Only needing " existing boron content * segregation coefficient " is the boron content sum total of sample resistivity corresponding concentration, here lacks than original relational expression in other words and takes advantage of a segregation coefficient K to get final product.
By these two kinds of method result calculated very near (error is minimum).In present production management, tend to use fixed charging capacity, head target resistance and mother alloy specification (concentration), sample resistance arrives between the head target resistivity tens usually.Situation about making in order at above-mentioned relation, sequence that often can be by sample resistivity (etc. difference 0.1,0.2,0.3 all can) obtains corresponding mother alloy value (corresponding one by one).Make the work that originally needs the professional to finish on computers, can solve by monocrystalline workman simple table look-up table.With the monocrystalline of 1-3 electrical resistivity range in the market, target resistance is placed on 2, if sample resistance roughly in the 10-2 scope, can carry out segmentation according to 0.1 or 0.2 as required voluntarily and get final product, can finish most doping work, precise and high efficiency.
Specific practice of the present invention is as follows:
At first polycrystalline silicon raw material is put into single crystal growing furnace, fusing in the protective atmosphere in the main chamber (being generally argon gas), seed crystal hangs from concubine insertion liquid silicon and gets sample, by isolating the major-minor chamber sample is taken out, and tests the electricalresistivity of sample then with four point probe
Little
The boron concentration N of sample
Little, mother alloy boron concentration Nx, the boron concentration Nm of the silicon single crystal of target resistivity all calculates by formula 1, promptly obtains boron concentration N by the electricalresistivity;
Need the mother alloy quality Gx that drops into to calculate by following formula
Nm * G=N * G+ (Gx ÷ 1000 ÷ 2.33) * Nx * K formula 2
Wherein, G is total charging capacity of multiple polycrystalline silicon raw material, and segregation coefficient K is a constant 0.8,
Utilize Excel software to calculate automatically formula 1 and formula 2, input comprises: target resistivity, and total charging capacity (units), mother alloy resistivity, the electricalresistivity of sample, work output is mother alloy quality Gx (g).Target resistivity is the interior value of electrical resistivity range (such as 1～3 Ω .cm) (such as getting 2 Ω .cm) according to customer requirement.In industrial production, first three input is more fixing, the sample electricalresistivity of a sequence of input
Little, promptly obtain the mother alloy quality Gx of a corresponding sequence by formula 2, form form.Form is printed.The workman measures the sample electricalresistivity after hanging and getting sample
Little, tabling look-up promptly needs the mother alloy quality Gx that drops into as can be known.
Example is as follows:
Charging capacity 60kg, mother alloy specification 0.02 Ω .cm, target resistance 2 Ω .cm, sample resistance also are 2 Ω .cm.
Formula is mixed in the use of mistake in advance: if use blindly mix in advance formula 2 ', think that sample resistivity is 2, the liquid silicon resistivity is exactly 2, corresponding concentration is 6.95E+15, then the boron content in the raw material is 4.171E+17, final doping up amount is 32.271g.
Formula is mixed in correct use in advance: sample resistivity is 2, then corresponding concentration is 6.95E+15, the boron concentration of liquid silicon then is 8.69E+15, by GB calculation formula 1 ', the resistivity that draws actual liquid silicon is 1.65, corresponding concentration is 8.54E+15 (having produced error in the conversion process), boron content in the raw material is 5.122E+17, final doping up amount is 2.83g (from following table as can be seen, this consumption is minimum to the variable effect of resistivity, absolute＜0.1).
Use the doping up formula: concrete outcome sees Table one, owing to wherein have only a correlated variables, the i.e. resistivity of sample.So obtain the relation of following sample resistivity and doping as sequence.
We can see clearly by three methods: formula is mixed in the use of mistake in advance can seriously strengthen doping; Method is mixed in correct use in advance also can be because of producing certain error in the switching process; Use the method for calculation of doping up the most directly perceived, accurately precision is also high.Through the test of quality portion, the accuracy of product resistivity improves greatly.
