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TETRAETHYLORTHOSIILICATE (TEOS) SEMI C45-0301 © SEMI 1991, 20 01 1 SEMI C45-0301 SPECIFICA TION A ND GUIDELINE FOR TETRAETHYLORTHOSILICA TE (TEOS) This specif ication and this guidelin e were tec hnically a pproved by th…
SULFURIC ACID SEMI C44-0301 © SEMI 1978, 20015
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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
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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
SEMI C45-0301 © SEMI 1991, 2001 TETRAETHYLORTHOSIILICATE (TEOS)2
Coulometric Karl Fischer water analyzer. Results are
obtained in ppm by dividing the micrograms of water
found in the sample by weight of TEOS in grams.
8.4 Trace Metals Analysis The following method
has given satisfactory results in determining trace metal
impurities at the specified value for each of the
following trace metals: aluminum (Al), arsenic (As),
calcium (Ca), chromium (Cr), copper (Cu), 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.
8.4.1 Special Reagents All water used in the Trace
metals Analysis and Boron Analysis should be a
deionized water meeting the criteria for Type E1.1 in
ASTM D5127.
8.4.1.1 Mixed Acid 1% HF - 2% HNO
3
prepared by
dilution of ultra pure acids with appropriate weights of
deionized water.
8.4.1.2 Standards
Composite standard solutions
containing 0, 1, 2, and 4 ppb multi-element standards
are prepared by diluting with mixed acid of appropriate
weights for ICP-MS. Single-element standards are
prepared (Ca, Fe, K, Na) for GFAA.
8.4.2 Sample Preparation In a clean environment,
place 100 g of sample in a clean PFA Teflon closed
bottle equipped with an inlet and outlet tube and
evaporate under a nitrogen purge at approximately
110°C. When dry, close the inlet and the outlet tube
and digest the residue at 100°C for 30 minutes with 7
mL of mixed acid solution. Cool and transfer the con-
tents with deionized water. Dilute the transferred con-
tents with deionized water to a final volume of 14 mL.
8.4.3 Analysis Analyze the samples by graphite
furnace atomic absorption (GFAA) for sodium,
calcium, potassium, and iron. Analyze the sample for
all other metallic elements by inductively coupled
plasma mass spectrometry (ICP-MS).
8.5 Boron Analysis The following method has
given satisfactory results in the determination of trace
levels of boron (B). Alternate methods may be used as
long as appropriate studies demonstrate recovery
between 75–125% of a known sample spike for half of
the specified value.
8.5.1 Standard Standards of 0, 2, and 4 ppm boron
are prepared by dilution of an aqueous boron stock
solution with deionized water meeting the criteria for
Type E1.1 in ASTM D5127.
8.5.2 Sample Preparation A 100 g sample of TEOS
is extracted with 10 mL of deionized water, that meets
the criteria for Type E1.1 in ASTM D5127, by
vigorously shaking the solution for minimum of 10
minutes on a mechanical shaker. Allow the layers to
separate and remove the aqueous portion to a separate
container.
8.5.3 Analysis The 10 mL water extract is analyzed
for boron by inductively coupled plasma atomic
emission spectroscopy (ICP-AES) at 249.68 nm.
9 Grade 2 Procedures
9.1 This section does not apply to this chemical.
10 Grade 3 Procedures
10.1 This section does not apply to this chemical.
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 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.
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.