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SEMI C33-0301 © SEMI 1986, 2001 n-METH YL 2-PYR R O LID O N E 6 Previous SEMI Refe rence # C1.25-9 5 C7.16-95 C8.11-0698 Grade 1 Grade 2 Grade 3 (Specificatio n) (Sp ecification) (Specificatio n) Boron ( B) 0.1 ppm max 2…

100%1 / 7923
n-METHYL 2-PYRROLIDONE SEMI C33-0301 © SEMI 1986, 20015
10.4 Trace Metal Analysis
10.4.1 The following method has given satisfactory
results in determining metal ion impurities at the values
specified for each of the following metals: aluminum
(Al), antimony (Sb), arsenic (As), 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 a recovery
between 75–125% of a known sample spike for half of
the value of each specified element.
10.4.2 Special Reagents
10.4.2.1 Nitric Acid, Ultra Pure — Use nitric acid
specified for low metal ion content.
10.4.2.2 Water — The water used for all the dilution,
calibration, and standards should meet, at a minimum,
the criteria for Type E1.1 in ASTM D5127 in regard to
cation analysis.
10.4.3 Sample Preparation
10.4.3.1 In a 100 mL volumetric, add 20 mL of sample
and fill to the mark such that the final solution contains
2% nitric acid.
10.4.4 Standard Preparation
10.4.4.1 Four standards are prepared such that the
final solution contains 2% nitric acid (i.e., 2% of 70%
nitric acid vol/vol) and 20% vol/vol sample. The four
standards are 0.5, 1, 5, and 10 ppb.
10.4.5 Analysis
10.4.5.1 This is a method of standard addition
procedure. Using the prepared solutions, analyze the
elements by inductively coupled plasma mass
spectrometry (ICP/MS).
10.4.5.2 Hot plasma conditions with shield are used
for the following elements: Ti, Mn, Ni, Cu, As, Sb, Sn,
Au, and Pb.
10.4.5.3 Cold plasma conditions with shield are used
for the follow elements, B, Na, Mg, Al, K, Ca, Cr, Fe,
and Zn.
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 This section does not apply to this chemical.
14 Tier A Procedures
14.1 This section does not apply to this chemical.
15 Tier B Procedures
15.1 This section does not apply to this chemical.
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.
Table 1 Impurity Limits and Other Requirements for n-Methyl 2-Pyrrolidone
Previous SEMI Reference # C1.25-95 C7.16-95 C8.11-0698
Grade 1 Grade 2 Grade 3
(Specification) (Specification) (Specification)
Assay (see NOTE 1) (CH
3
N(CH
2
)
3
CO) 99.5% min 99.8% min 99.8%
Color (APHA) 50 max 50 max 30 max
Water (H
2
O) 0.05% max 0.05% max 0.03% max
Free Amines (as CH
3
NH
2
) 50 ppm max 5,000 ppb max 5 ppm max
Chloride (Cl) 1 ppm max 500 ppb max 300 ppb max
Nitrate (NO
3
) -- 500 ppb max 400 ppb max
Phosphate (PO
4
) 5 ppm max 500 ppb max 250 ppb max
Sulfate (SO
4
) -- 500 ppb max 250 ppb max
Aluminum (Al) 0.1 ppm max 20 ppb max 5 ppb max
Antimony (Sb) -- 20 ppb max 10 ppb max
Arsenic (As) -- 20 ppb max 10 ppb max
Arsenic and Antimony (as As) 0.1 ppm max -- --
SEMI C33-0301 © SEMI 1986, 2001 n-METHYL 2-PYRROLIDONE6
Previous SEMI Reference # C1.25-95 C7.16-95 C8.11-0698
Grade 1 Grade 2 Grade 3
(Specification) (Specification) (Specification)
Boron (B) 0.1 ppm max 20 ppb max 10 ppb max
Cadmium (Cd) -- 20 ppb max --
Calcium (Ca) -- 20 ppb max 5 ppb max
Chromium (Cr) 0.1 ppm max 100 ppb max 10 ppb max
Cobalt (Co) -- 20 ppb max --
Copper (Cu) 0.1 ppm max 20 ppb max 5 ppb max
Gold (Au) 0.1 ppm max 20 ppb max 5 ppb max
Iron (Fe) 0.1 ppm max 20 ppb max 10 ppb max
Lead (Pb) 0.1 ppm max 20 ppb max 5 ppb max
Lithium (Li) -- 20 ppb max --
Magnesium (Mg) 0.1 ppm max 20 ppb max 5 ppb max
Manganese (Mn) 0.1 ppm max 100 ppb max 5 ppb max
Nickel (Ni) 0.1 ppm max 20 ppb max 5 ppb max
Potassium (K) 0.1 ppm max 20 ppb max 5 ppb max
Silver (Ag) -- 20 ppb max --
Sodium (Na) 0.3 ppm max 20 ppb max 10 ppb max
Strontium (Sr) -- 20 ppb max --
Tin (Sn) 0.1 ppm max 20 ppb max 5 ppb max
Titanium (Ti) 0.1 ppm max 20 ppb max 5 ppb max
Vanadium (V) -- 20 ppb max --
Zinc (Zn) 0.1 ppm max 100 ppb max 10 ppb max
Particles in bottles:
size, #/mL
≥ 1.0 µm, 10 max ≥ 0.5 µm, 200 max ≥ 0.5 µm, 15 max
NOTE 1: Assay by gas chromatography includes 3- and 4-methyl homologs.
