CN106294302B - A kind of silicon target dispensing adjusts polarity, resistivity measuring method - Google Patents
A kind of silicon target dispensing adjusts polarity, resistivity measuring method Download PDFInfo
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- CN106294302B CN106294302B CN201610650014.7A CN201610650014A CN106294302B CN 106294302 B CN106294302 B CN 106294302B CN 201610650014 A CN201610650014 A CN 201610650014A CN 106294302 B CN106294302 B CN 106294302B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 144
- 239000010703 silicon Substances 0.000 title claims abstract description 144
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000013078 crystal Substances 0.000 claims abstract description 78
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 55
- 239000011574 phosphorus Substances 0.000 claims abstract description 54
- 229910052796 boron Inorganic materials 0.000 claims abstract description 53
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000012535 impurity Substances 0.000 claims abstract description 47
- 239000002994 raw material Substances 0.000 claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 claims abstract description 30
- 238000005204 segregation Methods 0.000 claims abstract description 26
- GDFCWFBWQUEQIJ-UHFFFAOYSA-N [B].[P] Chemical compound [B].[P] GDFCWFBWQUEQIJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000009826 distribution Methods 0.000 claims abstract description 19
- 239000002019 doping agent Substances 0.000 claims abstract description 19
- 238000005266 casting Methods 0.000 claims abstract description 18
- 238000007711 solidification Methods 0.000 claims abstract description 13
- 230000008023 solidification Effects 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 8
- 125000004429 atom Chemical group 0.000 claims description 14
- 238000004364 calculation method Methods 0.000 claims description 12
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 7
- 238000009792 diffusion process Methods 0.000 claims description 6
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 5
- 241000894007 species Species 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 3
- 125000004437 phosphorous atom Chemical group 0.000 claims description 3
- 241000208340 Araliaceae Species 0.000 claims description 2
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 claims description 2
- 239000002178 crystalline material Substances 0.000 claims description 2
- 235000008434 ginseng Nutrition 0.000 claims description 2
- 230000000306 recurrent effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 239000002210 silicon-based material Substances 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 description 4
- NAWXUBYGYWOOIX-SFHVURJKSA-N (2s)-2-[[4-[2-(2,4-diaminoquinazolin-6-yl)ethyl]benzoyl]amino]-4-methylidenepentanedioic acid Chemical compound C1=CC2=NC(N)=NC(N)=C2C=C1CCC1=CC=C(C(=O)N[C@@H](CC(=C)C(O)=O)C(O)=O)C=C1 NAWXUBYGYWOOIX-SFHVURJKSA-N 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F40/00—Handling natural language data
- G06F40/10—Text processing
- G06F40/166—Editing, e.g. inserting or deleting
- G06F40/177—Editing, e.g. inserting or deleting of tables; using ruled lines
- G06F40/18—Editing, e.g. inserting or deleting of tables; using ruled lines of spreadsheets
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
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Abstract
A kind of silicon target dispensing adjusts polarity, resistivity measuring method, point 4 steps：1, according to silicon target target polar, resistivity, calculate corresponding boron or phosphorus difference content range；2, a, according to quality, dopant species, the dosage of known different silicon raw materials, the population mean boron phosphorus content of preliminary configuration production silicon target raw material；B, the single crystal growing furnace crystal pulling of selection setting production and application or ingot casting furnace superintendent crystalline substance parameter and effective segregation coefficient；3, theoretical according to directional solidification impurity segregation, measuring and calculating obtains silicon crystal and adulterates difference concentration distribution data per segment length, converses corresponding polarity, resistivity；4, compare measuring and calculating numerical value and silicon target desired value, adjusts silicon raw material dispensing boron phosphorus content again, the parameters of dispensing when finally determining silicon crystal material optimum utilization.This measuring method is simple, quick, reliable, can arbitrarily adjust it is envisioned that silicon target polarity, resistivity, can practical Instructing manufacture, open up silicon material source, greatly improve product utilization rate.
Description
Technical field
The present invention relates to silicon target preparing technical fields, and in particular to a kind of silicon target dispensing adjusts polarity, resistivity is surveyed
Calculation method.
