semi合集-English.pdf - 第6632页

SEMI C21-0301 © SEMI 1978, 2001 AMMONIUM HY DROXIDE 6 14 Tier A Procedures 14.1 This section does not apply to t h i s chemical. 15 Tier B P rocedures 15.1 This section does not apply to t h i s chemical. 16 Tier C P roc…

100%1 / 7923
AMMONIUM HYDROXIDE SEMI C21-0301 © SEMI 1978, 20015
NOTE 8: Each laboratory is responsible for verifying the
validity of each method within its own operation.
11.1 Non-Metal Impurities
11.1.1 See Section 8, which contains procedures for
the following tests:
Assay
Color (APHA)
Carbon Dioxide
Substances Reducing Permanganate
11.2 Anions
11.2.1 The following method has given satisfactory
results in determining anion impurities at the values
specified for each of the following anions: chloride
(Cl), phosphate (PO
4
), nitrate (NO
3
), and sulfate (SO
4
).
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 anion.
11.2.2 Reagents
11.2.2.1 Eluent — Prepare an eluent solution that is
2.2 mM sodium carbonate (Na
2
CO
3
) and 0.75 mM so-
dium bicarbonate (NaHCO
3
) in deionized water meet-
ing the criteria for Type E1.1 in ASTM D5127. Store
eluent under a helium gas blanket.
11.2.2.2 Regenerant — Prepare a 0.025 N sulfuric
acid (H
2
SO
4
) in deionized water meeting the criteria for
Type E1.1 in ASTM D5127.
11.2.2.3 Potassium Carbonate Solution — Prepare a
solution containing 500 mg of reagent grade potassium
carbonate (K
2
CO
3
) in 100 mL of water meeting the
criteria for Type E1.1 in ASTM D5127.
11.2.3 Sample Preparation
11.2.3.1 In a clean environment, place 200 g of sample
into a clean beaker. Add 1 mL of a 5 mg/mL potassium
carbonate solution and evaporate carefully (at 100°C) to
a volume of 0.5 mL. Dilute with water meeting the
criteria for Type E1.1 in ASTM D5127 to a final
volume of 20 mL.
11.2.4 Analysis
11.2.4.1 Using the prepared solutions and blanks,
analyze chloride, nitrate, phosphate, and sulfate by ion
chromatography. Run a reagent blank. Samples and
reagent blanks should be prepared and analyzed in
triplicate.
11.2.4.2 Columns — Precolumn should be AG4-A
(Dionex) or equivalent, and separation column should
be AS4-A (Dionex) or equivalent.
11.3 Trace Metals Analysis
11.3.1 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.
11.3.2 Special Reagents
11.3.2.1 Nitric Acid, Ultrapure — Use nitric acid of
low metal ion content.
11.3.2.2 2% Nitric Acid Solution — Dilute ultrapure
nitric acid with water meeting the criteria for Type E1.1
in ASTM D5127.
11.3.2.3 Water — The water used for dilution,
calibration, and standards should meet, at a minimum,
the criteria for Type E1.1 in ASTM D5127 in regard to
cation analysis.
11.3.2.4 Internal Standard Solution — Make up an
internal standard solution to a concentration of 1000
µg/mL from appropriate concentrated scandium, yttri-
um, indium, thulium, and thorium standard solutions.
11.3.3 Sample Preparation
11.3.3.1 In a clean environment, in a teflon bottle,
evaporate a 50.0 g sample at low heat until approxi-
mately 5 g of the sample remains. Cool to room temper-
ature, add 100 µL of the internal standard solution, and
dilute with 2% nitric acid to a final weight of 10.0 g.
11.3.4 Analysis
11.3.4.1 Using the prepared solutions and blanks,
calibrate the instrument and analyze calcium, iron,
sodium, and potassium by cool plasma inductively
coupled plasma mass spectrometry (ICP-MS) and the
remaining elements by normal plasma ICP-MS.
11.3.4.2 Calculations — All data were reported
relative to an appropriate 1.0 µg/L standard and
corresponding blank solution. Internal standard
corrections were applied to the data.
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 Sections 8 and 9 for available procedures.
SEMI C21-0301 © SEMI 1978, 2001 AMMONIUM HYDROXIDE6
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 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.
