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AMMON IUM FLUORIDE 40% SEMI C20-1101 © SEMI 1978, 2001 1 SEMI C20-1101 SPECIFICA TION A ND GUIDELINES FOR A MMONIUM FLUORIDE 40% This specific ation and these guid elines were techn ically ap proved by th e Global P roce…

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SEMI C19-0301 © SEMI 1978, 2001 ACETONE4
Previous SEMI Reference # C1.2-96
Grade 1
(Specification)
Zinc (Zn) 0.1 ppm max
Particles in bottles:
size, #/mL
≥1.0 µm, 10 max
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AMMONIUM FLUORIDE 40% SEMI C20-1101 © SEMI 1978, 20011
SEMI C20-1101
SPECIFICATION AND GUIDELINES FOR AMMONIUM FLUORIDE 40%
This specification and these guidelines were technically approved by the Global Process Chemicals
Committee and are the direct responsibility of the North American Process Chemicals Committee. Current
edition approved by the North American Regional Standards Committee on August 27, 2001. Initially
available at www.semi.org September 2001; to be published November 2001. This document replaces SEMI
C1.3, C7.18, and C11.2 in their entirety. Originally published in 1978, 1995, and 1994 respectively.
Previously published March 2001.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for ammonium fluoride 40% used in the
semiconductor industry and testing procedures to
support those standards. Test methods have been shown
to give statistically valid results. This document also
provides guidelines for grades of ammonium fluoride
40% for which a need has been identified. In the case of
the guidelines, the test methods may not have been
statistically validated yet.
2 Scope
2.1 The scope of this document is all grades of
ammonium fluoride 40% used in the semiconductor
industry.
2.2 The VLSI grade purity level is typically required
by semiconductor devices with geometries of 0.8–1.2
microns.
2.3 This standard does not purport to address safety
issues, if any, associated with its use. It is the
responsibility of the users of this standard to establish
appropriate safety and health practices and determine
the applicability of regulatory limitations prior to use.
3 Limitations
3.1 None.
4 Referenced Standards
SEMI C1 — Specifications for Reagents
NOTE 1: Unless otherwise indicated, all documents cited
shall be the latest published versions.
5 Terminology
5.1 None.
6 Physical Property (for information only)
Density at 25°C1.11 g/mL
7 Requirements
7.1 The requirements for ammonium fluoride 40% for
Grade 1, VLSI Grade, and Tiers A and B are listed in
Table 1.
8 Grade 1 Procedures
8.1 Assay — Accurately weigh 3 g of sample in a
polyethylene weighing bottle. Transfer with water to a
polyethylene beaker and dilute to 100 mL. Add 40 mL
of neutralized formaldehyde solution and stir
magnetically for 15 minutes or allow to stand for 1/2
hour. Titrate with standardized 1 N sodium hydroxide
to a slight pink color.
%Assay
=
mL
×
N
of NaOH
×
3.704
Weight of sample g
()
NOTE 2: Neutralized formaldehyde solution: Dilute 20 mL of
37% formaldehyde solution with 20 mL of water, add 0.1 mL
of phenolphthalein indicator solution, and titrate with 0.1 N
sodium hydroxide to a slight pink color.
8.2 Color — Dilute 2.0 mL of platinum-cobalt stock
solution (APHA No. 500) to 100 mL with water.
Compare this standard (APHA No. 10) with 100 mL of
sample in Nessler tubes. View vertically over a white
background. The sample must be no darker than the
standard.
8.3 pH of a 1% solution — Dilute 2.5 mL (2.8 g) of
sample to 100 mL with carbon dioxide- and ammonia-
free water. Using a pH meter determine the pH at 25°C
1 to 2 minutes after immersion of electrodes. The pH
range 6.0–7.5 corresponds to 0.2% free hydrogen
fluoride (HF) to 0.2% ammonium hydroxide (NH
4
OH)
in the original solution.
8.4 Chloride — Mix 2.2 mL (2.5 g) of sample with 20
mL of water containing 0.5 g of boric acid. Add 1 mL
of nitric acid and 1 mL of silver nitrate reagent solution,
and allow to stand for 5 minutes. Any turbidity
produced should be no greater than that produced when
0.01 mg of chloride ion (Cl) is treated as the sample.
