semi合集-English.pdf - 第6639页
SEMI C23-0301 © SEMI 1981, 2001 B U FFER E D O X ID E ETC H A N TS 4 17 Tier C P rocedures 17.1 This section does not apply to t h i s chemical. 18 Tier D P rocedures 18.1 This section does not apply to t h i s chemical.…
BUFFERED OXIDE ETCHANTS SEMI C23-0301 © SEMI 1981, 20013
produced when 0.01 mg of chloride ion (Cl) is treated
as the sample.
10.4 Nitrate — To 2 mL of water in a white plastic
beaker, add 0.9 mL (1g) of sample, 1 mL of sulfuric
acid, 0.05 mL of 0.01 N (0.002 M) potassium
permanganate, mix, and decolorize with sodium
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.
10.5 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 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
solution, 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.
10.6 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.
10.7 Trace Metals Analysis
10.7.1 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), silver (Ag), 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.
10.7.2 Special Reagents
10.7.2.1 Nitric Acid, Ultrapure — Use nitric acid
specified for low metal ion content.
10.7.2.2 4% Nitric Acid Solution — Dilute 40 mL of
ultrapure nitric acid to 1 L using water meeting the
criteria for Type E1.1 in ASTM D5127.
10.7.2.3 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.
10.7.2.4 Indium Internal Standard — Make up a
indium internal standard solution to a concentration of
20 µg/mL (ppm) from an appropriate concentrated
indium standard solution.
10.7.3 Sample Preparation
10.7.3.1 In a clean environment, weigh 10.0 g sample
into a cleaned Teflon beaker and evaporate the sample
on a 250°C hotplate to near dryness. Carefully add 1
mL of the ultrapure nitric and 3 mL of water and gently
warm for several minutes. Cool to room temperature,
add 25 µL of the indium internal standard, and dilute
with Type E1.1 water to a final weight of 25.0 g.
10.7.4 Analysis
10.7.4.1 Using the prepared solutions and blanks,
analyze sodium, potassium, calcium, and iron by
graphite furnace atomic absorption (GFAA) and the
remaining elements by inductively coupled plasma
mass spectrometry (ICP/MS). For calibration, the
standards are made up in 4% nitric acid solution with
final concentration of 20 ng/g of the indium internal
standard. Run a reagent blank.
11 Grade 3 Procedures
11.1 This section does not apply to this chemical.
12 Grade 4 Procedures
12.1 This section does not apply to this chemical.
13 Grade 5 Procedures
13.1 This section does not apply to this chemical.
14 VLSI Grade Procedures
14.1 This section does not apply to this chemical.
15 Tier A Procedures
15.1 This section does not apply to this chemical.
16 Tier B Procedures
16.1 This section does not apply to this chemical.
SEMI C23-0301 © SEMI 1981, 2001 BUFFERED OXIDE ETCHANTS4
17 Tier C Procedures
17.1 This section does not apply to this chemical.
18 Tier D Procedures
18.1 This section does not apply to this chemical.
Table 1 Impurity Limits and Other Requirements for Buffered Oxide Etchants
Previous SEMI Reference # C2.2-95 C7.23-0697
Grade 1 Grade 2
(Specification) (Specification)
Chloride (Cl) -- 4 ppm max
Nitrate (NO
3
) -- 10 ppm max
Phosphate (PO
4
) -- 1 ppm max
Sulfate (SO
4
) -- 2 ppm max
Aluminum (Al) 0.2 ppm max 10 ppb max
Antimony (Sb) -- 10 ppb max
Arsenic (As) -- 10 ppb max
Arsenic and Antimony (as As) 0.03 ppm max --
Boron (B) 0.2 ppm max 20 ppb max
Calcium (Ca) 0.2 ppm max 10 ppb max
Chromium (Cr) 0.1 ppm max 5 ppb max
Copper (Cu) 0.1 ppm max 5 ppb max
Gold (Au) 0.3 ppm max 10 ppb max
Iron (Fe) 0.2 ppm max 5 ppb max
Lead (Pb) 0.3 ppm max 10 ppb max
Magnesium (Mg) 0.2 ppm max 10 ppb max
Manganese (Mn) 0.2 ppm max 10 ppb max
Nickel (Ni) 0.2 ppm max 10 ppb max
Potassium (K) 0.3 ppm max 5 ppb max
Sodium (Na) 0.3 ppm max 5 ppb max
Tin (Sn) 0.3 ppm max 10 ppb max
Titanium (Ti) 0.3 ppm max 10 ppb max
Zinc (Zn) 0.3 ppm max 5 ppb max
Particles in bottles:
size, #/mL
≥ 1.0 µm, 25 max ≥ 0.5 µm, 150 max
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.
n-BUTYL ACETATE SEMI C24-0301 © SEMI 1978, 20011
SEMI C24-0301
SPECIFICATION FOR n-BUTYL ACETATE
This specification was technically approved by the Global Process Chemicals Committee and is 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 at www.semi.org February
2001; to be published March 2001. This document replaces SEMI C1.5 in its entirety. Originally published
in 1978; previously published June 1999.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for n-butyl acetate 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 n-butyl acetate 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 n-butyl
acetate used in the semiconductor industry.
2.2 These standards do not purport to address safety
issues, if any, associated with their use. It is the
responsibility of the user of these standards 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
4.1 SEMI Standards
SEMI C1 — Specifications for Reagents
4.2 ASTM Standards
1
ASTM D5127 — Standard Guide for Ultra Pure Water
Used in the Electronics and Semiconductor Industry
NOTE 1: As listed or revised, all documents cited shall be the
latest publications of adopted standards.
5 Terminology
5.1 None.
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
6 Physical Property (for information only)
Density at 25°C 0.88 g/mL
Boiling Point 126.5°C
7 Requirements
7.1 The requirements for n-butyl acetate for Grade 1
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 — Analyze the sample b y gas
chromatography (see SEMI C1, Section 3.1, Guidelines
for Assay by Wide Bore Column Gas
Chromatography). The parameters cited have given
satisfactory results.
Column: 30 meter × 530 micron I.D. fused silica
capillary, coated with 5 micron film of DB-1 or
equivalent (100% methyl silicone which has been
surface bonded and cross linked).
Column Temperature: 40°C isothermal for 5 minutes,
then programmed to 200°C at 10°C/min.
Injector Temperature: 150°C
Detector Temperature: 250°C
Sample Size: 0.2 µL splitless
Carrier Gas: Helium at 3 mL/min
Detector: Thermal Conductivity
Approximate Retention Times
(min):
Butyl Acetate 8.0
8.2 Color — Dilute 3.0 mL of platinum-cobalt stock
solution (APHA No. 500) to 100 mL with water.
Compare this standard (APHA No. 15) 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 Acidity — To 57 mL (50 g) of sample in a 250 mL
conical flask, add 0.5 mL of phenolphthalein indicator
solution and titrate with 0.1 N alcoholic potassium
hydroxide until a slight pink color persists for at least