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SULFURIC A C ID SEMI C44-0301 © SEMI 1978, 20 01 5 Previous SEMI Ref erenc e # C1.16-96 C 7.8-94 C11.5-9 4 C8.8-92 Grade 1 Grade 2 V LSI Grade Tier B Tier C (Specif ication) (Specif ication) (Guideline) (Guideline) (Guid…
SEMI C44-0301 © SEMI 1978, 2001 SULFURIC ACID4
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.
14 Tier A Procedures
14.1 This section does not apply to this chemical.
15 Tier B Procedures
15.1 Standardized test methods are being developed
for all parameters at the purity levels indicated. Until
standardized test methods are published, test
methodology shall be determined by user and producer.
The Chemical Reagent 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.
16 Tier C Procedures
16.1 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.
17 Tier D Procedures
17.1 This section does not apply to this chemical.
Table 1 Impurity Limits and Other Requirements for Sulfuric Acid
Previous SEMI Reference # C1.16-96 C7.8-94 C11.5-94 C8.8-92
Grade 1 Grade 2 VLSI Grade Tier B Tier C
(Specification) (Specification) (Guideline) (Guideline) (Guideline)
Assay (H
2
SO
4
) 95.0–97.0% 95.0–97.0 % 95.0–97.0% 95.0–97.0% 95.0–97.0%
Color (APHA) 10 max 10 max 10 max 10 max 10 max
Residue after Ignition -- -- 3 ppm max -- --
Chloride (Cl) 0.1 ppm max 100 ppb max 0.1 ppm max 50 ppb max 50 ppb max
Nitrate (NO
3
) 0.2 ppm max 200 ppb max 0.2 ppm max 100 ppb max 100 ppb max
Phosphate (PO
4
) 0.5 ppm max 500 ppb max 0.5 ppm max 100 ppb max 100 ppb max
Matters Reducing KMnO
4
(as O)
-- -- 2 ppm max -- --
Aluminum (Al) 0.2 ppm max 10 ppb max 0.02 ppm max 1 ppb max 100 ppt max
Ammonium (NH4) -- -- 1 ppm max -- --
Antimony (Sb) -- 5 ppb max -- 1 ppb max 100 ppt max
Arsenic (As) -- 10 ppb max -- 1 ppb max 100 ppt max
Arsenic and Antimony (as As) 0.005 ppm max -- 0.01 ppm max -- --
Barium (Ba) -- 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Beryllium (Be) -- 10 ppb max 0.01 ppm max 1 ppb max --
Bismuth (Bi) -- 10 ppb max 0.05 ppm max 1 ppb max --
Boron (B) 0.02 ppm max 20 ppb max 0.02 ppm max 1 ppb max 100 ppt max
Cadmium (Cd) -- 10 ppb max 0.01 ppm max 1 ppb max --
Calcium (Ca) 0.3 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Chromium (Cr) 0.2 ppm max 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Cobalt (Co) -- 5 ppb max 0.01 ppm max 1 ppb max --
Copper (Cu) 0.1 ppm max 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Gallium (Ga) -- 10 ppb max 0.01 ppm max 1 ppb max --
Germanium (Ge) -- 10 ppb max 0.01 ppm max 1 ppb max --
Gold (Au) 0.3 ppm max 5 ppb max 0.02 ppm max 1 ppb max --
Indium (In) -- -- 0.01 ppm max -- --
Iron (Fe) 0.2 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Lead (Pb) 0.3 ppm max 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Lithium (Li) -- 10 ppb max 0.01 ppm max 1 ppb max --
SULFURIC ACID SEMI C44-0301 © SEMI 1978, 20015
Previous SEMI Reference # C1.16-96 C7.8-94 C11.5-94 C8.8-92
Grade 1 Grade 2 VLSI Grade Tier B Tier C
(Specification) (Specification) (Guideline) (Guideline) (Guideline)
Magnesium (Mg) 0.3 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Manganese (Mn) 0.2 ppm max 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Molybdenum (Mo) -- 10 ppb max 0.02 ppm max 1 ppb max --
Nickel (Ni) 0.1 ppm max 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Niobium (Nb) -- 10 ppb max -- 1 ppb max --
Platinum (Pt) -- -- 0.05 ppm max -- --
Potassium (K) 0.3 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Silicon (Si) -- -- -- 1 ppb max --
Silver (Ag) -- 10 ppb max 0.01 ppm max 1 ppb max --
Sodium (Na) 0.3 ppm max 10 ppb max 0.1 ppm max 1 ppb max 100 ppt max
Strontium (Sr) -- 10 ppb max 0.02 ppm max 1 ppb max --
Tantalum (Ta) -- 10 ppb max -- 1 ppb max --
Thallium (Tl) -- 10 ppb max 0.05 ppm max 1 ppb max --
Tin (Sn) 0.2 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Titanium (Ti) 0.3 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Vanadium (V) -- 10 ppb max 0.01 ppm max 1 ppb max --
Zinc (Zn) 0.2 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Zirconium (Zr) -- 10 ppb max 0.05 ppm max 1 ppb max --
Particles in bottles
(size, #/mL)
≥ 1.0 µm, 25 max ≥ 0.5 µm, 25 max ≥ 0.5 µm, 250 max
(See NOTE 1.) (See NOTE 1.)
NOTE 1: 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: SEMI makes no warranties or representations as to the suitability of the standard 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.
TETRAETHYLORTHOSIILICATE (TEOS) SEMI C45-0301 © SEMI 1991, 20011
SEMI C45-0301
SPECIFICATION AND GUIDELINE FOR TETRAETHYLORTHOSILICATE
(TEOS)
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 October 17, 1999. Initially available at
www.semi.org February 2001; to be published March 2001. This document replaces SEMI C7.13 in its
entirety. Originally published in 1991; previously published June 1999.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for tetraethylorthosilicate 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 tetraethylorthosilicate
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
tetraethylorthosilicate 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)
6.1 Not applicable.
7 Requirements
7.1 The requirements for tetraethylorthosilicate for
Grade 1 and Tier A 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 by gas
chromatography (see SEMI C1, Section 3.1, Guidelines
for Assay by Wide Bore Column Gas
Chromatography). The parameters cited have given
satisfactory results.
8.1.1 Column 30 meter x 530 micron fused silica
capillary, coated with 5 micron film of DB-1 or
equivalent (100% methyl silicone which has been
surface bonded and cross linked).
8.1.2 Column Temperature 60°C isothermal for 1
minute, then programmed to 200°C at 20°C/min.
Injector Temperature: 120°C
Detector Temperature:
260°C
Sample Size: 1 µL splitless
Carrier Gas: Helium at 3 mL/min
Detector: Thermal Conductivity
Retention Times (min)
Water 2.0
Ethanol 2.5
TEOS 7.8
8.2 Color
Dilute 1.0 mL of platinum-cobalt stock
solution (APHA No. 500) to 100 mL with water.
Compare this standard (APHA No. 5) 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 Water The cell is dried with a dry nitrogen gas
stream for twenty minutes. Reagents are added and a
blank (no sample) is run. Add 5 g of sample to the dry