GB/T 4059-2018Test method for phosphorus content in polycrystalline silicon by zone-melting method under controlled atmosphere (English PDF)

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009.

This standard replaces GB/T 4059-2007 "Test method for molten phosphorus in silicon polycrystalline atmosphere zone", compared with GB/T 4059-2007, except for editing In addition to the series of changes, the main technical changes are as follows.

--- The determination range of the base phosphorus content was changed from "0.002 x 10^-9~100 x 10^-9" to "0.01 x 10^13cm-3~500 x 10^13cm-3" (See Chapter 1, Chapter 1 of the 2007 edition);

---Adjusted the normative reference file, deleted GB/T 1553, GB/T 1554, GB/T 1555, GB/T 13389, added GB/T 1550, GB/T 4060, GB/T 4842, GB/T 8979, GB/T 11446.1-2013, GB/T 24574, GB/T 24581, GB/T 25915.1-2010 (see Chapter 2, Chapter 2 of the 2007 edition);

--- Modified the definition of the core, deleted the "hollow drill bit" (see 3.3, 2007 version 3.3);

--- Revised the method principle of Method A and Method B (see 4.1, 4.2, 2007, 4.1, 4.2);

--- The environment of pickling and zone melting in the interference factor was modified to "not less than the 6-level clean ring specified in GB/T 25915.1-2010 Circumstance [see 5.3, Chapter 5 of the 2007 edition)];

--- Interference factors have increased the sample processing process, zone melting speed, silicon core and other three factors that have an impact on the test results (see 5.4, 5.6, 5.7);

--- Removed the requirements of the interference factor in the silicon single crystal rod after the melting, test environment requirements [see.2007 edition of Chapter 5 f), Chapter 5 g)];

--- Modified the requirements for deionized water and argon in reagents and materials (see 6.3, 6.4, 2007 edition 6.3, 6.5);

---Reagents and materials increase the requirements of nitrogen (see 6.5);

--- Revised the requirements of seed crystals in reagents and materials, modified from "n-type resistivity of not less than 500 ohm · cm" to "seed crystal should be Dislocation-free N-type < 111> high-resistance silicon single crystal, and the donor impurity content (atoms) is less than 2.5 x 10^12 cm -3, carbon content (atoms The number is less than 5×10 15 cm-3, and the crystal orientation deviation is less than 5°" (see 6.6, 6.1 of 2007 edition);

--- Added requirements for "coring equipment" in equipment [see 7.1, 2007, Chapter 7 a)];

--- "Vacuum internal heat zone furnace" was changed to "internal heat zone furnace" [see 7.5, 2007 edition of Chapter 7 d)];

--- Add ultrasonic cleaning equipment, nitrogen and argon purification device, conductivity type tester, two-probe resistivity test Instrument, low temperature infrared spectrometer or photoluminescence spectrometer (see 7.3, 7.6, 7.7, 7.8, 7.9);

--- Deleted laboratory materials such as qualitative filter paper, vacuum cleaner, and gloves for clean room [see Chapter 7 of the 2007 edition) e), Chapter 7 f), Chapter 7 g)];

--- Revised sampling requirements (see 8.2, 8.4, 2007 editions 8.2, 8.4);

--- Removed "Select resistivity greater than 500 ohm · cm, carbon content less than 0.2 x 10^-6, no dislocations, crystal orientation deviation less than 5 ° N-type < 111> high-resistance silicon single crystal cut seed crystal prepared" (see.2007 edition of 10.1.1);

--- Modify "seed crystal must be used within 36h after drying" to "seed crystal should be sealed for clean protection" (see 10.1, 2007) Version 10.1.2);

--- Added "cleaning sample core should be dried with high purity nitrogen" (see 10.2.2);

--- Removed the "clean core drill" "clean the pickling table with deionized water not less than 10Mohm · cm" (see version 10.3.1 of the 2007 edition, 10.3.2);

--- "In the clean, vacuum pumping, preheating the core" modified to "pre-heat the core after cleaning, charging, vacuum pumping, argon filling" (see 10.3, version 10.3.3 of the 2007 edition;

--- Revised the content of the ingot growth in the test procedure (see 10.4, 10.4 of the 2007 edition);

--- Added "Test for conductivity type according to GB/T 1550" [see 10.5.2a)];

--- Revised the evaluation content of the ingot in the test procedure [see 10.5.2b), 2007 edition of 10.5.2.4];

--- Removed the crystal orientation, crystal integrity of the ingot, minority carrier lifetime test (see.2007 edition of 10.5.2.1, 10.5.2.2, 10.5.2.3);

--- Removed the allowable difference and increased precision (see Chapter 12, Chapter 12 of the 2007 edition).

This standard is supported by the National Semiconductor Equipment and Materials Standardization Technical Committee (SAC/TC203) and National Semiconductor Equipment and Materials Standards. The Technical Subcommittee Materials Branch (SAC/TC203/SC2) jointly proposed and managed.

1 Scope

This standard specifies the test method for the phosphorus content of polysilicon.

This standard is applicable to the determination of the phosphorus content (atoms) in polycrystalline silicon rods deposited on silicon cores. The measurement range is 0.01 x 10^13cm-3~ 500 x 10^13 cm -3.

2 Normative references

The following documents are indispensable for the application of this document. For dated references, only the dated version applies to this document. For undated references, the latest edition (including all amendments) applies to this document.

GB/T 1550 Test method for conductivity type of extrinsic semiconductor materials

GB/T 1551 silicon single crystal resistivity determination method

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

GB/T 4842 argon

GB/T 8979 pure nitrogen, high purity nitrogen and ultra pure nitrogen

GB/T 11446.1-2013 electronic grade water

GB/T 14264 semiconductor material terminology

Photoluminescence test method for III-V impurity in GB/T 24574 silicon single crystal

GB/T 24581 Low-temperature Fourier transform infrared spectroscopy method for the determination of III and V impurity content in silicon single crystals

GB/T 25915.1-2010 Clean rooms and related controlled environments - Part 1: Air cleanliness

3 Terms and definitions

The following terms and definitions as defined in GB/T 14264 apply to this document.