CN109738451A - A kind of selective mechanisms method of list, polycrystalline silicon material - Google Patents
A kind of selective mechanisms method of list, polycrystalline silicon material Download PDFInfo
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Abstract
The present invention relates to a kind of selective mechanisms methods of list, polycrystalline silicon material.This method includes the following steps: step 1: the verification of virgin polycrystalline silicon supplied materials, step 2: artificial Rough Inspection raw material, step 3: raw material examining, step 4: raw material resistivity examining, step 5: the inspection of raw material impurity essence, step 6: material carbon oxygen concentration detection, step 7: raw material minority carrier life time detection, step 8: the detection of raw material base metal impurity content, step 9: packaging and warehousing, according to above-mentioned record data.This method scientific and precise, logicality is strong, and detection comprehensively, can filter out the silicon material of high quality.
Description
Technical field
The present invention relates to silicon material technical field of quality detection more particularly to a kind of selective mechanisms methods of list, polycrystalline silicon material.
Background technique
A kind of patent of the quality judging method of polycrystal silicon ingot, patent Shen are disclosed in existing Chinese patent database
Please number be 201510293032.X, patent application day be 2015.06.01, Authorization Notice No. CN104866975B, authorized announcement date
For 2018.04.24, structure includes following operating procedure: (1) by polycrystal silicon ingot evolution be processed into middle part containing polycrystal silicon ingot,
The polysilicon block of edge and corner different subregions；(2) using microwave photoconductive decay minority carrier life time scanner to the more of step (1)
Crystal silicon block carries out surface scan detection；(3) acquisition, processing step (2) Scanning Detction the data obtained, are calculated silico briquette and lack the sub- longevity
Order the factor, silico briquette minority carrier life time standard deviation factor, the lower minority carrier life time scale factor of silico briquette and the lower minority carrier life time in silico briquette bottom
Scale factor；(4) each data factor for obtaining step (3) brings following calculation formula into, calculates mass fraction: F (X)=X1
In the formula of × 18%+X2 × 20%+X3 × 40%+X4 × 22%: X1 is the silico briquette minority carrier life time factor；X2 is silico briquette minority carrier life time mark
The quasi- difference factor；X3 is the lower minority carrier life time scale factor of silico briquette；X4 is the lower minority carrier life time scale factor in bottom；(5) consider silicon
The influence in ingot edge containment region, the silico briquette mass fraction F (X) being calculated with step (4) is multiplied by polycrystal silicon ingot locating for silico briquette
In the parameter of corresponding each subregion obtain final comprehensive quality score；The parameter of each subregion are as follows: in the middle part of polycrystal silicon ingot
The partitioned parameters of silico briquette are 1；Partitioned parameters in polycrystal silicon ingot edge silico briquette are the arbitrary value in 0.95-0.97；In more
The partitioned parameters of crystal silicon ingot corner silico briquette are the arbitrary value of 0.7-0.81；(6) according to the final comprehensive quality score of step (5) to silicon
Block quality carries out judgement stepping；Step (3) the silico briquette minority carrier life time factor is silico briquette head, silico briquette tail portion minority carrier life time does not conform to
The inverse of the average value of the minority carrier life time in lattice region and silico briquette minority carrier life time effective coverage × silico briquette minority carrier life time effective coverage
Minority carrier life time average value × constant A product, the constant A are 0.1-1；The unqualified region of minority carrier life time is minority carrier life time
Range is the region of 0-3us；Step (3) the silico briquette minority carrier life time standard deviation factor is lower than silico briquette minority carrier life time effective coverage
The product of the inverse and a constant B of the standard deviation of the minority carrier life time of minority carrier life time average value, the constant B are 10-20；Step
(3) the lower minority carrier life time scale factor of the silico briquette is few son lower than silico briquette minority carrier life time effective coverage minority carrier life time average value
The product of the inverse and a constant C of service life proportion, the constant C are 35-45；Step (3) the silico briquette bottom is lower few
The scale factor in sub- service life is the inverse of the minority carrier life time proportion low compared with minority carrier life time within the scope of the 100-150mm of silico briquette bottom
With the product of a constant D, the constant D is 35-45.Disadvantage is that: this method only detects silicon material minority carrier life time, and
The all data and structure of the detection silicon material of non-holonomic system, therefore screening technique is not rigorous.