NOTICE: SEMI makes no warranties or representations as to the suitability of the standards set forth herein for any
particular application. The determination of the suitability of the standard is solely the responsibility of the user.
Users are cautioned to refer to manufacturer’s instructions, product labels, product data sheets, and other relevant
literature respecting any materials mentioned herein. These standards are subject to change without notice.
The user’s attention is called to the possibility that compliance with this standard may require use of copyrighted
material or of an invention covered by patent rights. By publication of this standard, SEMI takes no position
respecting the validity of any patent rights or copyrights asserted in connection with any item mentioned in this
standard. Users of this standard are expressly advised that determination of any such patent rights or copyrights, and
the risk of infringement of such rights, are entirely their own responsibility.
Copyright by SEMI® (Semiconductor Equipment and Materials
International), 3081 Zanker Road, San Jose, CA 95134. Reproduction o
f
the contents in whole or in part is forbidden without express written
consent of SEMI.
MIXED ACID ETCHANTS SEMI C34-0699 © SEMI 1981, 19991
SEMI C34-0699
SPECIFICATION AND GUIDELINE FOR MIXED ACID ETCHANTS
This specification and this guideline 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 April 23, 1999. Initially available on
SEMI OnLine May 1999; to be published June 1999. This document replaces SEMI C2.1 and C7.19 in their
entirety. Originally published in 1981 and 1995 respectively.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for mixed acid etchants 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 mixed acid etchants
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 mixed
acid etchants used in the semiconductor industry.
3 Limitations
3.1 None.
4 Referenced Documents
SEMI C1 — Specifications for Reagents
SEMI C2 — Specifications for Etchants
5 Terminology
mixed acid etchant — any combination of nitric,
hydrofluoric, and acetic acids with the relative
composition expressed in terms of volumes of 70%
nitric acid, 49% hydrofluoric acid, and glacial acetic
acid, respectively. In the expression, all the relative
volumes shall be reduced to a ratio of the smallest
whole numbers. For example, a 3:1:2 mixed acid
etchant would imply a mixture of 3 volumes of 70%
nitric acid, 1 volume of 49% hydrofluoric acid, and 2
volumes of glacial acetic acid. If a component is absent,
its relative volume shall be taken as zero. For example,
a 3:1:0 mixed acid etchant would imply that no acetic
acid is present.
6 Composition
6.1 The content of each of the components of a mixed
acid etchant shall be expressed on a weight/weight basis
of the 100% acids in the total mixture. For the volume-
to-weight conversion, the densities shall be taken as
1.415, 1.153 g/mL, and 1.050 g/mL for 70% nitric acid,
49% hydrofluoric acid, and glacial acetic acid,
respectively.
7 Tolerances
Nitric Acid: ± 1.0% (± 0.16 meq/g)
Hydrofluoric Acid: ± 0.5% (± 0.25 meq/g)
Acetic Acid: ± 1.0% (± 0.17 meq/g)
8 Requirements
8.1 The requirements for mixed acid etchants for
Grade 1 and Tier A are listed in Table 1.
9 Grade 1 Procedures
9.1 Total Acidity — Accurately weigh a sample
containing 30 to 40 milliequivalents of acidity in a
polyethylene weighing bottle. Transfer with water to a
250 mL polyethylene beaker and dilute to
approximately 100 mL. Add 10 drops of
phenolphthalein indicator solution and titrate with 1 N
standardized sodium hydroxide to a faint pink end
point. Calculate the total acidity (A):
Total Acidity
me
q
g
()
=
mL
×
N
of NaOH
Weight of sample g
()
=
A
9.2 Hydrofluoric Acid — Accurately weigh a sample
containing 0.3 to 0.5 g of hydrofluoric acid in a
polyethylene weighing bottle. Transfer with water to a
polyethylene beaker and dilute to approximately 100
mL. Add 10 drops of phenolphthalein indicator solution
and titrate with 1 N or stronger sodium hydroxide
solution to a faint pink endpoint. Add 25 mL of Acetate
Buffer for Hydrofluoric Acid Determination and 1 g of
Eriochrome Cyanine R indicator mixture. Mix
continuously by magnetic stirring and titrate with
standardized aluminum chloride solution to a pink-
purple endpoint.
% Hydrofluoric Acid
=
mL
×
HF factor of AlCl
3
soln.
Weight of sample g
()
9.3 Nitric Acid — Accurately weigh a sample
containing 0.9 to 1.1 g of nitric acid in a polyethylene
weighing bottle. Quantitatively transfer into a 100 mL
volumetric flask containing 50 mL of 2% boric acid
solution, dilute to volume with water, and mix
thoroughly. Following the manufacturer's direction,