GB/T 25074-2017_English: PDF (GB/T25074-2017)
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Solar-grade polycrystalline silicon
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Solar-grade polycrystalline silicon
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| Standard ID | GB/T 25074-2017 (GB/T25074-2017) | | Description (Translated English) | Solar-grade polycrystalline silicon | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H82 | | Classification of International Standard | 29.045 | | Word Count Estimation | 7,798 | | Date of Issue | 2017-11-01 | | Date of Implementation | 2018-05-01 | | Older Standard (superseded by this standard) | GB/T 25074-2010 | | Drafting Organization | Luoyang Silicon High Technology Co., Ltd., polysilicon material preparation National Engineering Laboratory, Nonferrous Metals Technology and Economy Research Institute, Jiangsu Zhongneng Silicon Technology Development Co., Ltd., Xinte Energy Co., Ltd., Yichang CSG Silicon Materials Co., Ltd., Inner Mongolia Shenzhou Silicon Co., Ltd., Asia Silicon (Qinghai) Co., Ltd. | | Administrative Organization | National Standardization Technical Committee of Semiconductor Equipment and Materials (SAC/TC203), Sub-Committee on Sub-Technical Committee of National Semiconductor Equipment and Materials Standardization Technical Committee (SAC/TC 203/SC 2) | | Regulation (derived from) | National Standard Announcement 2017 No. 29 | | Proposing organization | National Standardization Technical Committee of Semiconductor Equipment and Materials (SAC/TC203), Sub-Committee on Sub-Technical Committee of National Semiconductor Equipment and Materials Standardization Technical Committee (SAC/TC 203/SC 2) | | Issuing agency(ies) | People's Republic of China General Administration of Quality Supervision, Inspection and Quarantine, China National Standardization Administration | | Standard ID | GB/T 25074-2010 (GB/T25074-2010) | | Description (Translated English) | Solar-grade polycrystalline silicon | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H82 | | Classification of International Standard | 29.045 | | Word Count Estimation | 6,664 | | Date of Issue | 2010-09-02 | | Date of Implementation | 2011-04-01 | | Quoted Standard | GB/T 1550; GB/T 1551; GB/T 1553; GB/T 1557; GB/T 1558; GB/T 4059; GB/T 4060; GB/T 4061; GB/T 24574; GB/T 24581; SEMI MF1535 | | Drafting Organization | Luoyang Silicon Technologies Ltd. | | Administrative Organization | National Standardization Technical Committee of semiconductor equipment and materials | | Regulation (derived from) | National Standard Approval Announcement 2010 No.4 (Total No.159) | | Proposing organization | National Standardization Technical Committee materials and equipment semiconductor (SAC/TC 203) | | Issuing agency(ies) | Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China; Standardization Administration of China | | Summary | This standard specifies the classification of solar grade polysilicon products, technical requirements, test methods, inspection rules and packaging, signs, transport, storage and purchase order (or contract) content. This standard applies to the use of chlorine as a raw material silane (modified) and silane method Siemens rod polysilicon production process, massive polysilicon, granular polysilicon. Products are mainly used in solar grade polycrystalline silicon rods and directionally solidified ingot production. |
GB/T 25074-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 29.045
H 82
Replacing GB/T 25074-2010
Solar-grade polycrystalline silicon
太阳能级多晶硅
ISSUED ON: NOVEMBER 1, 2017
IMPLEMENTED ON: MAY 1, 2018
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions ... 6
4 Grade and classification ... 6
5 Requirements ... 7
6 Test method ... 8
7 Inspection rules ... 9
8 Marking, packaging, transportation, storage, and quality certificate ... 10
9 Contents of order form (or contract) ... 11
Appendix A (Informative) Reference technical indexes of solar-grade polycrystalline
silicon ... 13
Solar-grade polycrystalline silicon
1 Scope
This standard specifies the terms and definitions, grades and classifications,
requirements, test methods, inspection rules, marking, packaging, transportation,
storage, and quality certificates of solar-grade polycrystalline silicon.
This standard applies to rod-shaped polycrystalline silicon grown from chlorosilane and
silane or polycrystalline silicon blocks formed by crushing.
2 Normative references
The following documents are essential to the application of this document. For the dated
referenced documents, only the versions with the indicated dates are applicable to this
document; for the undated referenced documents, only the latest version (including all
the amendments) is applicable to this document.