Summary of the invention
The purpose of the present invention is in view of the deficienciess of the prior art, providing a kind of the single, more of screening more scientific and precise
Crystal silicon material selective mechanisms method.
To achieve the goals above, the technical solution taken of selective mechanisms method of a kind of list of the present invention, polycrystalline silicon material:
A kind of selective mechanisms method of list, polycrystalline silicon material, including the following steps:
Step 1: virgin polycrystalline silicon supplied materials is checked, manufacturer, lot number, rule in operator's verification raw material outer packing
Lattice, quantity check whether packaging is intact, and whether there is or not deformation, polyethylene packaging bag is whether there is or not breakage, and whether there is or not extraneous contaminations for raw material, if
Raw material is unqualified, directly retracts, otherwise enters step two；
Step 2: artificial Rough Inspection raw material, operator dismantle raw material outer packing one by one, check the structure and table of raw material
Face, it is ensured that surface color is normal, impulse- free robustness, non-oxidation sandwich, without fusible core phenomenon, carbon head material remains without graphite, without metal and
Nonmagnetic substance, chunk polysilicon linear dimension are 6mm-100mm, the size distribution ranges of chunk polysilicon are as follows: (a) linear ruler
The very little chunk polysilicon for 6mm-25mm has 0-15 parts by weight, and (b) linear dimension is that the chunk polysilicon of 25mm-50mm has 15-
35 parts by weight, (c) linear dimension is that the chunk polysilicon of 50mm-100mm has 65-100 parts by weight；
Step 3: raw material examining, operator check original using the raw material in infrared inspection instrument one by one detecting step two
Whether material is internal crack, impurity, stain, shade, crystallite, and the result that each raw material scans on infra-red inspection instrument is recorded in
Volume is separately stored, is stayed with stand-by；
Step 4: the raw material in step 3 is successively placed on resistance type measuring instrument, uses electricity by raw material resistivity examining
Categorical measures instrument is hindered to measuring at each raw edges 4mm, according to the data of resistance type measuring instrument, counts p-type raw material
Or N-type raw material and record it is on the regular payroll, separately store, stay with stand-by, N-type raw material base phosphorus resistivity p be 30 Ω .cm-50 Ω .cm, p-type
The raw material base phosphorus resistivity Ω of p >=50 .cm；
Step 5: the raw material in step 4 is successively used chemical vapour deposition technique to examine body impurity by the inspection of raw material impurity essence
Content alms giver data and body impurity content are by master data, according to the data of detection, count qualified raw material and record it is on the regular payroll,
Separately storage, is stayed with stand-by, in equal < 7.74ppba of P, As and Sb, body impurity content acceptor in body impurity content alms giver
The equal < 2.7ppba of B and Al；
Step 6: the detection of material carbon oxygen concentration, using each in list, polysilicon oxygen and carbon content tester successively measuring process five
The oxygen concentration and concentration of carbon of raw material, it is ensured that oxygen concentration≤1.0*1017/cm3, concentration of carbon≤5.0*1016/cm3, according to list, polycrystalline
The data of silicon oxygen and carbon content tester, count the carbon oxygen concentration of each raw material and record it is on the regular payroll, separately store, stay with stand-by；
Step 7: the detection of raw material minority carrier life time uses the minority of raw material in minority carrier life time detector successively detecting step six
Carrier lifetime, minority carrier lifetime >=10us, according to the data of detection, count qualified raw material and record it is on the regular payroll, point
Storage is opened, is stayed with stand-by；
Step 8: the detection of raw material base metal impurity content is successively examined using silicon material parent metal impurity content tester
The base metal impurity content of raw material in step 7 is surveyed, base metal impurity includes Fe, Cr, Ni, Cu, Zn, Na, TMI <
0.5ppmw successively records the data of each raw material, separately stores, stays with stand-by；
Step 9: qualified silicon material is successively sorted out vanning, is laid with bubble in cabinet by packaging and warehousing according to above-mentioned record data
Foam pad or carton carry out buffer protection, and cabinet is wound fastening using PE film outside.
