GB/T 30901-2025High purity ammonium fluoride solution (English PDF)

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents". Drafting.

This document replaces GB/T 30901-2014 "High-purity ammonium fluoride solution". Compared with GB/T 30901-2014, the only changes are structural adjustments and rewriting.

Aside from the logical changes, the main technical changes are as follows.

a) Added EL, UP, and UP-SSS product grades and indicator requirements (see Chapter 5);

b) The ammonium fluoride content has been changed (see 6.2, 5.2 in the 2014 edition);

c) The content of UP-SS grade ammonium fluorosilicate has been changed (see 6.2, 5.2 in the 2014 edition);

d) Fourteen new indicators, including silver, gold, and bismuth, have been added (see 6.2);

e) The method for determining ammonium fluoride content has been changed to automated potentiometric titration (see 7.3, 6.3 in the 2014 edition);

f) The method for determining the ammonium fluorosilicate content has been changed to inductively coupled plasma mass spectrometry (see 7.4, 6.4 in the 2014 edition);

g) The test procedure in the method for determining the content of anions such as chloride has been modified (see 7.7.4, 6.7.4 in the 2014 version);

h) The test procedures in the determination methods for the content of 35 impurity elements, including silver and aluminum, have been modified (see 7.8.4, 6.8.4 in the 2014 version);

i) The security clause has been removed (see Chapter 10 of the 2014 edition).

Please note that some content in this document may involve patents. The issuing organization of this document assumes no responsibility for identifying patents.

This document was proposed by the China Petroleum and Chemical Industry Federation.

This document is under the jurisdiction of the National Technical Committee on Chemical Standardization (SAC/TC63).

This document was drafted by: Zhongjuxin Technology Co., Ltd., Duofuduo New Materials Co., Ltd., and Zhejiang Kaisheng Fluorochemical Co., Ltd.

Company, Zhongjuxin (Hubei) Technology Co., Ltd., Guizhou Wengfu Lantian Fluorochemical Co., Ltd., Hubei Xingli Electronic Materials Co., Ltd., Guizhou Shengwei Kaiyang Chemical Co., Ltd., Hubei Yihua Fluorochemical Co., Ltd., Fujian Jianyang Jinshi Fluorine Industry Co., Ltd., and Metrohm China Ltd.

The company, Mettler Toledo Technologies (China) Co., Ltd., Fujian Yongjing Technology Co., Ltd., Qingdao Shenghan Chromatography Technology Co., Ltd.

CNOOC Tianjin Chemical Research and Design Institute Co., Ltd.

The main drafters of this document are: Zhang Xueliang, Xue Xujin, Zhao Xiaoya, Fu Tiezhu, Zhang Nan, Peng Fei, Ma Lei, Yang Bo, Wu Zhenqiu, Liu Binhua, and Yuan Chunwei.

Liu Chunhua, Tian Haifeng, Guo Fengxin, Cheng Wenhai, Ye Wenhao, Yang Jiancheng, Jiang Liangshu, Chen Wei, Wang Xuemei, Li Haiyan, Ying Yunjin, Li You, Hao He, Liu Shipeng, Ji Ran, Zhao Meijing, Li Xia.

The release history of this document and the document it replaces is as follows.

— First published in 2014, this is the first revision.

1 Scope

This document specifies the classification, requirements, test methods, inspection rules, marking and accompanying documents, packaging, and transportation of high-purity ammonium fluoride solutions. Storage.

This document applies to high-purity ammonium fluoride solutions.

Note. This product is mainly used in industries such as cleaning and etching of solar photovoltaic cells, integrated circuits, and ultra-large-scale integrated circuit chips.

2 Normative references

GB/T 191-2008

GB/T 6678

GB/T 6680

GB/T 6682-2008

GB/T 8170

GB/T 23769-2009

GB/T 23770-2009

JJG814-2015

3 Terms and Definitions

This document does not contain any terms or definitions that need to be defined.

4 Molecular formula and relative molecular mass

Molecular formula. NH4F.

Relative molecular mass. 37.04 (based on the 2022 international relative atomic mass).

5 Categories

High-purity ammonium fluoride solution is classified into 5 grades according to its intended use.

a) EL grade. mainly used in the manufacture of solar photovoltaic cells and liquid crystal display devices;

b) UP grade. Primarily used for cleaning and etching integrated circuits with linewidths of 0.8µm~1.2µm;

c) UP-S grade. Primarily used for cleaning and etching of integrated circuits with linewidths of 0.2µm~0.8µm;

d) UP-SS grade. Primarily used for cleaning and etching integrated circuits with linewidths of 0.09µm~0.2µm;

e) UP-SSS grade. mainly used for cleaning and etching of integrated circuits with line width less than 0.09µm.