Suppose: charging capacity 60kg, mother alloy specification 0.02 Ω .cm, target resistance 2 Ω .cm.As shown in the table: can obtain mother alloy doping weight by simple table look-up according to sample resistivity, when sample resistivity=target resistivity, doping is 0, precise and high efficiency.If change charging capacity, mother alloy specification, target resistance etc. only need simply after changing, the automatic computing by Excel can obtain one group of new numerical value, is adapted to large-scale production especially.The weighing apparatus that precision is used with routine in the table is as the criterion, and resistivity, mother alloy resistivity precision are respectively 0.1,0.001 Ω .cm; The quality precision is 0.001g.
Table one
| Charging capacity | 60 | The mother alloy specification | 0.02 |
| Target resistance | 2 |
| Sample resistivity | Doping agent weight | Sample resistivity | Doping agent weight |
| 9.0 | 126.758 | 5.6 | 105.424 |
| 8.9 | 126.365 | 5.5 | 104.390 |
| 8.8 | 125.964 | 5.4 | 103.318 |
| 8.7 | 125.553 | 5.3 | 102.204 |
| 8.6 | 125.133 | 5.2 | 101.047 |
| 8.5 | 124.702 | 5.1 | 99.844 |
| 8.4 | 124.261 | 5.0 | 98.592 |
| 8.3 | 123.810 | 4.9 | 97.287 |
| 8.2 | 123.347 | 4.8 | 95.927 |
| 8.1 | 122.873 | 4.7 | 94.509 |
| 8.0 | 122.387 | 4.6 | 93.027 |
| 7.9 | 121.888 | 4.5 | 91.478 |
| 7.8 | 121.376 | 4.4 | 89.857 |
| 7.7 | 120.851 | 4.3 | 88.159 |
| 7.6 | 120.312 | 4.2 | 86.379 |
| 7.5 | 119.759 | 4.1 | 84.510 |
| 7.4 | 119.190 | 4.0 | 82.545 |
| 7.3 | 118.606 | 3.9 | 80.476 |
| 7.2 | 118.005 | 3.8 | 78.297 |
| 7.1 | 117.387 | 3.7 | 75.996 |
| 7.0 | 116.751 | 3.6 | 73.565 |
| 6.9 | 116.096 | 3.5 | 70.990 |
| 6.8 | 115.422 | 3.4 | 68.260 |
| 6.7 | 114.727 | 3.3 | 65.360 |
| 6.6 | 114.011 | 3.2 | 62.273 |
| 6.5 | 113.273 | 3.1 | 58.982 |
| 6.4 | 112.512 | 3.0 | 55.463 |
| 6.3 | 111.725 | 2.9 | 51.694 |
| 6.2 | 110.914 | 2.8 | 47.647 |
| 6.1 | 110.075 | 2.7 | 43.289 |
| 6.0 | 109.207 | 2.6 | 38.584 |
| 5.9 | 108.310 | 2.5 | 33.489 |
| 5.8 | 107.382 | 2.4 | 27.951 |
| 5.7 | 106.420 | 2.3 | 21.913 |
| 2.2 | 15.301 | ||
| 2.1 | 8.031 | ||
| 2.0 | 0.000 |
By table one, can see clearly that the reduction of resistivity is not that usage quantity with mother alloy is simple linear pattern relation, in the time of high resistivity, the mother alloy consumption changes little; In the low-resistance part, the usage quantity of mother alloy sharply increases.This shows that the accuracy of mixing in advance is to be difficult to hold.