GB/T 1550 Test methods for conductivity type of extrinsic semiconducting
materials
GB/T 1551 Test method for measuring resistivity of monocrystal silicon - In-line
four-point probe and direct current two-point probe method
GB/T 1553 Test methods for minority carrier lifetime in bulk silicon and
germanium - Photoconductivity decay method
GB/T 1557 Test method for determining interstitial oxygen content in silicon by
infrared absorption
GB/T 1558 Test method for substitutional atomic carbon content of silicon by
infrared absorption
GB/T 4059 Test method for phosphorus content in polycrystalline silicon by zone-
melting method under controlled atmosphere
GB/T 4060 Test method for boron content in polycrystalline silicon by vacuum
zone-melting method
GB/T 13389 Practice for conversion between resistivity and dopant density for
boron-doped, phosphorus-doped, and arsenic-doped silicon
GB/T 14264 Semiconductor materials - Terms and definitions
GB/T 14844 Designations of semiconductor materials
GB/T 24574 Test methods for photoluminescence analysis of single crystal silicon
for III-V impurities
GB/T 24581 Test method for Ⅲ and Ⅴ impurities content in single crystal silicon -
Low temperature FT-IR analysis method
GB/T 24582 Test method for measuring surface metal impurity content of
polycrystalline silicon - Acid extraction-inductively coupled plasma mass
spectrometry method
GB/T 29057 Practice for evaluation of polycrystalline silicon rods by float-zone
crystal growth and spectroscopy
GB/T 29849 Test method for measuring surface metallic contamination of silicon
materials used for photovoltaic applications by inductively coupled plasma mass
spectrometry
GB/T 31854 Test method for measuring metallic impurities content in silicon
materials used for photovoltaic applications by inductively coupled plasma mass
spectrometry
3 Terms and definitions
The terms and definitions defined in GB/T 14264 apply to this document.
4 Grade and classification
4.1 Grade
The grades of solar-grade polycrystalline silicon products shall meet the requirements
of GB/T 14844.
4.2 Classification
Solar-grade polycrystalline silicon is divided into block and rod according to the shape,
divided into N-type and P-type according to the conductivity type, and divided into four
grades according to the difference in technical indexes.
5.3 Surface quality
5.3.1 No-need-to-cleaning or after-cleaning polycrystalline silicon shall meet the
requirements for direct use. The classification requirements for the surface quality of
polycrystalline silicon are generally as follows:
a) Dense polysilicon: The depth of surface particle dimples is less than 5 mm, the
cross-sectional structure is dense, the appearance has no abnormal color, and
there is no oxidized interlayer;
b) Popcorn polysilicon: The depth of surface particle dimples is 5 mm~20 mm,
the appearance has no abnormal color, and there is no oxidized interlayer;
c) Coral polysilicon: The cross-sectional structure is loose, the depth of surface
particle dimple is ≥20 mm, the appearance has no abnormal color, and there is
no oxidized interlayer.
5.3.2 Other classification requirements for the surface quality of polycrystalline silicon
shall be agreed upon between the supplier and the purchaser.
6 Test method
6.1 Before the test of donor impurity concentration, acceptor impurity concentration,
oxygen concentration, carbon concentration, minority carrier lifetime, conductivity
type, and resistivity of polycrystalline silicon, single crystal samples are required to be
prepared according to the methods specified in GB/T 4059, GB/T 4060 or GB/T 29057.
6.2 The determination of donor impurity concentration and acceptor impurity
concentration in polycrystalline silicon shall be carried out according to the provisions
of GB/T 24574 or GB/T 24581, or converted according to the methods specified in
GB/T 1551 and GB/T 13389. Arbitration inspection shall be carried out in accordance
with the provisions of GB/T 24581.
6.3 The determination of oxygen concentration in polycrystalline silicon shall be carried
out according to the provisions of GB/T 1557.
6.4 The determination of carbon concentration in polycrystalline silicon shall be carried
out according to the provisions of GB/T 1558.
6.5 The determination of minority carrier lifetime in polycrystalline silicon shall be
carried out according to the provisions of GB/T 1553.
6.6 The determination of the metal impurity content of the polycrystalline silicon matrix
shall be carried out in accordance with the provisions of GB/T 31854.
