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SEMI P15-92 © SEMI 1992, 2004 1 SEMI P15-92 (Reapproved 1104) DETERMINATION OF SODIUM AN D POTASSIUM IN POSITIVE PHOTORESIST METAL ION FREE (MIF) DEVELOPERS BY ATOMI C ABSORPTION SPECTROSCOPY This standard was techn ical…
SEMI P14-0997 © SEMI 1991, 19971
SEMI P14-0997
DETERMINATION OF TIN IN POSITIVE PHOTORESISTS BY GRAPHITE
FURNACE ATOMIC ABSORPTION SPECTROSCOPY
1 Scope
1.1 This procedure is a graphite furnace atomic
absorption analytical method for tin in photoresist. The
applicable concentration range is 0.1 to 1 ppm when the
sample is diluted one to ten. The precision was found to
be within 0.1 ppm in a round robin analysis between
four laboratories.
2 Instrument Conditions
2.1 An atomic absorption spectrometer equipped with
a graphite furnace is used with graphite tubes equipped
with pyrrolitically coated graphite platforms for
sampling.
2.2 The 224.6 nm emission line from a hollow cathode
tin lamp is used as the analytical absorption line.
Furnace Program*
Dry Step Char Step
Atomization
Step
Temperature (°C) 110 800 2700
Ramp time (s) 20 20 0 +
Hold time (s) 20 20 5
+ Maximum power heating
* Argon flow rate of 50 mL/min
3 Sample Preparation
3.1 The sample is diluted 1/10 (1 part sample + 9 parts
solvents weight/weight) in 2-methoxyethanol or another
suitable solvent for positive resist. The solvent should
contain less than 0.01 ppm of tin.
4 Standards
4.1 The standards should be weight/weight (mg/kg)
and should be diluted weight/weight since results will
be expressed in mg/kg.
4.2 A 50 ppm tin standard is prepared by diluting a
500 ppm tin standard in oil to 50 ppm with Xylene.
4.3 A 1 ppm standard is made by diluting the 50 ppm
standard in 2-methoxyethanol or another suitable
solvent.
5 Procedure
5.1 A 20 µL volume of 1 ppm tin standard is
transferred to the platform by Eppendorf pipette. The
furnace program is run and absorbance measured. The
absorbance of the 1ppm tin standard should be in the
range of 0.2 absorbance. Measure the absorbance of
the solvent and sample in an identical manner.
6 Calculation
p
pm tin (mg/kg
)
=
Abs. Sample × ppm Standard × dilution factor
Abs. Standar
d
6.1 Detection Limit — The detection limit is a
function of the dilution factor and can vary by
instrument. The solution factor should be taken into
account in calculation of the detection limit.
6.1.1
Detection limit (ppm) = s × dilution factor where
s = standard deviation of instrument reading in PPM.
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.
SEMI P15-92 © SEMI 1992, 2004 1
SEMI P15-92 (Reapproved 1104)
DETERMINATION OF SODIUM AND POTASSIUM IN POSITIVE
PHOTORESIST METAL ION FREE (MIF) DEVELOPERS BY ATOMIC
ABSORPTION SPECTROSCOPY
This standard was technically approved by the Global Micropatterning Committee and is the direct
responsibility of the North American Micropatterning Committee. Current edition approved by the North
American Regional Standards Committee on July 11, 2004. Initially available at www.semi.org September
2004; to be published November 2004. Originally published in 1992.
1 Scope
1.1 This procedure is a flame atomic absorption
analytical method for sodium and potassium analysis in
photoresist MIF developers. The applicable
concentration range is 20 to 1000 ppb.
NOTICE: This standard does not purport to address
safety issues, if any, associated with its use. It is the
responsibility of the users of this standard to establish
appropriate safety and health practices and determine
the applicability of regulatory or other limitations prior
to use.
2 Referenced Standards
2.1 None.
3 Terminology
3.1 None.
4 Instrument Conditions
4.1 Atomic Absorption Spectrometer — The analytical
wavelength for sodium is 589 nm and for potassium is
766 nm. The instrument conditions (i.e., slit width,
burner gas flow rates) should be set according to the
manufacturer’s manual. Optimize the nebulizer and
lamp alignment to maximize the absorbance of the 1
ppm standard.
