National standard for solar grade polysilicon

1 Scope

This standard specifies the product classification, technical requirements, test methods, inspection rules, and packaging, marking, transportation and storage of solar grade polysilicon.

This standard applies to rod-shaped polysilicon, granular polysilicon produced by using trichlorosilane or silicon tetrachloride as raw materials, including bulk polysilicon, carbon head materials, and silicon powder in the production process, as well as purification by physical purification. Polysilicon. The products are mainly used for the production of solar grade monocrystalline silicon rods and polycrystalline silicon ingots.

2 Normative references

The clauses in the following documents have been adopted as references to this standard. For dated references, all subsequent 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 to study whether the latest version of these documents can be used . For undated references, the latest version is applicable to this standard.

GB/T 1550 extrinsic semiconductor material conductivity type test method

GB/T 1552 Silicon, germanium single crystal resistivity test In-line four-probe method

Determination of minority carrier lifetime in GB/T 1553 silicon and germanium by photoconductivity attenuation method

GB/T 4059 Silicon Polyatomic Zone Phosphorus Test Method

GB/T 4060 silicon polycrystalline vacuum zone melting boron test method

GB/T 1558 Infrared absorption measurement method for gap oxygen content in silicon crystals

GB/T 1558 Determination of Substituted Carbon in Silicon Crystals by Infrared Absorption Method

Chemical Analysis of Substrate Metal Impurities in GB/T ××××-200× Silicon Polycrystalline Inductively Coupled Plasma Mass Spectrometry

GB/T 14264 Semiconductor Material Terms

ASTM F1389-00 Photoluminescence Spectra for Group III-V Impurities in Monocrystalline Silicon

ASTM F1724-01 Measurement of Metal Impurities on Polysilicon Surfaces by Atomic Absorption Spectroscopy

3 requirements

3.1 Classification

The products are classified into block, granular, powder, and rod-shaped polysilicon according to the appearance, and are classified into three levels according to the difference in purity.

3.2 Brand

Silicon polycrystalline grades are indicated as: SOGPSi—1□—2□

SOGPSi said solar grade silicon polycrystalline

1 â–¡ I letter for stick, N for block, G for granular, P for powder

2 â–¡ Arabic numerals represent silicon polycrystals, etc.

3.3 Technical Requirements

3.3.1 Rod, block silicon

The purity of solar grade rod-like and block polysilicon and related technical requirements should meet the requirements of Table 1.

Table 1

3.3.2 Powdered Polysilicon

The purity of powdery polysilicon and related technical requirements should meet the requirements of Table 2.

Table 2

3.3.3 carbon head material

The carbon in the carbon head material is removed and used as a solar ingot and pull rod. The technical requirements are the same as those in Table 1 for solar class grade and rod polysilicon purity requirements.

3.3.4 Powdered Material

Powdered materials can be solar-ingot-cast, and their technical requirements should meet the requirements of Class 2 in Table 2.

3.4 Size range

3.4.1 Broken bulk silicon polycrystals have an irregular shape and a random size distribution with a minimum linear dimension of 6 mm and a maximum of 100 mm.

3.4.2 The size distribution of bulk polysilicon is:

a) 15% of the maximum weight of 6-25mm;

b) 15% to 35% of the weight of 25 to 50mm;

c) The minimum weight of 65% is 50 to 100mm.

3.4.3 The diameter and length dimensions of rod-shaped polysilicon are agreed upon by both parties. Its diameter allowable deviation is 10%.

3.5 Structure and Surface Quality

3.5.1 Blocky, rod-shaped silicon polycrystalline structures should be dense.

3.5.2 Polycrystalline silicon shall be free to wash or be surface-cleaned and shall be used to achieve direct use. The appearance of all polysilicon should be colorless, discolored, free of visible contaminants and oxidized external surfaces.

3.5.3 The diameter of granular silicon is 1-3mm, and no foreign matter is visible to the naked eye.

3.5.4 The carbon of the carbon head material should be removed and there should be no residue.

3.5.5 Powdered polysilicon requires no visible foreign matter.

4 test methods

4.1 Purity and related technical requirements Inspection methods:

4.1.1 Polysilicon conductivity type test According to GB/T 1550 test.

4.1.2 polysilicon N-type resistivity test according to GB/T 1550 test.