6.7 The determination of the metal impurity content on the surface of polycrystalline
silicon shall be carried out according to the provisions of GB/T 24582 or GB/T 29849.
Arbitration inspection shall be carried out according to the provisions of GB/T 29849.
6.8 The inspection of the conductivity type of polycrystalline silicon shall be carried
out according to the provisions of GB/T 1550.
6.9 The determination of the resistivity of polycrystalline silicon shall be carried out
according to the provisions of GB/T 1551.
6.10 The dimension distribution range of polycrystalline silicon blocks shall be
inspected by sieving, or by a method agreed upon by the supplier and the purchaser.
The dimensions of the rod-shaped polycrystalline silicon are measured with a
measuring tool of corresponding precision.
6.11 The surface quality of polycrystalline silicon is inspected visually.
7 Inspection rules
7.1 Inspection and acceptance
7.1.1 The product shall be inspected by the quality supervision department of the
supplier to ensure that the product quality complies with the provisions of this standard;
the product quality certificate shall be filled in.
7.1.2 The buyer can inspect the received products. If the test results are inconsistent
with the provisions of this standard, it shall be reported to the supplier within 3 months
from the date of receipt of the product, and the supplier and the buyer shall negotiate to
resolve it.
7.2 Batch formation
Products shall be submitted for acceptance in batches, and each batch shall be composed
of polycrystalline silicon of the same grade, which is produced under similar process
conditions and traceable to the production conditions.
7.3 Inspection items
7.3.1 Each batch of products shall be inspected for donor impurity concentration,
acceptor impurity concentration, oxygen concentration, carbon concentration, minority
carrier lifetime, dimensions, and surface quality.
7.3.2 The matrix metal impurity content and the surface metal impurity content are the
items of type inspection, and the inspection frequency is determined through
negotiation between the supplier and the buyer.
c) the product quantity and net weight.
8.2 Packaging
The polycrystalline silicon shall be put into a clean high-purity resin packaging bag and
sealed, and the dense polysilicon shall be packed into a double-layer clean packaging
bag; then, the packaging bag is put into a packing box or drum. The packaging for
polycrystalline silicon blocks is based on customer requirements; the rod-shaped
polycrystalline silicon is fixed in a box and sealed with double-layer clean high-purity
resin packaging bags. When packaging, the packaging bag shall be prevented from
being damaged to avoid external contamination of the product and provide good
protection.
8.3 Transportation
During transportation, the product shall be loaded and unloaded lightly, not pressed or
squeezed, and anti-shock measures shall be taken.
8.4 Storage
The product shall be stored in a clean and dry environment.
8.5 Quality certificate
Each batch of products shall be accompanied by a quality certificate stating:
a) the supplier’s name;
b) the product name and grade;
c) the product batch number;
d) the gross weight and net weight of the product;
e) inspection results of all items and inspection department stamps;
f) the number of this standard;
g) the date of manufacture.
9 Contents of an order form (or contract)
The order form for the products listed in this standard shall include the following
contents:
a) the product name;
......
GB/T 25074-2010
Solar-grade polycrystalline silicon
ICS 29.045
H82
National Standards of People's Republic of China
Solar grade polysilicon
Solar-grade polycrystalinesilicon
2010-09-02 released
2011-04-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
China National Standardization Administration released
Foreword
This standard is proposed and managed by the National Semiconductor Equipment and Materials Standardization Technical Committee (SAC/TC203).
This standard was drafted. Luoyang Silicon High Technology Co., Ltd., Suntech Power Co., Ltd., China Electronics Standardization
Institute, China Nonferrous Metals Industry Standards Institute of Metrology and Quality, China Electronic Materials Industry Association, Xi'an Longsi Silicon Materials Co., Ltd.
Secretary, Sichuan Xinguang Silicon Technology Co., Ltd.
The main drafters of this standard. Yang Yuan, Yuan Jinman, Sun Shilong, Liu Yun, He Dongjiang, Wang Yichuan, Lu Jin, Cao Yu, Liang Hong.
Solar grade polysilicon
1 Scope
This standard specifies the solar grade polysilicon product classification, technical requirements, test methods, inspection rules and packaging, marking, transportation, storage
And purchase order (or contract) content.