8.5 Nitrate — To 2 mL of water in a white plastic
beaker, add 0.9 mL (1 g) of sample, 1 mL of sulfuric
acid, 0.05 mL of 0.01 N (0.002 M) potassium
permanganate, mix, and decolorize with sodium
SEMI C20-1101 © SEMI 1978, 2001 AMMONIUM FLUORIDE 40%2
arsenite reagent solution. Dilute to 50 mL with brucine
sulfate reagent solution and mix. Heat the solution in a
preheated (boiling water) bath for 10 minutes. Cool
rapidly in an ice bath to room temperature. The yellow
color of the sample should be no greater than that
produced when 0.01 mg of nitrate ion (NO
3
) is treated
as the sample.
8.6 Phosphate — To a 9 mL (10 g) sample in a
platinum dish, add 1 mL of sodium carbonate reagent
solution and 40 mL of nitric acid. Evaporate carefully,
to prevent spattering, to near dryness. Cool, wash down
the sides of the dish with 5 mL of nitric acid, and
evaporate to dryness. Repeat the evaporation with nitric
acid two more times to ensure complete removal of all
the fluoride. To the cooled dish, add 25 mL of 0.5 N
sulfuric acid to dissolve the residue, warming if
necessary. Cool, transfer to a color comparison tube,
and add 1 mL of ammonium molybdate reagent solu-
tion, 1 mL of p-(methylamino)phenol sulfate reagent
solution, and allow to stand at room temperature for 2
hours. Any blue color should be no greater than that
produced when 0.01 mg of phosphate ion (PO
4
) is
treated as the sample.
8.7 Sulfate — To 23 mL (25 g) of sample, add 10 mL
of sodium carbonate reagent solution and heat gently
until sample has been volatilized. To the residue add 5
mL of hydrochloric acid and evaporate to dryness in a
hood. Dissolve the residue in 10 mL of water and 1 mL
of dilute hydrochloric acid (1 + 19); filter if necessary.
Add 1 mL of barium chloride reagent solution, mix, and
allow to stand for 10 minutes. Any turbidity developed
should be no greater than that produced when 0.05 mg
of sulfate ion (SO
4
) solution is treated as the sample.
8.8 Arsenic and Antimony (as As) — To 30 mL (33 g)
in a fluoroplastic beaker, add 20 mL of nitric acid and 5
mL of hydrochloric acid, and evaporate to dryness in a
sand bath in a hood. Completely volatilize the
ammonium fluoride, but do not bake. Add 10 mL of
water and 5 mL of sulfuric acid and evaporate to dense
fumes of sulfur trioxide. Cool, cautiously add 10 mL of
water, and again evaporate to dense fumes of sulfur
trioxide. Cool, and cautiously wash into a generator
flask with water to make a volume of 35 mL. Proceed
as described in the General Method for Arsenic (and
Antimony) under SEMI C1, Section 3.4.5, starting with
the sentence that begins, “Swirl the flask....” Any red
color in the silver diethyldithiocarbamate solution of
the sample should be no greater than that of the
standard containing 0.001 mg of arsenic (As).
8.9 Trace Element Contents — By a suitable emission
spectrographic procedure, determine for each of the
specified trace elements that its content is not greater
than the stated specification limit (see SEMI C1,
Section 3.5, Guidelines for Emission Spectrography).
9 Grade 2 Procedures
9.1 This section does not apply to this chemical.
10 Grade 3 Procedures
10.1 This section does not apply to this chemical.
11 Grade 4 Procedures
11.1 This section does not apply to this chemical.
12 Grade 5 Procedures
12.1 This section does not apply to this chemical.
13 VLSI Grade Procedures
13.1 Specific procedures for this grade do not exist.
Refer to Section 8 for available procedures.
14 Tier A Procedures
14.1 Standardized test methods are being developed for
all parameters at the purity levels indicated. The
Process Chemicals Committee considers a test method
to be valid only if there is a documented recovery study
showing a recovery of 75–125%. Recovery is for a
known sample spike at 50% of the specified level.
15 Tier B Procedures
15.1 Standardized test methods are being developed for
all parameters at the purity levels indicated. The
Process Chemicals Committee considers a test method
to be valid if there is a documented recovery study
showing a recovery of 75–125%. Recovery is for a
known sample spike at 50% of the specified level.
16 Tier C Procedures
16.1 This section does not apply to this chemical.
17 Tier D Procedures
17.1 This section does not apply to this chemical.