Compared with prior art, the invention has the benefit that this method scientific and precise, logicality is strong, detection is comprehensive, energy
Enough filter out the silicon material of high quality.
Specific embodiment
A kind of selective mechanisms method of list, polycrystalline silicon material, including the following steps:
Step 1: virgin polycrystalline silicon supplied materials is checked, manufacturer, lot number, rule in operator's verification raw material outer packing
Lattice, quantity check whether packaging is intact, and whether there is or not deformation, polyethylene packaging bag is whether there is or not breakage, and whether there is or not extraneous contaminations for raw material, if
Raw material is unqualified, directly retracts, otherwise enters step two；
Step 2: artificial Rough Inspection raw material, operator dismantle raw material outer packing one by one, check the structure and table of raw material
Face, it is ensured that surface color is normal, impulse- free robustness, non-oxidation sandwich, without fusible core phenomenon, carbon head material remains without graphite, without metal and
Nonmagnetic substance, chunk polysilicon linear dimension are 6mm-100mm, the size distribution ranges of chunk polysilicon are as follows: (a) linear ruler
The very little chunk polysilicon for 6mm-25mm has 0-15 parts by weight, and (b) linear dimension is that the chunk polysilicon of 25mm-50mm has 15-
35 parts by weight, (c) linear dimension is that the chunk polysilicon of 50mm-100mm has 65-100 parts by weight；
Step 3: raw material examining, operator check original using the raw material in infrared inspection instrument one by one detecting step two
Whether material is internal crack, impurity, stain, shade, crystallite, and the result that each raw material scans on infra-red inspection instrument is recorded in
Volume is separately stored, is stayed with stand-by；
Step 4: the raw material in step 3 is successively placed on resistance type measuring instrument, uses electricity by raw material resistivity examining
Categorical measures instrument is hindered to measuring at each raw edges 4mm, according to the data of resistance type measuring instrument, counts p-type raw material
Or N-type raw material and record it is on the regular payroll, separately store, stay with stand-by, N-type raw material base phosphorus resistivity p be 30 Ω .cm-50 Ω .cm, p-type
The raw material base phosphorus resistivity Ω of p >=50 .cm；
Step 5: the raw material in step 4 is successively used chemical vapour deposition technique to examine body impurity by the inspection of raw material impurity essence
Content alms giver data and body impurity content are by master data, according to the data of detection, count qualified raw material and record it is on the regular payroll,
Separately storage, is stayed with stand-by, in equal < 7.74ppba of P, As and Sb, body impurity content acceptor in body impurity content alms giver
The equal < 2.7ppba of B and Al；
Step 6: the detection of material carbon oxygen concentration, using each in list, polysilicon oxygen and carbon content tester successively measuring process five
The oxygen concentration and concentration of carbon of raw material, it is ensured that oxygen concentration≤1.0*1017/cm3, concentration of carbon≤5.0*1016/cm3, according to list, polycrystalline
The data of silicon oxygen and carbon content tester, count the carbon oxygen concentration of each raw material and record it is on the regular payroll, separately store, stay with stand-by；
Step 7: the detection of raw material minority carrier life time uses the minority of raw material in minority carrier life time detector successively detecting step six
Carrier lifetime, minority carrier lifetime >=10us, according to the data of detection, count qualified raw material and record it is on the regular payroll, point
Storage is opened, is stayed with stand-by；
Step 8: the detection of raw material base metal impurity content is successively examined using silicon material parent metal impurity content tester
The base metal impurity content of raw material in step 7 is surveyed, base metal impurity includes Fe, Cr, Ni, Cu, Zn, Na, TMI <
0.5ppmw successively records the data of each raw material, separately stores, stays with stand-by；
Step 9: qualified silicon material is successively sorted out vanning, is laid with bubble in cabinet by packaging and warehousing according to above-mentioned record data
Foam pad or carton carry out buffer protection, and cabinet is wound fastening using PE film outside.
The present invention is not limited to the above embodiments, on the basis of technical solution disclosed by the invention, the skill of this field
For art personnel according to disclosed technology contents, one can be made to some of which technical characteristic by not needing creative labor
A little replacements and deformation, these replacements and deformation are within the scope of the invention.