This standard applies to chlorosilane as raw material (modified) Siemens method and silane process and other production of rod-shaped polycrystalline silicon, massive polycrystalline
Silicon, granular polysilicon products. Products are mainly used for the production of solar grade monocrystalline silicon rods and directional solidification polycrystalline silicon ingot.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. All dated references, which are subsequently owned
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to reach an agreement based on this standard research
Whether you can use the latest versions of these files. For undated references, the latest version applies to this standard.
GB/T 1550 extrinsic semiconductor conductive material type test methods
GB/T 1551 silicon single crystal resistivity measurement method
Determination of minority carrier lifetime in silicon and germanium photoconductive attenuation method
Determination of oxygen content in interstitial of GB/T 1557 silicon by infrared absorption method
GB/T 1558 silicon substituted carbon atoms in infrared absorption measurement method
GB/T 4059 silicon polycrystalline atmosphere phosphorus test method
GB/T 4060 silicon polycrystalline vacuum zone test method of molten boron
GB/T 4061 silicon polycrystalline cross-section chemical corrosion test methods
Photoluminescence measurement of group Ⅲ-Ⅴ impurities in GB/T 24574 silicon single crystals
GB/T 24581 Low-temperature Fourier transform infrared spectroscopy measurement of single crystal silicon Ⅲ, Ⅴ impurity content of the test method
SEMIMF1535 Non-contact Measurement of Complex Carrier Lifetime of Silicon Wafers with Microwave Reflectance Photoconductive Attenuation Method
3 requirements
3.1 classification
According to the appearance of the product is divided into bar, block and granular, according to the level of difference is divided into three levels.
3.2 grade
Polycrystalline grade is expressed as.
SGPSi -
That solar grade polysilicon
□ -
Rods are denoted by the letter I, N is massive, and G is granular
Use Arabic numerals for polysilicon grades
4 technical requirements
4.1 level
Solar grade polysilicon grade and related technical requirements shall comply with the provisions of Table 1. Each grade of product should meet this grade at the same time
If the index exceeds the standard, it will drop to the next level.
Table 1
Project (a)
Solar grade polysilicon level indicators (a)
1 grade 2 grade 3 grade
Phosphorus resistivity/Ω · cm ≥100 ≥40 ≥20
Base boron resistivity/Ω · cm ≥500 ≥200 ≥100
Minority carrier lifetime/μs ≥100 ≥50 ≥30
Oxygen concentration/(atoms/cm3)? 1.01017? 1.01017? 1.51017
Carbon concentration/(atoms/cm3) ≦ 2.5 × 1016 ≦ 4.0 × 1016 ≦ 4.5 × 1016
Project (2)
Solar grade polysilicon grade index (two)
1 grade 2 grade 3 grade
Donor impurity concentration/10-9 ≤1.5 ≤3.76 ≤7.74
Acceptor impurity concentration/10-9 ≤0.5 ≤1.3 ≤2.7
Minority carrier lifetime/μs ≥100 ≥50 ≥30
Oxygen concentration/(atoms/cm3)? 1.01017? 1.01017? 1.51017
Carbon concentration/(atoms/cm3) ≦ 2.5 × 1016 ≦ 4.0 × 1016 ≦ 4.5 × 1016
Matrix metal impurities/10-6
Fe, Cr, Ni, Cu, Zn, TMI
(Totalmetalimpurities)
Total metal impurity content. ≤ 0.05
Fe, Cr, Ni, Cu, Zn, TMI
(Totalmetalimpurities)
Total metal impurity content. ≤ 0.1
Fe, Cr, Ni, Cu, Zn, TMI
(Totalmetalimpurities)
Total metal impurity content. ≤ 0.2
Note 1. The detection of matrix metal impurities can be used secondary ion mass spectrometry, plasma mass spectrometry and neutron activation analysis, by the supply and demand sides to negotiate settlement.
Note 2. The base metal impurities as a reference project, by the supply and demand sides to negotiate settlement.
4.2 size range
4.2.1 Broken block polycrystalline silicon has a random shape and random size distribution, the linear size of a minimum of 3mm, the maximum
200mm. Bulk polysilicon size distribution range.
a) 3mm ~ 25mm up to 15% by weight;
b) 15% ~ 35% of the weight of 25mm ~ 100mm;
c) Minimum weight 65% of 100mm ~.200mm.