Background technology
Silicon target is a kind of important magnetron sputtering plating target source, be mainly used for glass, plane is shown, photovoltaic,
The fields such as optic communication storage.As magnetron sputtering technology fast development and application field are expanded, the demand of silicon target is increasingly
Increase, market prospects are boundless.But due to the application field of silicon target difference, user requires different, the resistivity of silicon target
Range is wider, such as：1~3 Ω cm ,≤1 Ω cm ,≤0.05 Ω cm ,≤0.02 Ω cm ,≤0.01 Ω cm etc..
How to accurately control electrical resistivity range is technological difficulties and emphasis prepared by silicon target, this is also the technological core of each manufacturer
One of secrecy.
In silicon target makes production, blank raw material polarity, resistivity determine finished product polarity, resistivity (substantially not
Become), blank source is routinely that monocrystalline, polycrystalline pole is made by single crystal growing furnace czochralski method and is made by ingot furnace directional solidification method
Then target is made by cutting, grinding, cleaning in polycrystalline side's ingot.Chinese patent CN10377007A provides a kind of silicon target making
Technique, the column crystal silicon target being prepared by single crystal growing furnace czochralski method, purity is high, does not have crackle, hole and whirlpool；China
Patent CN104451564A provides a kind of method preparing siliceous target using directional solidification processes, is oriented by ingot furnace solidifying
Gu large scale, crystal perfection polycrystalline silicon target is prepared in method.Silicon target dispensing regulation resistance rate is not mentioned in two patents
Method, the latter only mention high-purity polycrystalline silicon raw material (its phosphorus content is almost 0) addition boron dope agent, make boron content in silicon material
For 5~25ppm, p-type can be obtained, the silicon target that resistivity is 0.025~0.05 Ω cm, there is no clearly other range silicon targets
How material polarity, resistivity are adjusted, and how to be adjusted if any phosphorus element content in silicon materials.
Invention content
The purpose of the present invention is to provide a kind of silicon target dispensings to adjust polarity, resistivity measuring method, it is intended to single crystal growing furnace,
When ingot furnace produces silicon target blank raw material, by the control of dopant content in polycrystalline silicon ingredient, required optimal resistance is obtained
Rate material instructs actual production, developing silicon material source, improves product availability, reduces production cost.
Silicon target is a kind of high-purity, low-resistance silicon crystal.In silicon crystal, generally using boron (B) or phosphorus (P) as mixing
Miscellaneous dose, boron phosphorus content in silicon is adjusted, that is, controls boron phosphorus doping amount, resistivity is made to be controlled.In production silicon target blank raw material
When, single crystal growing furnace is drawn belongs to directional solidification scope with ingot casting furnace superintendent crystalline substance, therefore, according to silicon target target polar, resistivity, and
By boron phosphorus doping amount, directional solidification impurity simulates segregation process in silicon, is adulterated in accurately calculating silicon crystal per segment length
Amount, and the key problem in technology that conversion obtains corresponding polarity, resistivity is the present invention.
Realize that technical scheme is as follows：
The present invention applies mechanically computing capability by the powerful spreadsheet formulas of EXCEL softwares, carries out programming calculating, is divided into
4 steps：
1, the 1st step：According to silicon target target polar (p-type or N-type), the resistivity upper limit, lower limit, calculate corresponding boron or
Phosphorus atom concentration, corresponding boron difference content range or phosphorus difference content range.
2, second step：A, it is detected through chemical examination according to the existing opposed polarity of known production, the silicon raw material of resistivity or silicon raw material
Boron phosphorus content, dopant species, dosage, the population mean boron phosphorus content of preliminary configuration production silicon target raw material, boron phosphorus contains
Difference control is measured in the corresponding boron of step 1 target resistivity upper and lower limit or phosphorus difference content range；B, selection setting is practical raw
Single crystal growing furnace crystal pulling parameter or ingot casting furnace superintendent crystalline substance parameter are produced, and setting rate of crystalline growth parameter calculates boron phosphorus effective segregation coefficient.
3, third step：Raw material parameter, production furnace parameters, effective segregation coefficient parameter are tentatively configured according to second step,
And directional solidification impurity segregation is theoretical, theoretical modeling measuring and calculating obtains doping difference concentration distribution of the silicon crystal per segment length, and changes
Calculation obtains corresponding polarity, resistivity.
