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AMMONIUM HYDROXIDE SEMI C21-0301 © SEMI 1978, 20 01 1 SEMI C21-0301 SPECIFICA TIONS AND GUIDELINES FOR A MMONIUM HYDROXIDE These specific ations and gui delines were technica lly approv ed by the Global Proc ess Chem ic …

SEMI C20-1101 © SEMI 1978, 2001 AMMONIUM FLUORIDE 40%4

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Grade 1 VLSI Grade Tier A Tier B

(Specification) (Guideline) (Guideline) (Guideline)

Particles in bottles:

size, #/mL

≥ 1.0 µm, 25 max ≥ 0.5 µm, 250 max

See NOTE 2. See NOTE 2.

NOTE 1: For III-V compound users only.

NOTE 2: Due to the limitations of current particle counters, particle size and number are to be agreed upon between supplier and user. See SEMI

C1, Section 3.9 for particle counting methodology.

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AMMONIUM HYDROXIDE SEMI C21-0301 © SEMI 1978, 20011

SEMI C21-0301

SPECIFICATIONS AND GUIDELINES FOR AMMONIUM HYDROXIDE

These specifications and 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 October 17, 1999. Initially available on

SEMI OnLine February 2001; to be published March 2001. This document replaces SEMI C1.4, C7.1, C8.1,

C11.1, and C17.1 in their entirety. Originally published in 1978, 1990, 1992, 1994, and 1997 respectively;

previously published June 2000.

1 Purpose

1.1 The purpose of this document is to standardize

requirements for ammonium hydroxide 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 hydroxide

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 hydroxide 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 The guideline for VLSI grade ammonium

hydroxide is only applicable for materials that remain

below 25°C during transport and storage.

4 Referenced Standards

4.1 SEMI Standards

SEMI C1 — Specifications for Reagents

4.2 ASTM Standards

ASTM D5127 — Standard Guide for Ultra Pure Water

Used in the Electronics and Semiconductor Industry

1 American Society for Testing and Materials, 100 Barr Harbor

Drive, West Conshohocken, Pennsylvania 19428-2959, USA.

Telephone: 610.832.9585, Fax: 610.832.9555. Website:

www.astm.org

NOTE 1: As listed or revised, all documents cited shall be the

latest publications of adopted standards.

5 Terminology

5.1 None.

6 Physical Property (for information only)

Density at 25°C

0.90 g/mL

7 Requirements

7.1 The requirements for ammonium hydroxide for

Grades 1, 2, 3, and 4, and VLSI Grade are listed in

Table 1.

8 Grade 1 Procedures

NOTE 2: Each laboratory is responsible for verifying the

validity of the method within its own operation.

8.1 Assay — Accurately weigh a small glass-stoppered

flask containing about 15 mL of water. Deliver from a

pipet about 2 mL of the sample near the water surface,

stopper immediately, and reweigh. Add 0.1 mL of

methyl red indicator solution and titrate with

standardized 1 N hydrochloric acid to a yellow-to-red

color change.

%Assay

of HCl

1.703

Weight of sample g

()

8.2 Appearance — Place 15 mL of the sample in a 20

× 150 mm test tube and compare with water in a similar

tube. Viewed across the column by means of

transmitted light, the two liquids should be equal in

clarity and free from suspended matter.

8.3 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.

8.4 Carbon Dioxide — Dilute 11 mL (10 g) of sample

with 10 mL of carbon dioxide-free water and add 5 mL

of a clear, saturated solution of barium hydroxide. Any

turbidity should be no greater than that produced when

SEMI C21-0301 © SEMI 1978, 2001 AMMONIUM HYDROXIDE2

the same volume of the barium hydroxide solution is

added to 21 mL of the carbon dioxide-free water

containing 0.5 mg of anhydrous sodium carbonate.

8.5 Substances Reducing Permanganate — Dilute 3

mL (2.7 g) of sample with 5 mL of water. Add 50 mL

of 10% sulfuric acid and 0.05 mL of 0.1 N (0.02 M)

potassium permanganate. Boil for 5 minutes. The pink

color should not be entirely discharged.