4.2.2 granular silicon particle size range of 1mm ~ 3mm.
4.2.3 Rod polycrystalline diameter, length dimensions agreed upon by both supply and demand.
4.3 surface quality
4.3.1 block, rod polysilicon cross-section structure should be dense.
4.3.2 polysilicon disposable or after surface cleaning, should be made to achieve direct use requirements. All polysilicon appearance should be no stains, discoloration,
No visible visible contaminants and oxidized outer surface.
4.3.3 polycrystalline oxide oxide interlayer is not allowed.
5 test method
5.1 polysilicon conductivity type test according to GB/T 1550 test.
5.2 polysilicon resistivity measurement according to GB/T 1551 test.
5.3 minority carrier lifetime measurement according to GB/T 1553 or SEMIMF1535 test.
5.4 polysilicon oxygen concentration measured according to GB/T 1557 test.
5.5 Polycrystalline carbon concentration measured according to GB/T 1558 test.
5.6 Polysilicon cross-section test Press GB/T 4061 test.
5.7 Polysilicon III-V impurity content in accordance with GB/T 24574 or GB/T 24581 test.
5.8 The size of rod-shaped polysilicon measured with a vernier caliper, block polycrystalline silicon, granular polysilicon size distribution using screening test, or by
To be mutually agreed method test.
5.9 Polysilicon surface quality with visual inspection.
6 inspection rules
6.1 inspection and acceptance
6.1.1 The product shall be inspected by the supplier's quality supervision department to ensure that the product quality meets the requirements of this standard and the product quality certificate is filled in.
6.1.2 The purchaser may inspect the product received. If the test result is inconsistent with the provisions of this standard, it should be three months from the date of receipt of the product
Inward suppliers proposed by the supply and demand sides negotiated settlement.
6.2 group approved
Products should be submitted in batches of acceptance, each batch should be the same brand, with similar process conditions and production conditions can be traced back to the production of polysilicon composition.
6.3 inspection items
Each batch of product should be based on phosphorus resistivity or donor impurity concentration, boron resistance or acceptor impurity concentration, minority carrier lifetime, oxygen concentration
Degree, carbon concentration, structure, surface quality and size of the test; substrate metal impurities by both supply and demand.
6.4 Sampling for the supplier, the sample preparation should be GB/T 4059, GB/T 4060, GB/T 4061 or by both supply and demand.
6.5 test results to determine
6.5.1 The grade of polysilicon is determined by the radical resistivity or donor impurity concentration, the boron-based resistivity or acceptor impurity concentration, minority carrier lifetime, oxygen
Concentration, carbon concentration determination; base metal impurities is a reference project, negotiated by both supply and demand.
6.5.2 In the judgment of the project if there is a test results failed, then double sampling of the substandard projects reinspection. Retest results
Still unqualified products, should be directly judged as unqualified.
7 packaging, marking, transportation and storage
7.1 Packaging
Polysilicon should be packed in clean polyethylene bags, sealed; disposable material into double polyethylene bags, and then the bags
Into the box or drum. Bulk polysilicon packaging specifications for each bag net weight of 5000g or 10000g. Rod-shaped polycrystalline silicon each individually
Packaging, and fixed with the box, package. Polyethylene bags should be protected from damage during packaging to avoid external contamination of the product and to be provided in the best way possible
Good protection.
7.2 mark
Outside the box (barrel) should be marked with "care and ease" and "anti-corrosion, moisture-proof" words or signs, and marked.
a) the name of the supplier;
b) product name;
c) product brand;
d) the number of products;
e) Product net weight.
7.3 Transportation
Products should be light in the transport process light unloading, do not pressure do not squeeze, and take shock measures.
7.4 Storage
Products should be stored in a clean, dry environment.
7.5 Quality Certificate
Each batch of product should be accompanied by a certificate of quality, stating.
a) the name of the supplier;
b) product name, brand;
c) product lot number;
d) product gross weight, net weight;
e) the test results and inspection department mark;
f) the standard number;
g) Date of manufacture.
8 Order Contents
The products listed in this standard order form should include the following.
a) product name
b) status;
c) Specifications;
d) weight;
e) This standard number;
f) others.
T/B
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