4, the 4th step：The polarity, resistivity and the silicon target target polar that are obtained according to step 3, resistivity ratio are compared with repeating
Set-up procedure 2 produces the population mean boron phosphorus content of silicon target raw material, and step 3 silicon crystal is accordingly calculated per segment length phase
Polarity, the resistivity answered, when finally determining the best availability of required optimal resistivity, that is, crystalline material, using not in dispensing
The weight of same polarity, the silicon raw material of resistivity, dopant species, dopant weight, the technologies such as boron phosphorus content obtained after dispensing
Parameter.
The silicon raw material requirement：Purity 5N or so or more p-type or N-type polycrystalline silicon, iron, aluminium in silicon raw material,
The fewer the metals content impurities such as calcium the better, and silicon target quality on the one hand can be improved in this way；On the one hand it in theoretical calculation, can be ignored
The micro influence that metal impurities bring resistivity.
The dopant is boron master alloy, phosphorus master alloy, 6N grades of high purity boron powder, and when theoretical calculation only selects one of which
It inputs, i.e., need to produce P-type silicon target and use boron master alloy or high purity boron powder, N-type silicon target need to be produced and use phosphorus master alloy.
The measuring method, theoretical calculation do not consider the vacuum effumability of P elements impurity, in measuring and calculating N-type silicon target
Afterwards, when instructing actual production, the volatile quantity of P elements impurity should numerically be increased in results of measuring.
Measuring method advantage of the present invention is：
1) it is configured silicon raw material parameter adjustment, is simulated and is segregated by directional solidification impurity, can accurately calculate to obtain boron and phosphorus
The crystal distribution difference concentration data of matter, and convert and obtain every section of crystal polarity, resistivity.Reached it is arbitrary adjust it is envisioned that
Silicon target polarity, the purpose of resistivity.
2) present invention is used because polarity, resistivity meet silicon target improving silicon target blank availability significant effect
It is required that crystal pulling crystal bar, ingot casting silicon ingot blank can whole utilizations.
3) present invention carries out table prgraming program calculating by EXCEL softwares, and measuring method is simple, quick, reliable, can be real
It is horizontal to improve production technology for border Instructing manufacture.
4) present invention can be according to existing opposed polarity, resistivity silicon raw material progress dispensing be produced, can also be according to city
Field heavily B doped p-doped difference silicon raw material quality carries out dispensing, opens up silicon material source significantly.
5) measuring method of the present invention can equally be well applied to the crystal pulling of photovoltaic industry solar cell material and ingot casting technology is led
Domain.
Description of the drawings
Fig. 1 is the 1st step of measuring method, silicon target target polar, resistivity boron phosphorus difference content range computational chart；
Fig. 2 is measuring method second step a, and the parameters such as configuration silicon target raw material population mean boron phosphorus content, weight calculate
Table；
Fig. 3 is measuring method second step b, and silicon target production furnace parameters and effective segregation coefficient computational chart is arranged；
Fig. 4 is measuring method third step, and theoretical modeling calculates crystal pulling crystal bar or ingot casting silicon ingot silicon crystal per segment length pole
Property, resistivity computational chart.
Fig. 1~4 are Excel software programming computation sheets, are an organic wholes, and it is that silicon target dispensing is adjusted to merge
Polarity, the Excel software table program calculation programs of resistivity measuring method.
1) in Fig. 1,2,3, i.e., the 1st, in 2a, 2b step computational chart, it is variable number to have the numerical value of light colour fills unit lattice
Value need to input given data or setting numerical parameter, and no color filling cell numerical value, which is result of calculation numerical value, (please don't individually repair
Change).After variable value input, result of calculation numerical value can apply mechanically formula according to program and make corresponding calculating variation.
2) in Fig. 2, i.e., in 2a steps computational chart, there are two two kinds of distributions of table, and wherein distribution one is
Know polarity, the resistivity for producing existing silicon raw material, select a kind of dopant, adjusts each gravimetric value and calculate dispensing parameter；Dispensing
Method two is the boron phosphorus content of known existing silicon raw material chemical examination detection, selects a kind of dopant, adjusts each gravimetric value accounting and matches
Expect parameter.Distribution one is such as selected, inputs " 1 " in the first unit lattice of the upper left corner in one computation sheet of distribution, " dispensing
One " text unit lattice of method have automatically become light colour filling, in two computation sheet of distribution in the first unit lattice of the upper left corner
It automatically becomes " 0 "；Distribution two is such as selected, " 0 " is inputted in the first unit lattice of the upper left corner in one computation sheet of distribution,
" distribution two " text unit lattice have automatically become light colour filling, upper left corner first unit in two computation sheet of distribution
It is automatically become in lattice " 1 ".