Table 1 Impurity Limits and Other Requirements for Ammonium Hydroxide
Previous SEMI Reference # C1.4-95 C7.1-96 C8.1-0298 C17.1-0298 C11.1-94 --
Grade 1 Grade 2 Grade 3 Grade 4 VLSI Grade Tier D
(Specification) (Specification) (Specification) (Specification) (Guideline) (Guideline)
Assay (as NH
3
) 28.0 - 30.0% 28.0 - 30.0% 28.0 - 30.0% 28.0 - 30.0% 25.0 - 27.0% o
r
28.0 - 30.0%
28.0 - 30.0%
Appearance To pass test -- -- -- -- --
Color (APHA) 10 max 10 max 10 max 10 max 10 max 10 max
Residue after Ignition -- -- -- -- 2 ppm max --
Residue after Evaporation -- -- -- -- 10 ppm max --
Substances Reducing KMnO
4
(as O)
-- -- -- -- 5 ppm max --
Substances Reducing
Permanganate
To pass test To pass test To pass test To pass test -- --
Carbon Dioxide (CO
2
) 20 ppm max 20,000 ppb max 20 ppm max 20 ppm max -- 20 ppm max
Carbonate (CO
2
) -- -- -- -- 10 ppm max --
Chloride (Cl) 0.5 ppm max 200 ppb max 100 ppb max 50 ppb max 0.5 ppm max 30 ppb max
Nitrate (NO
3
) -- 400 ppb max 100 ppb max 50 ppb max -- 30 ppb max
Phosphate (PO
4
) 0.5 ppm max 200 ppb max 100 ppb max 40 ppb max 0.2 ppm max 30 ppb max
Silica (SiO
2
) -- -- -- -- 0.2 ppm max --
Sulfide (S) -- -- -- -- 0.2 ppm max --
Sulfate (SO
4
) -- 200 ppb max 100 ppb max 50 ppb max 2 ppm max 30 ppb max
Total Sulfur (SO
4
) 1 ppm max -- -- -- -- --
Aluminum (Al) 0.3 ppm max 10 ppb max 1 ppb max 100 ppt max 0.05 ppm max 10 ppt max
Antimony (Sb) -- 5 ppb max 1 ppb max 100 ppt max -- 10 ppt max
Arsenic (As) -- 5 ppb max 1 ppb max 100 ppt max -- 10 ppt max
Arsenic and Antimony (as As) 0.05 ppm max -- -- -- 0.05 ppm max --
Barium (Ba) -- -- -- -- 0.01 ppm max 10 ppt max
Beryllium (Be) -- -- -- -- 0.01 ppm max --
Bismuth (Bi) -- -- -- -- 0.02 ppm max --
Boron (B) 0.1 ppm max 10 ppb max 1 ppb max 100 ppt max 0.01 ppm max 10 ppt max
Cadmium (Cd) -- -- -- -- 0.01 ppm max 10 ppt max
Calcium (Ca) 0.3 ppm max 10 ppb max 1 ppb max 100 ppt max 0.1 ppm max 10 ppt max
Chromium (Cr) 0.2 ppm max 10 ppb max 1 ppb max 100 ppt max 0.01 ppm max 10 ppt max
Cobalt (Co) -- -- -- -- 0.01 ppm max --
Copper (Cu) 0.1 ppm max 10 ppb max 1 ppb max 100 ppt max 0.01 ppm max 10 ppt max
Gallium (Ga) -- -- -- -- 0.01 ppm max --
Germanium (Ge) -- -- -- -- 0.05 ppm max --
Gold (Au) 0.3 ppm max 10 ppb max 1 ppb max 100 ppt max 0.02 ppm max --
AMMONIUM HYDROXIDE SEMI C21-0301 © SEMI 1978, 20017
Previous SEMI Reference # C1.4-95 C7.1-96 C8.1-0298 C17.1-0298 C11.1-94 --
Grade 1 Grade 2 Grade 3 Grade 4 VLSI Grade Tier D
(Specification) (Specification) (Specification) (Specification) (Guideline) (Guideline)
Indium (In) -- -- -- -- 0.01 ppm max --
Iron (Fe) 0.1 ppm max 10 ppb max 1 ppb max 100 ppt max 0.05 ppm max 10 ppt max
Lead (Pb) 0.2 ppm max 10 ppb max 1 ppb max 100 ppt max 0.01 ppm max 10 ppt max
Lithium (Li) -- -- -- -- 0.01 ppm max --
Magnesium (Mg) 0.3 ppm max 10 ppb max 1 ppb max 100 ppt max 0.05 ppm max 10 ppt max
Manganese (Mn) 0.2 ppm max 10 ppb max 1 ppb max 100 ppt max 0.01 ppm max 10 ppt max
Molybdenum (Mo) -- -- -- -- 0.01 ppm max --
Nickel (Ni) 0.1 ppm max 10 ppb max 1 ppb max 100 ppt max 0.01 ppm max 10 ppt max
Platinum (Pt) -- -- -- -- 0.02 ppm max --
Potassium (K) 0.3 ppm max 10 ppb max 1 ppb max 100 ppt max 0.1 ppm max 10 ppt max
Silver (Ag) -- -- -- -- 0.01 ppm max --
Sodium (Na) 0.3 ppm max 10 ppb max 1 ppb max 100 ppt max 0.2 ppm max 10 ppt max
Strontium (Sr) -- -- -- -- 0.01 ppm max --
Thallium (Tl) -- -- -- -- 0.02 ppm max --
Tin (Sn) 0.3 ppm max 10 ppb max 1 ppb max 100 ppt max 0.02 ppm max 10 ppt max
Titanium (Ti) 0.3 ppm max 10 ppb max 1 ppb max 100 ppt max 0.01 ppm max 10 ppt max
Vanadium (V) -- -- -- -- 0.01 ppm max --
Zinc (Zn) 0.3 ppm max 10 ppb max 1 ppb max 100 ppt max 0.05 ppm max 10 ppt max
Zirconium (Zr) -- -- -- -- 0.01 ppm max --
Particles in bottles:
size, #/mL
≥ 1.0 µm, 25
max
≥ 0.5 µm, 25
max
≥ 0.5 µm, 25
max
≥ 0.5 µm, 25
max (see
NOTE 1)
≥ 0.5 µm, 250
max
(See NOTE 2.)
NOTE 1: Care must be taken in analyzing particles because of the potential formation of microbubbles.
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.
NOTICE: 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. 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.