UPW-Micro Conference November 2008 Slide 1
High Flow Filter for UPW Applications – A Field Case Study
Gary Van Schooneveld, CT Associates Inc.Peter Nadolny, W.L. Gore and Associates, Inc
November 12, 2008
UPW-Micro Conference November 2008 Slide 2
• Critical feature sizes of current and developing semiconductor devices continue to drive the need for improved filter retention of particles smaller than 50 nm.
• Improvements in the retention of small particles in ultrapure water filters have typically come at the expense of increased pressure drop across the filter.
• Recent advances in membrane materials and structure has resulted in filters with improved particle retention and reduced pressure loss.
• This paper will review the performance of a newly developed 20 nm filter from WL Gore installed in a ultrahigh purity water system.
Introduction
UPW-Micro Conference November 2008 Slide 3
Presentation Outline
• Filter description and selection
• Water system description
• Post installation rinse-up measurements
• Particle and pressure drop performance
• 6 month performance check
• Summary
UPW-Micro Conference November 2008 Slide 4
Case Study Filter Description
• 10” Cartridge
• Media – Hydrophilic expanded PTFE
• Supports and Housing – Polypropylene
• O-rings – Viton Type 2-222
UPW-Micro Conference November 2008 Slide 5
Screening Tests – Filter Rinse-up
T h o rn to n2 0 0 C R
7 7 6 1 N R M
U P W
S iev e rs5 0 0 R L
e lec tro n icflo w m ete r
U P W
U P W
1 0 lp m
U P W re tu rn o r d ra in
U P W re tu rn o r d ra in
1 0 0 - 1 5 0 m L /m in
5 0 - 8 0 m L /m in
d ra in
U P W re tu rn
v en t
filte rh o u s in g
Pd iffe ren tia l
p re ssu resen so r
P M S M 5 0
U P W re tu rn o r d ra in
1 0 0 m L /m in
1 0 lp m
UPW-Micro Conference November 2008 Slide 6
Screening Tests – Filter Retention
H ig h P u rityW ate r
F lo wC o n tro lV a lv e
P e ris ta lticP u m p
P S L S u sp en s io no r T rito n X -1 0 0
S o lu tio n
3 0 0m l/m in
P M S M 5 01 0 0
m l/m in
P 1D ra in
D ra in
V en t
S h u t-o ff V a lv e
F ilte rH o u sin g
R e tu rn
P
d iffe ren tia lp re ssu re sen so r
P 2
1 0 lp m
e lec tro n icflo w m ete r
The test is a modified version of SEMATECH Provisional Test Method for Determining Particle Contribution and Retention by UPW Distribution System Components (1992).
Technology Transfer Number 92010949B.
UPW-Micro Conference November 2008 Slide 7
Filter Performance Comparisons
Attribute GORE 20 nm High Flow Filter
Supplier A - 20 nm (Polysulfone)
Supplier B -
40 nm (PES)
Particle Rinse Volume
(1 count added 50 nm)< 30 hours < 30 hours < 30 hours
TOC Rinse Volume
(0.1 ppb added)< 40 hours < 40 hours < 40 hours
Resistivity Rinse Volume
(0.1 M-cm added)< 1 hour < 1 hour < 1 hour
Non-Volatile Residue Rinse volume (0.1 ppb added)
< 3 hours < 35 hours < 50 hours
Filtration Efficiency – PSL Challenge ( 50 nm)
> 99.9% > 99.9% > 90%
Particles Released After Flow Stoppage ( 50 nm)
3 x 106 100 x 106 300 x 106
Pressure Drop @ 10 LPM 0.7 psid 2.2 psid 2.6 psid
Filters tested at 10 liters per minute flow rate.
UPW-Micro Conference November 2008 Slide 8
High Purity Water System Schematic
C atio nR esinC ity
W ate r
M ix edB ed
C arb o nF ilte r
0 .4 5 m ic ro nfilte r
C h a rg edM em b ran e
F ilte r
F 1
P 1
F 2
P 2
P 6P 7P 8
T 2R 2
P T 1
T O CM o n ito r
C h a rg edM em b ran e
F ilte r
0 .4 5 m ic ro nfilte r
H ig hP u rityT an k
F ilte r
1 8 5 /2 5 4 n mU V L ig h t
A n io nR esin
P 3 P 4
F 3
P 5
R 1
T 1
F 5
P 1 3
F M
1 8 5 /2 5 4 n mU V L ig h t
U ltra H ig h P u rityW ate r S y stem
UPW-Micro Conference November 2008 Slide 9
High Purity Water System
Parameter Typical Performance
Particle Concentration < 1 count/mL 100 nm
Total Organic Carbon (TOC) 40 – 100 ppb
Resistivity 18.1 M - cm
UPW-Micro Conference November 2008 Slide 10
UPW System Schematic (before case study filter installation)
U ltra -H ig hP u rityT an k
1 8 5 n m U V L ig h t
M ix edB e d
0 .4 5 m ic ro nfilte r
N R MM o n ito r
T O CM o n ito r
0 .0 5 m ic ro nfilte r
F 4
P 9 P 1 0 P 1 1
P 1 2
T 3
R 3
P T 2
P a rtic leC o u n te r
H ig h P u rityW a te r S y s tem
UPW-Micro Conference November 2008 Slide 11
Ultrahigh Purity Water System
Parameter Typical PerformanceParticle Concentration (# /mL 100 nm
< 0.05
Total Organic Carbon (ppb) < 1
Resistivity (M – cm) 18.2
Non-Volatile Residue (ppb) < 1
Operating Pressure (MPa) 0.27
Flow Rate (Lpm) 20
UPW-Micro Conference November 2008 Slide 12
Case Study Details
• The average flow rate for the water system at the time of the filter installation was 20 Lpm (4.5 gpm).
• The outlet pressure after the water system final filter was 0.26 MPa (37 psi).
• The water temperature was 27oC.
• The filter was installed in the final filter position replacing the 0.05 m filter in October 2007.
UPW-Micro Conference November 2008 Slide 13
UPW System Schematic(after case study filter installation)
U ltra -H ig hP u rityT an k
1 8 5 n m U V L ig h t
C u rren t U ltra H ig h P u rity W ate r S y stemB lo ck D iag ram
M ix edB e d
0 .4 5 m ic ro nfilte r
N R MM o n ito r
T O CM o n ito r
2 0 n me P T F E filte rF 4
P 9 P 1 0 P 1 1
P 1 2
T 3
R 3
P T 2
P a rtic leC o u n te r
H ig h P u rityW a te r S y s te m
UPW-Micro Conference November 2008 Slide 14
Case Study Instrumentation
Property Location Instrument
Particle concentrationEnd of loop
Out of filterPMS UDI 50 (x2)
Particle concentration Into test filter PMS M50
TOC End of loopG.E. Sievers Model
500RL
Nonvolatile residue End of loopFluid Measurement
Technologies Model 7700 NRM
Resistivity End of loop Thornton Model 200CR
Pressure Drop Filter housing vent portsSentra 0 – 10 psi P
sensor
UPW-Micro Conference November 2008 Slide 15
Test Results
UPW-Micro Conference November 2008 Slide 16
TOC Rinse-up
Time After Installation (hours)
0.1 1 10 100
Tot
al O
rgan
ic C
arbo
n a
dded
(pp
b)
0.01
0.1
1
10
100
1000
Increase due to increased TOC in incoming water.
Time After Installation (hours)
0 20 40 60 80 100
To
tal O
rga
nic
Car
bo
n (
ppb
)
0
2
4
6
8
10
Average incoming atend of test
Time After Installation (hours)
0.1 1 10 100
Tot
al O
rgan
ic C
arbo
n (
ppb)
0.1
1
10
Average incoming atend of test
UPW-Micro Conference November 2008 Slide 17
NVR Rinse-up
Time After Installation (hours)
0.01 0.1 1 10 100
Non
-vol
atile
res
idue
add
ed (
ppb)
0.01
0.1
1
10
Time (hours)
20 40 60 80 100
Non
-vo
latil
e re
sidu
e (p
pb)
0
1
2
3
4
5
6
7
Average incomingIncoming 3 sigma confidence limits
Time (hours)
0.01 0.1 1 10 100
Non
-vol
atile
re
sidu
e (
ppb)
0.1
1
10
Average incomingIncoming 3 sigma confidence limits
UPW-Micro Conference November 2008 Slide 18
Resistivity Rinse-up
Time After Installation (hours)
0.01 0.1 1 10 100
Res
istiv
ity d
ecr
ease
(M
-cm
)
0.01
0.1
1
10
Time After Installation (hours)
0 5 10 15 20
Res
istiv
ity (
M
-cm
)
16
17
18
19
Average Incoming
Time After Installation (hours)
0.01 0.1 1 10
Res
istiv
ity (
M
-cm
)
16
17
18
19
Incoming Average
UPW-Micro Conference November 2008 Slide 19
Particle rinse-up after filter installation – first 100 hours
Time After Installation (hours)
0.01 0.1 1 10 100C
um
ula
tive
Pa
rtic
le C
on
cen
tra
tion
(#
/mL
)0.001
0.01
0.1
1
10
100
1000
> 0.05 m> 0.10 m> 0.15m> 0.20 m
Particle conconcentration measured at end of loop
Time After Installation (hours)
0.01 0.1 1 10 100
Cu
mu
lativ
e P
artic
le C
on
cen
tra
tion
(#
/mL
)
0.001
0.01
0.1
1
10
100
1000
> 0.05 m> 0.10 m> 0.15 m> 0.20 m
Particle concentration measured at filter outlet
UPW-Micro Conference November 2008 Slide 20
Particle rinse-up after filter installation(10 – 480 hours)
Time After Installation (hours)
10 100
Cu
mu
lativ
e P
art
icle
Co
nce
ntr
atio
n (
#/m
L)
0.0001
0.001
0.01
0.1
1
10
> 0.05 m> 0.10 m> 0.15m> 0.20 m
Particle conconcentration measured at end of loop
Time After Installation (hours)
10 100
Cu
mu
lativ
e P
art
icle
Co
nce
ntr
atio
n (
#/m
L)
0.0001
0.001
0.01
0.1
1
10
> 0.05 m> 0.10 m> 0.15 m> 0.20 m
Particle concentration measured at filter outlet
Average particle concentration, 430 - 480 hours:• 0.057 per mL 50 nm • 0.015 per mL 100 nm
UPW-Micro Conference November 2008 Slide 21
Filter Rinse Measurements
Time required to achieve specified concentration added (hours) Contaminant
1 ppb 0.1 ppb NVR 0.3 3 TOC 0.7 20
Time required to achieve specified resistivity decrease (hours) Instrument
1.0 M-cm 0.1 M-cm Thornton CR200 < 0.08 0.4
Time required to achieve specified concentration (hours) Particle size
10/ml 1/ml 0.1/ml 0.05 µm 0.5 2.4 17 0.10 µm 0.2 1.2 5 0.15 µm < 0.2 0.6 2 0.20 µm < 0.2 0.3 1
Flushing times required to achieve NVR and TOC cleanliness levels
Flushing times required to achieve inorganic cleanliness levels
Flushing times required to achieve particulate cleanliness levels
UPW-Micro Conference November 2008 Slide 22
Performance Improvement – Particles
Channel Size (PMS UDI 50)
> 0.05 um >0.10 um > 0.15 um
Pa
rtic
le c
on
cen
tra
tion
(#
/lite
r)
0
500
1000
1500
2000
2500
Filter inlet concentrationEnd of loop prior to filter changeEnd of loop after filter change
Channel Size (PMS UDI 50)
> 0.05 um >0.10 um > 0.15 um
Pa
rtic
le c
on
cen
tra
tion
(#
/lite
r)1
10
100
1000
10000
Filter inlet concentrationEnd of loop prior to filter changeEnd of loop after filter change
UPW-Micro Conference November 2008 Slide 23
Performance Improvement – Pressure Loss
Pre
ssu
re D
rop
Acr
oss
Fitl
er
(psi
d)
0
2
4
6
8
10
Pressure drop acrossprior filter @ 4.5 gpmPressure drop across Gore20 nm high-flow filter @ 4.5 gpm
90.2% pressure drop reduction
UPW-Micro Conference November 2008 Slide 24
Particle levels 6 months after installation(exiting the filter)
Time (hours)
0 20 40 60 80 100
Cu
mu
lativ
e C
on
cen
trat
ion
(#/
mL
)
0.001
0.01
0.1
1
> 50 nm (30 minute ave.)> 100 nm (30 minute ave.)> 50 nm (4 hour ave.)> 100 nm (4 hour ave.)
Particle concentration - 100 hour average :• 0.041 per mL 50 nm • 0.013 per mL 100 nm
UPW-Micro Conference November 2008 Slide 25
Filter Case Study Summary (1)
• A 0.05 m filter was replaced with a 20 nm expanded hydrophilic PTFE filter in this case study.
• Particle concentrations 50 nm and 100 nm at the end of the supply loop were reduced 62% and 55% respectively when measured 100 hours after filter installation.
• Pressure drop across the filter was reduced by over 90%.
• Non-volatile residue recovered to 1 ppb added within 20 minutes of rinsing.
UPW-Micro Conference November 2008 Slide 26
Filter Case Study Summary (2)
• TOC recovered to 1 ppb added within 45 minutes of rinsing.
• Resistivity recovered to 0.1 M-cm with 5 minutes of rinsing.
• Particle concentrations out of the filter 50 nm and 100 nm achieved one count/mL within 150 and 75 minutes of rinsing respectively.
• Particle concentrations out of the filter measured 6 months after filter installation were slightly lower than the concentrations measured at 480 hours.