3) in Fig. 2, i.e., in 2a steps computational chart, there are two two kinds of distributions of table, and " dispensing obtains silicon raw material ginseng
Number " is respectively in the two table lower right corner, including raw material weight, volume, boron concentration, corresponding boron content, phosphorus concentration, corresponding phosphorus content six
A parameter.Such as configure P-type silicon target raw material, in parameter " corresponding boron content " subtract " corresponding phosphorus content " should be in the 1st step on
Lower limit corresponds in the content range of boron difference；N-type silicon target raw material is such as configured, " corresponding phosphorus content " subtracts " corresponding boron in parameter
Content " should be in the content range that bound corresponds to phosphorus difference in the 1st step.
4) in Fig. 3, i.e., in 2b steps computational chart, top is there are two table, when crystal pulling parameter list, second is that ingot casting parameter
Table.Actual production inputs " 1 " in crystal pulling parameter list as used single crystal growing furnace crystal pulling in upper left corner first unit lattice, and " crystal pulling is joined
Number " text unit lattice have automatically become light colour filling, are automatically become " 0 " in the first unit lattice of the upper left corner in ingot casting parameter list；
Actual production inputs " 0 " in crystal pulling parameter list as used polycrystalline ingot furnace ingot casting in upper left corner first unit lattice, and " ingot casting is joined
Number " text unit lattice have automatically become light colour filling, are automatically become " 1 " in the first unit lattice of the upper left corner in ingot casting parameter list.
5) in Fig. 4, i.e. all result of calculation of third step computational chart is according to 2a, 2b step parameter setup algorithm
As a result, 0,1,2,3,4 ... n numerical value of the 1st row in table, representative is the long chip of silicon crystal to being crystal bar when length, i.e. crystal pulling
For silicon ingot, every the height of 1cm, (1cm is of the invention from bottom to top when the length of 1cm, ingot casting from head to tail portion
Preferred value)；Fig. 4 measuring and calculating emphasis result sees that " polarity " and " resistivity ", numerical value cell are filled out with light colour in the row of table the 2nd, 3
It fills and highlights, need with the 1st step target polar, resistivity ratio compared with the 4th step of progress repeats to adjust.
Specific implementation mode
In order to make those skilled in the art more fully understand the present invention program, enable objects, features and advantages of the present invention
It is more obvious and easy to understand, below invention is further described in detail.
The present invention relates to theoretical calculation main formulas three categories：
First, according to semiconductor equipment material industry association SEMI MF723-99 and standard GB/T/T 13389-
1992 boron-doping p-doped single crystal silicon resistivities and formula in concentration of dopant conversion regulation：
1) boron-doping silicon single crystal calculates concentration of dopant value, i.e. p-type resistivity to concentration by resistivity value：
In formula：ρ --- resistivity, Ω cm；N --- concentration of dopant, atoms/cm3.
2) p-doped silicon single crystal calculates concentration of dopant value, i.e. N-type resistivity to concentration by resistivity value：
In formula：χ=log10ρ；A0=-3.1083；
A1=-3.2626；B1=1.0265；
A2=-1.2196；B2=0.38755；
A3=-0.13923；B3=0.041833.
3) boron-doping silicon single crystal calculates resistivity value, i.e. p-type concentration to resistivity by concentration of dopant value：
4) p-doped silicon single crystal calculates resistivity value, i.e. N-type concentration to resistivity by concentration of dopant value：
In formula：Y=(log10N)-16；A ' 0=-3.0769；
A ' 1=2.2108；B ' 1=-0.68157；
A ' 2=-0.62272；B ' 2=0.19833；
A ' 3=0.057501；B ' 3=-0.018376.
Second is that boron and phosphorus matter atomic concentration and the mutual conversion formula of content in silicon：
1) boron impurity atomic concentration is converted to content in silicon：
MB=NB ÷ (5 × 1022) × 10.81 ÷ 28.09 × 106 ... ... ... formula (5)
In formula：MB --- boron impurity content, ppmw；NB --- boron impurity concentration, atoms/cm3.