Claims (1)
1. the adulterating method of a monocrystalline silicon for photovoltaics is characterized in that step is as follows:
At first polycrystalline silicon raw material is put into single crystal growing furnace, melt in the protective atmosphere in the main chamber, seed crystal hangs from concubine insertion liquid silicon and gets sample, by isolating major and minor chamber sample is taken out, and tests the electricalresistivity of sample then with four point probe
Little,
The boron concentration N of sample
Little, mother alloy boron concentration Nx, the boron concentration Nm of target resistivity silicon single crystal all calculates by formula 1
N=(1.33E+16/ ρ)+1.082E+17/ ρ * [1+ (54.56 * ρ) ^1.105)] formula 1
Promptly obtain boron concentration N by the electricalresistivity;
Need the mother alloy quality Gx that drops into to calculate by formula 2
Nm * G=N * G+ (Gx ÷ 1000 ÷ 2.33) * Nx * K formula 2
Wherein, G is total charging capacity of polycrystalline silicon raw material, and segregation coefficient K is a constant 0.8;
Utilize Excel software to calculate automatically formula 1 and formula 2, input comprises: target resistivity, the Ω .cm of unit; Total charging capacity G, units; Mother alloy resistivity, the Ω .cm of unit; The electricalresistivity of sample
Little, the Ω .cm of unit; Work output is mother alloy quality Gx, the g of unit; Generate the sample electricalresistivity by Excel software
LittleWith the form of the respective value of mother alloy quality Gx, the workman is according to the sample electricalresistivity who measures
LittleTable look-up and needing to obtain the mother alloy quality Gx of input.
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| CN102181919A (en) * | 2011-04-13 | 2011-09-14 | 天津市环欧半导体材料技术有限公司 | Method for controlling resistivity of head of Czochralski silicon |
| CN102181926A (en) * | 2011-04-08 | 2011-09-14 | 光为绿色新能源有限公司 | Polycrystalline silicon ingot doping method and ingot casting equipment for implementing method |
| CN102817075A (en) * | 2012-08-18 | 2012-12-12 | 安阳市凤凰光伏科技有限公司 | Master alloy production method by using polycrystalline foundry furnace |
| CN103048360A (en) * | 2012-11-30 | 2013-04-17 | 西安隆基硅材料股份有限公司 | Method for measuring concentration of germanium or/and tin impurity in crystalline silicon |
| CN105755533A (en) * | 2016-05-20 | 2016-07-13 | 麦斯克电子材料有限公司 | Method for preparing high-resistance silicon single crystal by Czochralski method |
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| CN102181926A (en) * | 2011-04-08 | 2011-09-14 | 光为绿色新能源有限公司 | Polycrystalline silicon ingot doping method and ingot casting equipment for implementing method |
| CN102181919A (en) * | 2011-04-13 | 2011-09-14 | 天津市环欧半导体材料技术有限公司 | Method for controlling resistivity of head of Czochralski silicon |
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| CN102817075A (en) * | 2012-08-18 | 2012-12-12 | 安阳市凤凰光伏科技有限公司 | Master alloy production method by using polycrystalline foundry furnace |
| CN103048360A (en) * | 2012-11-30 | 2013-04-17 | 西安隆基硅材料股份有限公司 | Method for measuring concentration of germanium or/and tin impurity in crystalline silicon |
| CN103048360B (en) * | 2012-11-30 | 2015-11-25 | 西安隆基硅材料股份有限公司 | Germanium in crystalline silicon is or/and the measuring method of tin impurity concentration |
| CN105755533A (en) * | 2016-05-20 | 2016-07-13 | 麦斯克电子材料有限公司 | Method for preparing high-resistance silicon single crystal by Czochralski method |
| CN106294302A (en) * | 2016-08-10 | 2017-01-04 | 宁夏高创特能源科技有限公司 | A kind of silicon target dispensing regulation polarity, resistivity measuring method |
| CN106294302B (en) * | 2016-08-10 | 2018-10-09 | 宁夏高创特能源科技有限公司 | A kind of silicon target dispensing adjusts polarity, resistivity measuring method |
| CN107492582A (en) * | 2017-07-28 | 2017-12-19 | 山西潞安太阳能科技有限责任公司 | It is a kind of reduction solar battery sheet it is hidden split, the method for sliver |
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Application publication date: 20101208 |