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SEMI P16-92 © SEMI 1992, 2004 1 SEMI P16-92 (Reapproved 1104) DETERMINATION OF TIN IN PO SITIVE PHO TORESIST METAL ION FREE (MIF) DEVELOPERS BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROSCOPY This standard was techn ical…
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.
SEMI P17-92 © SEMI 1992, 19991
SEMI P17-92 (Reapproved 0299)
DETERMINATION OF IRON, ZINC, CALCIUM, MAGNESIUM, COPPER,
BORON, ALUMINUM, CHROMIUM, MANGANESE, AND NICKEL IN
POSITIVE PHOTORESIST METAL ION FREE (MIF) DEVELOPERS BY
INDUCTIVELY COUPLED PLASMA EMISSION SPECTROSCOPY (ICP)
This standard was technically reapproved by the Resist Committee and is the direct responsibility of the North
American Microlithography Committee. Current edition approved by the North American Regional Standards
Committee in October 1998. Initially available at www.semi.org February 1999; to be published February 1999.
Originally published in 1992; previously published in 1996.
1 Scope
This procedure is an ICP plasma emission analysis for
determination of iron, zinc, calcium, magnesium,
copper, boron, aluminum, chromium, manganese, and
nickel in photoresist MIF developers. The applicable
concentration range and detection limit will depend
upon the element and instrument.
2 Spectrometer
An instrument with resolution sufficient to separate the
analytical emission lines in Table 1 is required.
Table 1. Analytical Lines of the Elements
Elements Analytical Line nm
Aluminum 396.152
Calcium 317.933
Copper 324.754
Iron 239.562
Boron 208.960
Magnesium 285.213
Nickel 231.604
Zinc 213.856
Chromium 283.563
Manganese 257.610
3 Standards
The standards should be weight/weight (mg/kg) and
should be diluted weight/weight since results will be
expressed in mg/kg.
The standards are prepared by diluting a concentrated
standard. For example, a 500 ppm standard is diluted to
50 ppm with deionized water. This solution is then
diluted to 0.25 ppm.
4 Plasma Conditions
The sample is pumped in the region of 0.7 mL/min.
usually with a peristaltic pump attached to the
nebulizer. The argon plasma flow rate and RF power
should be optimized for the sample using settings
recommended in the manufacturer manual. Generally, a
plasma gas flow rate of 12 L/min and an RF power of
1.25 kW is required.
5 Quantitation
No sample preparation nor dilution is required.
The detector gain is set by measuring the 0.25 ppm
standard. The standard should be run intermittently to
satisfy reasonable precision. Standard and sample
readings should be repeatable within 0.03 ppm. The
effect of sample viscosity on delivery of diluted sample
to the plasma was not found to be a factor for this
procedure. This effect can be checked by adding an
internal standard of an element known not to be present
in the sample (such as Yttrium) at 1 ppm and checking
the emission response vs. an external 1 ppm Yttrium
standard.
6 Calculation
ppm element (mg/kg)=
Ιx
Ιs
×0.25 ppm
Where Ιx = emission intensity of sample
Ιs = emission intensity of 0.25 ppm standard