2) phosphorus impurity atoms concentration is converted to content in silicon：
MP=NP ÷ (5 × 1022) × 30.97 ÷ 28.09 × 106 ... ... ... formula (6)
In formula：MP --- phosphorus impurities content, ppmw；NP --- phosphorus impurities concentration, atoms/cm3.
3) boron impurity content is converted to atomic concentration in silicon：
10.81 ÷ 106 ... ... ... ... formula (7) of NB=MB × 5 × 1022 × 28.09 ÷
4) phosphorus impurities content is converted to atomic concentration in silicon：
30.97 ÷ 106 ... ... ... ... formula (8) of NP=MP × 5 × 1022 × 28.09 ÷
In formula (5)~(8)：5 × 1022 be the atom or molecular density of silicon, unit/cm3；28.09 be the atom of silicon
Amount；10.81 be the atomic weight of boron；30.97 be the atomic weight of phosphorus.
Third, impurity directional solidification segregates theoretical formula in silicon：
1) effective segregation coefficient Keff and equilibrium segregation coefficient K0 abides by BPS relational expressions：
In formula：K0 is equilibrium segregation coefficient, and Keff is effective segregation coefficient, and δ is thickness of diffusion layer, and D is that impurity is molten in silicon
Diffusion coefficient in body, f are rate of crystalline growth.The present invention searches document Optimal Parameters and is set as：The K0 of boron is 0.8, phosphorus
K0 is 0.35；The δ of boron is 0.01mm, and the δ of phosphorus is 0.01mm；The D of boron is 4.00 × 10-5cm2/s, and the D of phosphorus is 2.80 × 10-
5cm2/s；Crystal average growth rate f is routinely 1~2mm/min.
2) solid impurity concentration C S and melt impurity concentration CL relational expressions：
CS=Keff × CL ... ... ... ... ... ... formula (10)
Silicon target dispensing adjusts polarity, resistivity measuring method Excel software table program calculation journeys below in conjunction with the accompanying drawings
Sequence explanation：
1) it in Fig. 1, i.e. in the 1st step computational chart, according to silicon target target polar, the resistivity upper limit, lower limit, calculates pair
Answer boron or phosphorus atom concentration, corresponding boron difference content range or phosphorus difference content range.P-type resistivity involved in table is to dense
In degree formula (1), N-type resistivity to concentration formula (2) and silicon boron or phosphorus impurity atoms concentration be converted to content formula (5),
(6)；
2) in Fig. 2, i.e., in 2a steps computational chart, according to the existing opposed polarity of known production, resistivity silicon raw material or
Boron phosphorus content of the silicon raw material through chemical examination detection, dopant species, dosage, configuration calculate production silicon target raw material parameter.In table
It is dense to also relate to boron or phosphorus impurity atoms in p-type resistivity to concentration formula (1), N-type resistivity to concentration formula (2) and silicon
Degree is converted to boron or phosphorus impurities content in content formula (5), (6) and silicon and is converted to atomic concentration formula (7), (8), also
The mutual conversion of following equation is applied：
Volume (cm3)=weight (g) ÷ solid silicons density (for 2.329g/cm3)
Amount of impurities (atoms)=impurity concentration (atoms/cm3) × volume (cm3)
Silicon raw material gross weight in 2a step computational charts is determined per stove charge by specifically producing the type of furnace, conventional 80
Stove single crystal growing furnace list stove charge 60Kg or so, 90 stove single crystal growing furnace 100Kg or so, maximum single crystal growing furnace once feeds currently on the market
Amount can reach 300Kg or so；Polycrystalline ingot furnace list stove charge has 450Kg, 500Kg, 800Kg, 1000Kg or so etc..