4.1.3 polysilicon P type resistivity test according to GB/T 1550 test.

4.1.4 N-type minority carrier lifetime measurement according to GB/T 1550 test.

4.1.5 The concentration of oxygen in polysilicon is measured according to GB/T 1558.

4.1.6 Polysilicon carbon concentration measurement According to GB/T 1558 test.

4.1.7 polysilicon profile sandwich test according to GB/T 4061 test.

4.1.8 Polysilicon in the matrix metal impurities in accordance with GB/T×××-200× test.

4.1.9 The content of B and P in polysilicon is tested according to ASTM F1389-00.

4.1.10 Polysilicon surface metal impurities are tested according to ASTM F1724-01.

4.2 Size Inspection Method:

The size of the rod-like silicon polycrystal is measured with a vernier caliper, and the size distribution of the bulk silicon polycrystal is examined by sieving, or by a method mutually agreed upon by the supplier and the buyer (for example, a monolithic weight method). The size distribution of the granular polysilicon can be examined by sieving.

4.3 The powdered polysilicon and carbon head material are agreed upon by both parties.

4.4 The surface quality of polysilicon is checked visually.

5 Inspection Rules

5.1 Inspection and Acceptance

5.1.1 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 fill in the product quality certificate.

5.1.2 The acquirer may inspect the received product. If the inspection result is inconsistent with the provisions of this standard, it shall be submitted to the supplier within one month from the date of receipt of the product, and shall be resolved through consultation between the supplier and the buyer.

5.2 Batches

The products shall be submitted for acceptance in batches, each batch shall have the same grade, have the same nominal purity and characteristics, and be made of silicon polycrystals or silicon polycrystals of the same reaction times produced under similar process conditions and traceable to the production conditions.

5.3 Inspection items

Each batch of products should be tested for N-type resistivity, P-type resistivity, minority carrier lifetime, oxygen-carbon concentration, structure, surface quality, and size. Matrix metal impurities are sampled or negotiated by both parties.

5.4 Sampling and sample preparation

5.4.1 For sampling and preparation by the supplier, the n-type resistivity, P-type resistivity, and sample preparation of the rod-shaped silicon polycrystalline body shall be conducted in accordance with GB4059, GB4060, and GB4061. The bulk silicon polycrystalline silicon shall be cast on representative sites. Reference GB4059, GB4060 sampling, sample preparation.

5.4.2 The arbitration sampling plan shall be agreed by both the supplier and the buyer, and the sampling site and sample preparation shall be conducted according to 6.4.1.

5.5 Determination of test results

5.5.1 The purity of polysilicon is determined by N-type resistivity, P-type resistivity, and oxygen-carbon concentration. The minority carrier lifetime and matrix metal impurities are reference items.

5.5.2 If there is a failure in the test result in the determination item, double sampling shall be repeated for the unqualified item. If repeated tests still fail, the batch of products is rejected or degraded.

6 Packaging, Marking, Transport and Storage

6.1 Packaging

The polycrystalline silicon is disposable or washed in a certain manner, dried, packed in a clean polyethylene bag, sealed, and then placed in a packaging box or a packaging drum. The bulk silicon polycrystalline package has a net weight of 5000g ± 25g or 10000g ± 50g per bag. The rod-shaped silicon polycrystals are individually packaged and fixed in boxes and sealed. During the packaging, the polyethylene bags should be prevented from being damaged so as to avoid external contamination of the products and provide good protection according to the best method.

6.2 Signs

Outside the packing box (barrel) should be marked with "careful light" and "anti-corrosion, moisture-proof" words or signs, and indicate:

a) The name of the acquirer;

b) product name, brand number;

c) product quantity, net weight;

d) supplier name

6.3 Quality Certificate

Each batch of products should be accompanied by a quality certificate stating:

a) supplier name;

b) product name and brand number;

c) product lot number;

d) Product gross weight, net weight;

e) The results of various inspections and the imprint of the inspection department;

f) the standard number;

g) The date of manufacture.

6.4 Transportation

The product should be lightly loaded and unloaded during transport, do not press or squeeze, and take anti-shock measures.

6.5 Storage

The product should be stored in a clean, dry environment.

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