6 Requirements

6.1 Appearance. Colorless and transparent liquid.

6.2 The high-purity ammonium fluoride solution shall conform to the requirements of Table 1 when tested according to the test methods specified in this document. Table 1 project index EL level UP level UP-S level UP-SS level UP-SSS level Ammonium fluoride (NH4F) w/% 35.0±1.0 or 40.0±1.0 Ammonium fluorosilicate [(NH4)2SiF6]/(mg/kg) <= - - 10 5 1 Chroma/Black Level <= 10 10 10 10 5 pH (10 g/L solution, 25°C). 6.0~7.5 Chloride (as Cl)/(mg/kg) <= 5 5 0.2 0.05 0.01 Nitrate (as NO3)/(mg/kg) <= 3 3 0.1 0.05 0.01 Phosphate (as PO4)/(mg/kg) <= 1 1 0.1 0.05 0.01 Sulfate (as SO4)/(mg/kg) <= 5 5 0.2 0.05 0.01 Silver (Ag)/(µg/kg) <= -10 1 0.1 0.02 Aluminum (Al)/(µg/kg) <= 100 10 1 0.1 0.02 Arsenic (As)/(µg/kg) <= 300 10 1 0.1 0.02 Gold (Au)/(µg/kg) <= -10 1 0.1 0.02 Boron (B)/(µg/kg) <= 100 10 1 0.1 0.02 Barium (Ba)/(µg/kg) <= 100 10 1 0.1 0.02 Beryllium(Be)/(µg/kg) <= - - 1 0.1 0.02 Bismuth (Bi)/(µg/kg) <= - 10 1 0.1 0.02 Calcium (Ca)/(µg/kg) <= 100 10 1 0.1 0.02 Cadmium (Cd)/(µg/kg) <= 50 10 1 0.1 0.02 Cobalt (Co)/(µg/kg) <= - - 1 0.1 0.02 Chromium (Cr)/(µg/kg) <= 20 10 1 0.1 0.02 Copper (Cu)/(µg/kg) <= 20 10 1 0.1 0.02 Iron (Fe)/(µg/kg) <= 100 10 1 0.1 0.02 Gallium(Ga)/(µg/kg) <= - - 1 0.1 0.02 Germanium (Ge)/(µg/kg) <= - 10 1 0.1 0.02 Table 1 (continued) project index EL level UP level UP-S level UP-SS level UP-SSS level Potassium (K)/(µg/kg) <= 100 10 1 0.1 0.02 Lithium (Li)/(µg/kg) <= 20 10 1 0.1 0.02 Magnesium (Mg)/(µg/kg) <= 100 10 1 0.1 0.02 Manganese (Mn)/(µg/kg) <= 50 10 1 0.1 0.02 Molybdenum (Mo)/(µg/kg) <= - 10 1 0.1 0.02 Sodium (Na)/(µg/kg) <= 100 10 1 0.1 0.02 Niobium (Nb)/(µg/kg) <= - - 1 0.1 0.02 Nickel (Ni)/(µg/kg) <= 50 10 1 0.1 0.02 Lead (Pb)/(µg/kg) <= 50 10 1 0.1 0.02 Palladium (Pd)/(µg/kg) <= -10 1 0.1 0.02 Antimony (Sb)/(µg/kg) <= 50 10 1 0.1 0.02 Tin (Sn)/(µg/kg) <= 20 10 1 0.1 0.02 Strontium (Sr)/(µg/kg) <= -10 1 0.1 0.02 Tantalum (Ta)/(µg/kg) <= -10 1 0.1 0.02 Titanium (Ti)/(µg/kg) <= 100 10 1 0.1 0.02 Thallium(Tl)/(µg/kg) <= - 10 1 0.1 0.02 Vanadium (V)/(µg/kg) <= - - 1 0.1 0.02 Zinc (Zn)/(µg/kg) <= 50 10 1 0.1 0.02 Zirconium (Zr)/(µg/kg) <= - 10 1 0.1 0.02 Particles/(pieces/mL) (>=1.0µm) <= 50 - - - - (>=0.5µm) <= - 25 5 - - (>=0.2µm) <= - - - 10 10 (>=0.1µm) <= - - - - 50

7 Test Methods

Warning. Some reagents or materials used in this test method are corrosive. Operators should exercise caution and avoid skin contact.

If it comes into contact with skin, rinse immediately with water; in severe cases, seek immediate medical attention.