3) in Fig. 3, i.e., in 2b steps computational chart, selection setting actual production single crystal growing furnace crystal pulling parameter or ingot casting furnace superintendent are brilliant
Parameter, and setting rate of crystalline growth parameter calculate boron phosphorus effective segregation coefficient.Two table of top is that selection production method is single
Brilliant stove crystal pulling or polycrystalline furnace ingot casting, if boule diameter need to be arranged in crystal pulling, normal ranges are 50~300mm, as ingot casting needs to be arranged
Silicon ingot length and width determines that conventional crucible is rectangular, and length is equal with width, and G5 crucible internal diameters are by specifically producing type of furnace crucible internal diameter
840 × 840mm, G6 are 1000 × 1000mm.According to dispensing total weight, boule length or silicon ingot height, unit length are calculated
Volume, unit weight, preferred unit length of the present invention are 1cm.Following equation involved in two table of top：(wherein length
That is height)
Boule length or silicon ingot height (cm)=throwing stove raw material weight (g) ÷ unit weights (g/cm)
Crystal bar unit length volume (cm3/cm)=3.14 × diameter square (mm2) ÷, 4 × 1 (cm) ÷ 100
Silicon ingot unit height volume (cm3/cm)=silicon ingot length × wide (mm2) × 1 (cm) ÷ 100
Unit weight (g/cm)=unit length volume (cm3/cm) × solid silicon density (for 2.329g/cm3)
Effective segregation coefficient Keff involved in the table of lower part and equilibrium segregation coefficient K0 relation formulas (9), give birth to according to crystal
Long speed f calculates separately out the effective segregation coefficient Keff of boron and phosphorus.
4) in Fig. 4, i.e., in third step computational chart, raw material parameter is configured according to second step, production furnace parameters, is effectively divided
Solidifying figure parameters and directional solidification impurity segregation are theoretical, and theoretical modeling measuring and calculating show that doping difference of the silicon crystal per segment length is dense
Degree distribution, and convert and obtain corresponding polarity, resistivity.Solid impurity concentration C S involved in table is closed with melt impurity concentration CL
It is formula (10) and p-type concentration to resistivity formula (3), N-type concentration to resistivity formula (4), cycle calculations are public in table
Formula is as follows：
Epicycle clout weight=above take turns clout weight-unit weight
Epicycle clout volume=epicycle clout weight ÷ solid silicon density
Epicycle solidification impurity=unit length volume × above take turns clout concentration × Keff
Epicycle despumation=unit length volume × above take turns clout concentration × (1-Keff)
(wherein, Keff is boron or phosphorus effective segregation coefficient；Upper wheel clout concentration × Keff is this section of crystal concentration, is
Formula (10) is applied)
Clout concentration=(epicycle clout volume × above wheel clout concentration+epicycle despumation) ÷ epicycle clout volumes
This section of crystal concentration=epicycle solidification impurity ÷ unit lengths volume=above takes turns clout concentration × Keff
The absolute value of this section of crystal difference concentration=(this section of crystal phosphorus impurities of crystalline boron impurity concentration-this section concentration)
When this section of crystal phosphorus impurities concentration of this section of crystalline boron impurity concentration ＞, this section of crystal is p-type, is otherwise N-type.According to
This section of crystal difference concentration converses this section of crystal resistivity (i.e. p-type concentration to resistivity formula (3), N-type concentration to resistance
The application of rate formula (4)).
Example 1：The a diameter of Ф 170mm crystal bars of a stove, p-type, 0.02~0.01 Ω of resistivity are produced using 90 single crystal growing furnaces
The silicon target blank material of cm, it is known that single crystal growing furnace list stove inventory is 100Kg or so, and crystal pulling crystal average growth rate is
1.2mm/min, how dispensing obtains optimal material utilization rate for measuring and calculating.
It is analyzed through silicon target dispensing adjusting polarity, resistivity measuring method Excel software table program calculation programs, the 1st
Step obtains p-type, 0.02~0.01 Ω cm silicon targets of resistivity, and corresponding boron difference content range is 24.93~
65.32ppmw；2b steps obtain 100Kg silicon materials and can draw Ф 170mm crystal bars length to be about 1816mm, the effective segregation coefficient of boron
Keff is 0.8079, and the effective segregation coefficient Keff of phosphorus is 0.3664；It is adjusted repeatedly through 2a steps distribution two and third step
Whole measuring and calculating obtains, as 0.01 Ω cm of crystal bar head resistivity summary ＜ 0.02 Ω cm, tail portion ＞, when whole crystal bar is p-type, i.e.,
When silicon target blank availability is 100%, the content for preparing boron in the silicon raw material for adding up to 100Kg answers >=32.5ppmw, phosphorus
Content should be within the scope of 0~4ppmw；Through 2a steps distribution one can also calculate actual production using opposed polarity,
The ingredients by weight of resistivity silicon raw material and the weight for using boron master alloy or high purity boron powder.