8.6 Chloride — To 22 mL (20 g) of sample, add 10

mL of sodium carbonate reagent solution and evaporate

to dryness on a steam bath in a hood. Dissolve the

residue in 10 mL of water. Add 1 mL of nitric acid.

Filter, if necessary, through a chloride-free filter. Dilute

to 20 mL with water and add 1 mL of silver nitrate

reagent solution. Any turbidity produced should be no

greater than that produced when 0.01 mg of chloride

ion (Cl) is treated as the sample.

8.7 Phosphate — Evaporate 22 mL (20 g) of sample to

dryness on a steam bath in a hood. Take up the residue

with 25 mL of approximately 0.5 N sulfuric acid. Add 1

mL of ammonium molybdate reagent solution and 1 mL

of p-(methylamino)phenol sulfate reagent solution, and

allow to stand for 2 hours at room temperature. Any

blue color should be no greater than that produced

when 0.01 mg of phosphate ion (PO

) is treated as the

sample.

8.8 Total Sulfur (as SO

) — To 56 mL (50 g) of

sample, add 1 mL of sodium carbonate reagent solution

and evaporate on a steam bath in a hood to a volume of

about 5 mL. Add 2 mL of bromine water and evaporate

to dryness. Dissolve the residue with 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

) is treated

as the sample.

8.9 Arsenic and Antimony (as As) — Evaporate 44 mL

(40 g) of sample in a 150 mL beaker to a small volume

in a hood. Cool, cautiously add 10 mL of water and 5

mL of sulfuric acid, and 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 0.002 mg of arsenic (As).

8.10 Trace Metal Analysis — The following method

has given satisfactory results in determining trace metal

impurities at the value specified for each of the

following trace metal impurities at the value specified

for each of the following trace metals: aluminum (Al),

boron (B), calcium (Ca), chromium (Cr), copper (Cu),

gold (Au), iron (Fe), lead (Pb), magnesium (Mg),

manganese (Mn), nickel (Ni), potassium (K), sodium

(Na), tin (Sn), titanium (Ti), and zinc (Zn). Alternate

methods may be used as long as appropriate studies

demonstrate recovery between 75 - 125% of a known

sample spike for half of the value of each specified

item.

8.10.1 Special Reagents

8.10.1.1 5% Mannitol Solution — Weigh out 5 g of

Mannitol Powder (ACS Reagents Grade), and dilute to

100 mL using water meeting the criteria for Type E1 in

ASTM D5127. Mannitol solution is subject to attack by

microorganisms and should be carefully monitored for

such contamination.

8.10.1.2 Hydrochloric Acid, Ultra Pure — Use

hydrochloric acid specified for ultra low metal ion

content.

8.10.1.3 2% (v/v) Hydrochloric Acid Solution —

Dilute 20 mL of ultra pure hydrochloric acid to 1 L

using water meeting the criteria for Type E1 in ASTM

D5127.

8.10.2 Sample Preparation

8.10.2.1 In a clean environment, place 250 mL of

aqueous ammonium hydroxide in a PTFE dish. Add 0.5

mL of freshly prepared 5% mannitol solution. Slowly

evaporate on a hot plate, avoiding loss of sample by

effervescence or spattering until approximately 1 mL of

liquid remains. Cool. Add 1 mL of ultra pure, 12 M

hydrochloric acid. Continue heating until approximately

0.5 mL of liquid remains. Cool. Transfer quantitatively

to 50 mL volumetric flask using 2% (v/v) hydrochloric

acid for rinsing and dilution to volume. Run reagent

blank.

8.10.3 Analysis

8.10.3.1 Using the acid sample and reagent blank,

analyze group 1 elements by flame atomic absorption

spectroscopy and all other elements by plasma emission

spectroscopy.

NOTE 3: Due to the uncertainty of the acid concetration in

the liquid residue, the final concentration can be estimated at

approximately 1-2% (v/v). Standard calibration solutions are

to use this same acid concentration.

9 Grade 2 Procedures

NOTE 4: Each laboratory is responsible for verifying the

validity of the method within its own operation.

9.1 Non-Metal Impurities

9.1.1 See Section 8, which contains procedures for the

following tests: