uppliers to the worlds semiconductor manufacturing industry have

been forced to keep costs down during the current industry down-
turn, and BOC Edwards (BOCE), a major supplier of equipment,
materials and services for the industry, is no exception.
BOCEs electronic gas purification and filling facility in Medford, OR, felt
the impact of the stagnant semiconductor industry in spring 2001, as the
plant was investing in quality initiatives, including QS-9000 automotive qual-
ity certification, kaizen and Six Sigma. Since these initiatives required invest-
ment, BOCE steered along Medfords quality road with sharp eyes looking
for positive results; and Medford delivered. One of the plants leading qual-
ity achievements in 2001 was a Six Sigma Black Belt (BB) project involving
tungsten hexafluoride (WF
6
) gas.
Business Drivers
The cost and quality demands of the semiconductor industry set the stage
for launching the BB project. Chip manufacturers focus on managing costs
more stringently during economic downturns. They must balance costs in
an industry where sophisticated processes use specialty gases and chemicals
to fabricate semiconductor devices that must be consistently pure to avoid
costly yield failures. This puts pressure on suppliers to offer the best prices
and still maintain consistently high quality materials required for the micro-
scopic geometries of the devices.
The plant chose the electronic gas, WF
6
, for its BB project because of the
importance of the material to the industry. Electronic gases such as WF
6
are
typically supplied in steel or nickel cylinders and are used in the production
of electronic devices.
WF
6
is used to make dynamic random access memory (DRAM). The tung-
sten atoms in WF
6
are excellent conductors of electricity and form part
of the circuitry in a semiconductor. DRAMs are memory chips and make it
possible to save files on a computer. Impurities can poison DRAMs and
destroy the memory at a considerable expense to the chip manufacturer.
Therefore, the WF
6
used in the process needs to be consistent and clean.
The BB project was sensitive to the cost and quality demands of the indus-
try, and the project offered the Medford team an opportunity to address the
cost challenges.
Purified WF
6
is an expensive material to make because of its high raw
material cost, extensive processing requirements and stringent purity
requirements. Even though Medford was producing high quality WF
6
, not
all specifications were being met 100% of the time. This resulted in expen-
sive rework.
CA S E S T U D Y
Process Improvement
At BOC Edwards
THIS ELECTRONIC
GAS FILLING FACILITY
USED SIX SIGMA TO
REDUCE COST AND
IMPROVE QUALITY.
S
By Brian Zievis,
BOC Edwards
38
I
F E B R U A R Y 2 0 0 3
I
W W W . A S Q . O R G
Pr ocess I mpr ovement at BOC Edwar ds
Project Implementation
To start the Six Sigma project, a team of chemists
and process engineers set out to reduce the variation
in tested cylinders of WF
6
to eliminate defects and
improve the consistency of the material. To complete
its mission, the team opened the Six Sigma toolbox
and applied statistical methods to Medfords WF
6
processes.
The team applied statistical tools to the gas analysis
laboratory by performing a measurement systems
analysis. The impurities measured in WF
6
are at low
concentrations, and the lab is in charge of testing
both gas phase and liquid phase impurities.
A typical WF
6
gas specification is shown in Table 1.
The impurities tested in the gas phase are measured
in parts per million, and the metal or elemental impu-
rities tested in the liquid phase are measured in parts
per billion units. When impurity specifications are as
low as those in the table, even the slightest measure-
ment or sampling errors can make the results appear
inconsistent. The team realized that before the prod-
uct could be improved, the cause of measurement
variation needed to be understood and minimized.
Experimentation
The team chose regression analysis to measure the
performance of the analytical methods that test gas
phase impurities in WF
6
. A gas blending system (see
Figure 1) was used to produce reference standards of
each gas impurity in a range of concentrations (stan-
dard addition). The device uses mass flow controls to
blend gas components in a matrix of WF
6
. Each blend-
ed level of impurity gave corresponding responses
from the instruments being validated. The analytical
lab used a gas chromatograph (GC) and a fourier
transform infrared spectrometer (FTIR) to measure
WF
6
s gas phase impurities. Once the standard addi-
tion experiments were completed, regression curves
for the resulting data told how well the methods meas-
ured each specified impurity.
These experiments revealed some errors. For exam-
ple, the results for the GC method that measure
carbon dioxide (CO
2
) fit into a quadratic prediction
response rather than a linear one. Regression
Manifold
xxxx xxxxx xxx xxxx xxxxx
xxx xxxx xx xxxxx xx
Product
Standard Diluent
Standards
blender
Uses cylinder gas
or permeation gas
standards.
More rigorous than
gas analysis industry
standards.
Detection limits
calculated at 99.73%
confidence.
Figure 1. Gas Blending System
Table 1. Typical WF
6
Gas Specifications
Tungsten hexafluoride (WF
6
)
Gas phase impurities Specification parts per million
N
2
1
O
2
+ Ar 1
CO 0.5
CO
2
1
SiF
4
0.5
SF
6
0.5
CF
4
1
Acidity (HF) 10
Liquid phase metals Specification parts per billion
Al 10
As 10
B 10
Ca 15
Cd 2
Cr 10
Cu 20
Fe 10
K 10
Mn 10
Na 10
Mg 10
Mo 25
Ni 100
U 0.05
Th 0.05
S I X S I G M A F O R U M M A G A Z I N E
I
F E B R U A R Y 2 0 0 3
I
39
experiments for the impurity using the FTIR provided
a much better method and gave a tight, linear
response for the impurity.
Figure 2 shows a comparison between the linear
regression experiments for the GC and FTIR. Simply
put, the blue prediction intervals for the GC experi-
ment were much wider than those calculated for the
FTIR method. After discovering the FTIR provided
the best measurement, it became the standard
method for testing CO
2
.
Deviations were found as regression experiments
were performed on all the gas phase impurities.
Method parameters were adjusted, and experiments
were repeated until prediction intervals for the
responses were made as lean as possible. Detection
limits (99.73% confidence in a WF
6
matrix) plummet-
ed, and analytical result distributions narrowed.
Experiments were also performed on the high reso-
lution inductively coupled plasma mass spectrometer
(ICP-MS) used to measure metal impurities in WF
6
. In
this case, gauge repeatability and reproducibility
(R&R) studies were used to assess the measurement
system.
To test hazardous material such as WF
6
using an
ICP-MS, a number of sample preparation steps are
performed. Each of these steps contributes to meas-
urement error, and the gauge R&R studies run on the
ICP-MS were able to quantify those errors. Once
known, the plant fixed the errors by modifying the
procedures and reinstructing the chemists.
Removing the noise from the measurements helped
link any remaining variation to the way the cylinder
valves were being prepared. When the plant modified
the way it prepared the valves used for WF
6
cylinders,
its liquid phase metal results improved. Some results
gave nothing more than flattened responses, such as
those for potassium (see Figure 3).
Measurement Systems Analysis Benefits
The optimized analytical methods reduced standard
deviations and kept borderline results from tripping
over specification limits. Product that once may have
been mistakenly rejected because of measurement
errors could now be approved.
Several benefits resulted from the measurement sys-
tems analysis:
To maintain the measurement improvement
gains, the team implemented control charts for
critical instrument parameters, such as the chro-
matographic response factor for nitrogen impuri-
ty (see Figure 4). The statistical charts ensured the
lab instruments remained stable and kept instru-
ment noise from cluttering the control charts used
to monitor final product results, such as those for
nitrogen (see Figure 5). The charts then became
more reliable at detecting process variation so it
could be removed. Natural process boundaries,
rather than customer specifications, became the
acceptance criteria for processing WF
6
.
Pr ocess I mpr ovement at BOC Edwar ds
40
I
F E B R U A R Y 2 0 0 3
I
W W W . A S Q . O R G
0
10
5
0 1 2 3 4 5 6 7 8 9 10
G
C

C
O
2

m
e
a
s
u
r
e
m
e
n
t
GC standard addition
0
5
4
3
2
1
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
F
T
I
R

C
O
2

m
e
a
s
u
r
e
m
e
n
t
FTIR standard addition
Linear gas chromotograph (GC)
model for CO
2
GC CO
2
measurement = 0.178799
+ 1.05995 GC standard addition
Standard deviation = 0.230309
R-Sq* = 99.6%
R-Sq(adj)** = 99.6%
Regression
99.73% confidence interval
99.73% prediction interval
Regression
99.73% confidence interval
99.73% prediction interval
Linear fourier transform infrared
spectrometer (FTIR) model for CO
2
FTIR CO
2
measurement = 0.0422653
+ 1.12868 FTIR standard addition
Standard deviation = 0.0162956
R-Sq = 100%
R-Sq(adj) = 100%
* R-Sq: coefficient of determination.
** R-Sq(adj): coefficient of determination adjusted for degrees of freedom.
Figure 2. GC and FTIR Linear Regression
Experiment Results
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
1 10 19 28 37 46 55 64 73 82 91 100 109 118 127 136 145
P
a
r
t
s

p
e
r

b
i
l
l
i
o
n
Figure 3. Liquid Phase Metal Test Results
For Potassium
Pr ocess I mpr ovement at BOC Edwar ds
With its reengineered and finely tuned processes,
the lab reduced the total cost of producing WF
6
.
The lab also produced a more efficient workplace,
as less time was required to analyze WF
6
.
The new WF
6
analysis process flow diagrams now
included fewer steps. All method redundancies
were removed. Some methods were even elimi-
nated because the plant was able to roll old meth-
ods for testing impurities into those that are more
efficient and accurate.
Modified test plans allowed batch testing for some
impurities. At the same time, test results on ana-
lytical reports for the material were more accurate
and consistent.
Inefficiencies on the Plant Floor
With the measurement systems analysis completed,
the Six Sigma team expected production methods on
the plant floor were responsible for any remaining
inconsistencies in the purity of the final product.
The team first looked at process variation causing
the amount of hydrogen fluoride (HF) found in WF6
cylinders, because the impurity was a leading cost fac-
tor of the plant. After optimizing the FTIR method
that tested HF, results for the impurity remained
inconsistent. The team realized additional lab
improvements were not going to fix the problem, so it
shifted its focus from the lab to improving the WF
6
fill-
ing process itself. Team members brainstormed and
listed the variables that might be causing the HF
rejects.
The purifier used to produce high purity WF
6
included operating parameters that were critical to
delivering high purity WF
6
, but the team believed the
purifier settings were likely not causing the HF prob-
lems. The purifier had already been studied exten-
sively, long before the Six Sigma project started, and it
was automated with alarms that signaled any out of
control conditions.
The cylinder package variables, on the other hand,
were more suspicious. Packaging in the cylinder gas
industry refers to parameters involving cylinders and
valves. Cylinders can vary by type, the way they are
washed, dried and evacuated on filling systems before
fill and how they are filled. Valves can vary by their
construction or the way they are maintained. Package
variables can impact the final purity of electronic
gases, especially when impurities are as low as those
included in WF
6
specifications.
The team decided to test the four packaging vari-
ables it suspected were influencing the amount of HF
in WF
6
cylinders. This time, a design of experiments
(DOE) was developed using a four-factor fractional
factorial. Following Six Sigma guidelines, the team
S I X S I G M A F O R U M M A G A Z I N E
I
F E B R U A R Y 2 0 0 3
I
41
Individual
UCL
CL
USL
Individual: Control limit (CL): 0.0243243 Upper control limit (UCL): 0.4
Lower control limit (LCL): None Rule violation subgroup size 1
Upper specification limit (USL): 1 Lower specification limit (LSL): None
0
0.2
0.4
0.6
0.8
1
Date:
3
/
9
/
0
2
6
/
2
/
0
1
6
/
1
2
/
0
1
9
/
8
/
0
1
9
/
1
9
/
0
1
1
0
/
1
9
/
0
1
1
1
/
1
8
/
0
1
1
/
2
0
/
0
2
1
/
2
5
/
0
2
Figure 5. Nitrogen Concentration Control Chart
8.0
18.0
15.5
13.0
10.5
A B C D
-1 1 -1 1 -1 1 -1 1
H
y
d
r
o
g
e
n

f
l
o
u
r
i
d
e
p
a
r
t
s

p
e
r

m
i
l
l
i
o
n
Figure 6. Variables Main Effects on Amount
Of Measurable Hydrogen Fluoride
Individual: Control limit (CL): 0.0048890 Upper control limit (UCL): 0.0052571
Lower control limit (LCL): 0.0045210 Rule violation subgroup size 1
Individual
CL
LCL
UCL
0.0042
0.0044
0.0046
0.0048
0.005
0.0052
0.0054
0.0056
0.0058
5 10 15 20 25 30
Figure 4. Gas Chromotograph Response
Factor for Nitrogen Impurity
Pr ocess I mpr ovement at BOC Edwar ds
avoided the traditional one factor at a time approach
and developed a disciplined, well thought out experi-
ment using replication and randomization.
Sixteen WF
6
cylinders were filled using combina-
tions of the suspect variables set at two levels. The gas
laboratory then measured the HF concentration in
each of the cylinders. Statistical analysis of the main
and interactive effects of the variables identified two
package variables where low level settings yielded high
HF in WF
6
. When both variables were set at their high
settings, they produced WF
6
with the lowest amounts
of HF. Figure 6 (p. 41) shows the main effects of the
variables at the two levels on the measured results of
HF in the cylinders.
The DOE results led to a dramatic reduction in the
cost of HF defects and, at the same time, delivered
improved WF
6
by reducing the amount of impurity in
the final product. The team then implemented proce-
dures to control the package variables. Solving the
troublesome HF problem in WF
6
improved yields by
15.5%. Had the DOE not been performed, the signifi-
cance of the packaging variables would likely have
remained undetected. Instead, the concentration of
HF in tested cylinders of WF
6
decreased and became
more consistent.
Overall Applications
Six Sigma methods used to improve WF
6
were imme-
diately applied to all Medfords gas production
processes, resulting in cost reductions and material
improvements. In addition, the plants quality invest-
ment in kaizen training started to pay off as the kaizen
teams began using new high powered statistical meth-
ods to solve other plant challenges.
All these initiatives take place in a QS-9000 work-
place now that Medford received its certification in
February 2002. The Six Sigma WF
6
project has become
a process improvement recipe for other cylinder gas
plants, and electronic materialsBOCEs division that
supplies semiconductor gases and materialshas initi-
ated BB projects throughout its production plants to
deliver consistently purer materials at more competi-
tive prices.
42
I
F E B R U A R Y 2 0 0 3
I
W W W . A S Q . O R G
WHAT DO YOU THINK OF THIS ARTICLE? Please share
your comments and thoughts with the editor by e-mailing
godfrey@asq.org.