Above-mentioned results of measuring data are shown in the data in attached drawing, and actual production is instructed using the results of measuring technical parameter, system
Number of actual measurements value and the results of measuring for obtaining crystal bar are almost the same.
Example 2：840 × the side 840mm of a stove silicon ingot, N-type, resistivity ＜ 0.2 Ω cm are produced using polycrystalline ingot furnace
Silicon target blank material, it is known that ingot furnace list stove inventory is 500Kg or so, and cast ingot crystals average growth rate is 1.6mm/
Min, how dispensing obtains optimal material utilization rate for measuring and calculating.
It is analyzed through silicon target dispensing adjusting polarity, resistivity measuring method Excel software table program calculation programs, the 1st
Step obtains N-type, resistivity 0.2~0.02 (setting value) Ω cm silicon targets, and corresponding phosphorus difference content range is 0.68~
28.94ppmw；2b steps obtain 500Kg silicon materials can the 840 × side 840mm of ingot casting silicon ingot height be about 304mm, boron effectively point
Solidifying COEFFICIENT K eff is 0.8105, and the effective segregation coefficient Keff of phosphorus is 0.3720；Through 2a steps distribution two and third step
Adjustment measuring and calculating repeatedly obtains, and prepares content >=3.8ppmw of phosphorus in the silicon raw material for adding up to 500Kg, the content of boron 0~
When within the scope of 0.3ppmw, 0.2 Ω cm of silicon ingot bottom resistance rate ＜, the equal 0.03 Ω cm of ＞ in top, monoblock silicon ingot are N-type, i.e.,
Silicon target blank availability is 100%.Actual production, which can also be calculated, through 2a steps distribution one uses not homopolarity
Property, resistivity silicon raw material ingredients by weight and using phosphorus master alloy weight.
In view of phosphorus is about 1/3 in ingot furnace vacuum volatilization, actual production is instructed using above-mentioned results of measuring technical parameter
When answer divided by 2/3, i.e., the ÷ 2/3=5.7ppmw of phosphorus content >=3.8, value are used for actual production, the practical measurement of silicon ingot are made
Numerical value is almost the same with results of measuring.
Described in above example, specific implementation example only of the invention.The present invention is programmed into row by EXCEL software tables
Program calculates, and can also be calculated certainly into line program by other computer softwares or programming software, protection scope of the present invention is simultaneously
Not limited to this, any one skilled in the art in the technical scope disclosed by the present invention, can readily occur in
Change or replacement should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of silicon target dispensing adjusts polarity, resistivity measuring method, it is characterised in that：The measuring method is soft by EXCEL
The powerful spreadsheet formulas of part applies mechanically computing capability, carries out programming calculating, is divided into 4 steps：
1st step：According to silicon target target polar p-type or N-type, the resistivity upper limit, lower limit, calculates corresponding boron or phosphorus atoms are dense
Degree, corresponding boron difference content range or phosphorus difference content range；
Second step：A, according to the existing opposed polarity of known production, the boron phosphorus of silicon raw material or silicon raw material through chemical examination detection of resistivity
Content, dopant species, dosage, the population mean boron phosphorus content of preliminary configuration production silicon target raw material, boron phosphorus content difference
Control is in the corresponding boron of the 1st step target resistivity upper and lower limit or phosphorus difference content range；B, selection setting actual production list
Brilliant stove crystal pulling parameter or ingot casting furnace superintendent crystalline substance parameter, and setting rate of crystalline growth parameter calculate boron phosphorus effective segregation coefficient；
Third step：Raw material parameter, production furnace parameters, effective segregation coefficient parameter, and orientation are tentatively configured according to second step
Impurity segregation theory is solidified, theoretical modeling measuring and calculating obtains doping difference concentration distribution of the silicon crystal per segment length, and converts and obtain
Corresponding polarity, resistivity；
4th step：The polarity, resistivity and the silicon target target polar that are obtained according to third step, resistivity ratio are compared with repeating to adjust
Second step produces the population mean boron phosphorus content of silicon target raw material, and third step silicon crystal is accordingly calculated per segment length phase
Polarity, the resistivity answered, when finally determining the best availability of required optimal resistivity, that is, crystalline material, using not in dispensing
The weight of same polarity, the silicon raw material of resistivity, dopant species, dopant weight, the boron phosphorus content technology ginseng obtained after dispensing
Number.