5 Standards
5.1 The standards should be weight/weight (mg/kg)
and should be diluted weight/weight since results will
be expressed in mg/kg.
5.2 The standards are prepared by diluting a
concentrated stock. For example, a 500 ppm standard of
sodium is diluted to 50 ppm with de-ionized water. This
solution is then diluted to 1 ppm.
6 Procedure
6.1 No sample preparation nor dilution is required.
6.2 Set the absorbance reading to zero with the flame
ignited and no sample aspirating. Measure the
absorbance of the 1 ppm standards and samples. The
absorbance of the standard should be in the range of 0.2
absorbance. Duplicate sample and standard readings
should be within 0.01 absorbance. The effect of
viscosity on delivery to the burner can be determined
by adding 2 ppm of a potassium internal standard to the
sample and checking the absorbance versus an external
2 ppm potassium standard. The potassium level in the
developer, if any, should be subtracted.
7 Calculation
ppm (mg/kg) =
Abs. Sample
p
pm Standard
R
Abs. Standard
R = Recovery factor due to sample viscosity if
applicable.
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 or equipment mentioned
herein. These standards are subject to change without
notice.
By publication of this standard, Semiconductor
Equipment and Materials International (SEMI) takes no
position respecting the validity of any patent rights or
copyrights asserted in connection with any items
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 of
the contents in whole or in part is forbidden without express written
consent of SEMI.
SEMI P16-92 © SEMI 1992, 2004 1
SEMI P16-92 (Reapproved 1104)
DETERMINATION OF TIN IN POSITIVE PHOTORESIST METAL ION
FREE (MIF) DEVELOPERS BY GRAPHITE FURNACE ATOMIC
ABSORPTION SPECTROSCOPY
This standard was technically approved by the Global Micropatterning Committee and is the direct
responsibility of the North American Micropatterning Committee. Current edition approved by the North
American Regional Standards Committee on July 11, 2004. Initially available at www.semi.org September
2004; to be published November 2004. Originally published in 1992.
1 Scope
1.1 This procedure is a graphite furnace atomic
absorption analytical method for tin in photoresist MIF
developers. The applicable concentration range is 20 to
1000 ppm.
NOTICE: This standard does not purport to address
safety issues, if any, associated with its use. It is the
responsibility of the users of this standard to establish
appropriate safety and health practices and determine
the applicability of regulatory or other limitations prior
to use.
2 Referenced Standards
2.1 None.
3 Terminology
3.1 None.
4 Instrument Conditions
4.1 An atomic absorption spectrometer equipped with a
graphite furnace is used with graphite tubes equipped
with pyrolytic coated graphite platforms for sampling.
4.2 The 224.6 nm emission line from a hollow cathode
tin lamp is used as the analytical absorption line.
Table 1 Furnace Program*
Dry Step
Char Step
Atomization
Step
Temperature
(°C)
110 800 2700
Ramp time (s) 20 20 0
#2
Hold time (s) 20 20 5
#1: * Argon flow rate of 50 mL/min
#2: + Maximum power heating
5 Standards
5.1 The standards should be weight/weight (mg/kg)
and should be diluted weight/weight since results will
be expressed in mg/kg.
5.2 A 50 ppm tin standard is prepared by diluting a 500
ppm tin standard to 50 ppm with de-ionized water.
5.3 A 1 ppm standard is made by diluting the 50 ppm
standard.
6 Procedure
6.1 No sample preparation nor dilution is required.
6.2 A 20 mL volume of 1 ppm tin standard is
transferred to the platform by Eppendorf pipette. The
furnace program is run and absorbance measured. The
absorbance of the 1 ppm tin standard should be in the
range of 0.2 absorbance. Measure the absorbance of the
sample in an identical manner.
7 Calculation
ppm tin (mg/kg) =
Abs. Sample
p
pm Standard
Abs. Standard
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 or equipment mentioned
herein. These standards are subject to change without
notice.
By publication of this standard, Semiconductor
Equipment and Materials International (SEMI) takes no
position respecting the validity of any patent rights or
copyrights asserted in connection with any items
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 of
the contents in whole or in part is forbidden without express written
consent of SEMI.