Claims (1)
1. a kind of selective mechanisms method of list, polycrystalline silicon material, characterized in that it comprises the following steps:
Step 1: virgin polycrystalline silicon supplied materials is checked, manufacturer, lot number, specification, number in operator's verification raw material outer packing
Amount checks whether packaging is intact, and whether there is or not deformation, polyethylene packaging bag is whether there is or not breakage, and whether there is or not extraneous contaminations for raw material, if raw material is not
Qualification is directly retracted, otherwise enters step two；
Step 2: artificial Rough Inspection raw material, operator dismantle raw material outer packing one by one, check structure and the surface of raw material, really
Protect surface color normal, impulse- free robustness, non-oxidation sandwich, without fusible core phenomenon, carbon head material remains without graphite, without metal and nonmagnetic
Substance, chunk polysilicon linear dimension are 6mm-100mm, the size distribution ranges of chunk polysilicon are as follows: (a) linear dimension is
The chunk polysilicon of 6mm-25mm has 0-15 parts by weight, and (b) chunk polysilicon that linear dimension is 25mm-50mm has 15-35 weight
Part is measured, (c) linear dimension is that the chunk polysilicon of 50mm-100mm there are 65-100 parts by weight；
Step 3: raw material examining, operator are checked in raw material using the raw material in infrared inspection instrument one by one detecting step two
Whether portion has crack, impurity, stain, shade, crystallite, the result that each raw material scans on infra-red inspection instrument is recorded it is on the regular payroll, point
Storage is opened, is stayed with stand-by；
Step 4: the raw material in step 3 is successively placed on resistance type measuring instrument, uses resistance class by raw material resistivity examining
Type measuring instrument, according to the data of resistance type measuring instrument, counts p-type raw material or N-type to measuring at each raw edges 4mm
Raw material and record it is on the regular payroll, separately store, stay with stand-by, N-type raw material base phosphorus resistivity p be 30 Ω .cm-50 Ω .cm, p-type raw material
The base phosphorus resistivity Ω of p >=50 .cm；
Step 5: the raw material in step 4 is successively used chemical vapour deposition technique to examine body impurity content by the inspection of raw material impurity essence
Alms giver's data and body impurity content are by master data, according to the data of detection, count qualified raw material and record on the regular payroll, separate
Storage, stay with stand-by, equal < 7.74ppba of P, As and Sb in body impurity content alms giver, the B in body impurity content acceptor and
The equal < 2.7ppba of Al；
Step 6: the detection of material carbon oxygen concentration uses each raw material in list, polysilicon oxygen and carbon content tester successively measuring process five
Oxygen concentration and concentration of carbon, it is ensured that oxygen concentration≤1.0*1017/cm3, concentration of carbon≤5.0*1016/cm3, according to list, polysilicon oxygen
The data of carbon content tester, count the carbon oxygen concentration of each raw material and record it is on the regular payroll, separately store, stay with stand-by；
Step 7: the detection of raw material minority carrier life time uses the minority carrier of raw material in minority carrier life time detector successively detecting step six
Sub- service life, minority carrier lifetime >=10us count qualified raw material and record on the regular payroll, separately storage according to the data of detection
It deposits, stays with stand-by；
Step 8: the detection of raw material base metal impurity content successively detects step using silicon material parent metal impurity content tester
The base metal impurity content of raw material in rapid seven, base metal impurity include Fe, Cr, Ni, Cu, Zn, Na, TMI < 0.5ppmw,
The data of each raw material are successively recorded, separately stores, stays with stand-by；
Step 9: qualified silicon material is successively sorted out vanning, is laid with foam pad in cabinet by packaging and warehousing according to above-mentioned record data
Or carton carries out buffer protection, cabinet is wound fastening using PE film outside.
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| CN110687167A (en) * | 2019-10-17 | 2020-01-14 | 赛维Ldk太阳能高科技(新余)有限公司 | Detection method of silicon material |
| CN112642515A (en) * | 2020-11-05 | 2021-04-13 | 中国恩菲工程技术有限公司 | Polycrystalline silicon crushing, sorting and packaging system |
| CN115356343A (en) * | 2022-10-21 | 2022-11-18 | 北京科技大学 | Method and system for detecting quality of iron alloy for steelmaking |
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Application publication date: 20190510 |