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SEMI P32-1104 © SEMI 1998, 2004 3 7.3 Environment 7.3.1 The measurement is recomm ended to be performed in a clean room or clean zone at constant temperature. The stability of temperature should be better tha n ± 2°C. Dr…

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SEMI P32-1104 © SEMI 1998, 2004 2
6 Apparatus
6.1 Measurement Equipment
6.1.1 Flame Atomic Absorption Spectrometer (F-AAS)
and ICP-MS can be applied to the dry ashing method.
6.1.2 Graphite Furnace Atomic Absorption
Spectrometer (GF-AAS), Electrothermal Atomization
Atomic Absorption Spectrometer (ETA-AAS), ICP-
MS, MIP-MS, and Inductively Coupled Plasma Atomic
Emission Spectrometer (ICP-AES) can be applied to
the direct method.
6.1.3 Instrument Condition — Recommended
instrumental conditions are summarized in Table 1 for
each target metal.
Table 1 Measurement Equipment and Metal Elements
Plasma Ion Source Mass Spectrometry
Element
Atomic Absorption
Spectroscopy
ICP-MS (Note 1) MIP-MS (Note 2)
ICP-Atomic Emission
Spectrometer
Al 309.2 nm
27
Al
27
Al 396.2 nm
Ca 422.7 nm
40
Ca,
44
Ca (Note 3)
40
Ca 393.4 nm
Cr 357.9 nm
359.4 nm
52
Cr,
53
Cr
(Note 3)
52
Cr 267.7 nm
283.6 nm
Cu 324.7 nm
63
Cu,
65
Cu
63
Cu,
65
Cu 324.8 nm
Fe 248.3 nm
56
Fe,
54
Fe
(Note 3)
56
Fe,
54
Fe 259.9 nm
Mg 285.2 nm
24
Mg,
25
Mg,
26
Mg
24
Mg,
25
Mg,
26
Mg 279.6 nm
Mn 279.5 nm
55
Mn (Note 3)
55
Mn 257.6 nm
Ni 232.0 nm
341.4 nm
58
Ni,
60
Ni
(Note 3)
58
Ni,
60
Ni 221.6 nm
231.6 nm
K 766.5 nm
39
K,
41
K (Note 3)
39
K,
41
K 766.5 nm
Na 589.0 nm
23
Na
23
Na 589.0 nm
NOTE 1: ICP-MS — Ar is used as the plasma generation gas.
NOTE 2: MIP-MS — N
2
is used as the plasma generation gas.
NOTE 3: Beware of interfering ion (see Table 2).
Table 2 Interfering Ions
Object Metal Interfering Ion
39
K
38
Ar
1
H
41
K
40
Ar
1
H
40
Ca
40
Ar
52
Cr
40
Ar
12
C,
36
Ar
16
O,
38
Ar
14
N
55
Mn
40
Ar
14
C
1
H,
40
Ar
15
N,
38
Ar
16
O
1
H
56
Fe
40
Ar
16
O,
38
Ar
18
O
58
Ni
40
Ar
18
O
7 Vessels, Reagents, and Environment
7.1 Vessel
7.1.1 Quartz glass volumetric flask
7.1.2 Quartz glass measuring pipette
7.1.3 Quartz glass beaker
7.1.4 PTFE vessel
7.1.5 Platinum crucible
7.2 Reagents
7.2.1 DI Water — Resistivity ≥ 18.0 MΩ cm at 25°C
per ASTM D 1193.
7.2.2 Organic Reagent — Use commercially
guaranteed reagent for trace metal analysis.
7.2.3 Inorganic Reagent — Use commercially
guaranteed reagent for trace metal analysis.
7.2.4 Standard Reagent — Use the commercially
guaranteed reagents which have certified trace metals
concentration.
SEMI P32-1104 © SEMI 1998, 2004 3
7.3 Environment
7.3.1 The measurement is recommended to be
performed in a clean room or clean zone at constant
temperature. The stability of temperature should be
better than ± 2°C. Dry ashing method should be
performed in a draft chamber with HEPA filter, if
possible.
7.3.2 In the case of volumetric analysis, the
measurement environment is set to the standard
temperature of measuring tools such as volumetric flask
and measuring pipette.
8 Procedures
8.1 Flow Chart of Measurement — Refer to Figure 1
as suggested analysis process.
Figure 1
Flow Chart of Trace Metal Measurement
SEMI P32-1104 © SEMI 1998, 2004 4
8.2 Blank Test
8.2.1 Prepare a blank test solution.
8.2.2 Measure each blank test solution.
8.2.3 The observed data should be adjusted for background correction, if necessary.
8.2.4 Confirmation 1 — Blank level should be equal or less than half the specification level in the photoresist.
8.3 Working Curve
8.3.1 The concentration range in the working curve should cover the anticipated concentration in photoresist test
solution.
8.3.2 Prepare a standard solution with a known metal concentration using the reagents that are used in preparing the
photoresist test solution.
8.3.3 Measure each metal element in the standard solution.
8.3.4 The observed data should be adjusted for the blank level and background correction.
8.3.5 Prepare a working curve for each metal element.
8.3.6 Confirmation 2 — Working curve should be linear in the concentration range of standard solution.
8.4 Measurement of Photoresist Test Solution
8.4.1 Dry Ashing Method
8.4.1.1 Remove the solvent of photoresist by evaporation using Platinum crucible.
8.4.1.2 Ash the matrix by heating using Platinum crucible. Ashing temperature should be referred to Table 3. Resist
cannot be ashed without possible loss of some elements, so loss of each element should be investigated before trace
metal analysis.
Table 3 Recommended Ashing Temperature
Element Ashing Temperature (°C) Flame Component
Al 1000 N
2
O-C
2
H
2
Ca 800 Air-C
2
H
2
N
2
O-C
2
H
2
Cr 800 Air-C
2
H
2
N
2
O-C
2
H
2
Cu 800 Air-C
2
H
2
F3 (NOTE 4) 600
300 (if FeCl
3
presents)
Air-C
2
H
2
N
2
O-C
2
H
2
Mg 600 Air-C
2
H
2
N
2
O-C
2
H
2
Mn 800 Air-C
2
H
2
N
2
O-C
2
H
2
Ni 800 Air-C
2
H
2
K (NOTE 5) < 500 Air-C
2
H
2
H
2
-O
2
Na (NOTE 5) < 500 Air-C
2
H
2
H
2
-O
2
NOTE 4: Iron can be present as ferric chloride and ferric chloride boils at 310°C.
NOTE 5: These elements tend to volatilize over 500°C.
8.4.1.3 Dissolve the ash in platinum crucible with acid.
8.4.1.4 Prepare a photoresist test solution in a volumetric flask with a constant volume of solvent.
8.4.1.5 In F-AAS analysis, analytical wavelength should be determined referring to Table 1. In ICP-MS analysis,
analytical mass number should be determined referring to Table 1.
8.4.1.6 Measure each metal element in the photoresist test solution.
8.4.1.7 The observed data should be adjusted for blank level and background corrections.