2. measuring method according to claim 1, it is characterised in that：The silicon raw material requirement：Purity is in 5N or more
P-type or N-type polycrystalline silicon.
3. measuring method according to claim 1, it is characterised in that：The dopant be boron master alloy, phosphorus master alloy,
6N grades of high purity boron powder, when theoretical calculation, only select one of which, that is, produce P-type silicon target and use boron master alloy or high purity boron powder,
It produces N-type silicon target and uses phosphorus master alloy.
4. measuring method according to claim 1, it is characterised in that：Boron and phosphorus matter atomic concentration and content in the silicon
Mutually converting calculation formula is：
1）Boron impurity atomic concentration is converted to content in silicon：
MB = NB÷（5×1022）×10.81÷28.09×106；
In formula：MB--- boron impurity content, ppmw；NB--- boron impurity concentration, atoms/cm3；
2) phosphorus impurity atoms concentration is converted to content in silicon：
MP = NP÷（5×1022）×30.97÷28.09×106；
In formula：MP--- phosphorus impurities content, ppmw；NP--- phosphorus impurities concentration, atoms/cm3；
3）Boron impurity content is converted to atomic concentration in silicon：
NB = MB ×5×1022×28.09÷10.81÷106；
4）Phosphorus impurities content is converted to atomic concentration in silicon：
NP = MP ×5×1022×28.09÷30.97÷106；
In formula：5×1022For the atom or molecular density of silicon, unit/cm3；28.09 be the atomic weight of silicon；10.81 being boron
Atomic weight；30.97 be the atomic weight of phosphorus.
5. measuring method according to claim 1, it is characterised in that：In second step b, the calculating boron phosphorus effectively divides
In solidifying coefficient, it is set as through searching document parameter：The equilibrium segregation coefficient K of boron0It is 0.8, the equilibrium segregation coefficient K of phosphorus0For
0.35；The thickness of diffusion layer δ of boron is 0.01mm, and the thickness of diffusion layer δ of phosphorus is 0.01mm；The diffusion coefficient D of boron is 4.00 × 10- 5cm2The diffusion coefficient D of/s, phosphorus are 2.80 × 10-5cm2/s；Crystal average growth rate f is 1~2mm/min.
6. measuring method according to claim 1, it is characterised in that：In second step b, calculates boule length or silicon ingot is high
Degree, unit length volume, unit weight, unit length 1cm are related to following equation：
Boule length or silicon ingot height（cm）=throw stove raw material weight（g）÷ unit weights（g/cm）；
Crystal bar unit length volume（cm3/cm）=3.14 × diameter square (mm2) ÷4×1(cm)÷100；
Silicon ingot unit height volume（cm3/cm）=silicon ingot length × wide (mm2) ×1(cm)÷100；
Unit weight（g/cm）=unit length volume（cm3/cm）× solid silicon density；
Wherein solid silicon density is 2.329g/cm3。
7. measuring method according to claim 1, it is characterised in that：In third step, theoretical modeling calculate crystal pulling crystal bar or
Ingot casting silicon ingot silicon crystal is related to recurrent formula per in segment length polarity, resistivity computation sheet：
Epicycle clout weight=above take turns clout weight-unit weight；
Epicycle clout volume=epicycle clout weight ÷ solid silicon density；
Epicycle solidification impurity=unit length volume × above take turns clout concentration × Keff；
The wheel clout of epicycle despumation=unit length volume × above concentration ×（1-Keff）；
Clout concentration=（Epicycle clout volume × above wheel clout concentration+epicycle despumation）÷ epicycle clout volumes；
This section of crystal concentration=epicycle solidification impurity ÷ unit lengths volume=above takes turns clout concentration × Keff；
This section of crystal difference concentration=（This section of crystal phosphorus impurities concentration of crystalline boron impurity concentration-this section）Absolute value；
K in above-mentioned formulaeffFor boron or phosphorus effective segregation coefficient.
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| CN109735896A (en) * | 2019-03-22 | 2019-05-10 | 内蒙古中环协鑫光伏材料有限公司 | A method of it improving monocrystalline silicon resistivity and controls precision |
| CN112986685B (en) * | 2021-02-09 | 2023-11-10 | 西安奕斯伟材料科技股份有限公司 | Method and device for measuring resistivity of monocrystalline silicon rod |
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