Post on 08-Sep-2020
Slide 1Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
A comparison of optical particle counting and
aerosol-based particle counting technologies for
UPW monitoring and diagnostics.
Gary Van Schooneveld1, Siqin He2, Pat Keady3
1CT Associates, Inc., 7121 Shady Oak Road, Eden Prairie, MN 55344
2Kanomax FMT, 4104 Hoffman Road, White Bear Lake, MN 55110
3Aerosol Devices Inc., 2614 S. Timberline Road, Fort Collins, CO 80525
CTAssociatesinc.com
Slide 2Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Introduction
• Liquid optical particle counting (OPC) utilizing light-scattering has been and
continues to be a key technology used by the semiconductor industry to count
particles in ultrapure water (UPW).
• Demand for detecting particles smaller than the current capabilities of these
instruments (<< 20 nm) has resulted in development and introduction of
instruments that utilize alternate detection techniques such as acoustic
emission1, laser induced breakdown detection2 and nebulization/aerosol
particle counting3.
• Each of these techniques deploy technologies that detect particles, and
potentially other forms of contamination, that differ from the OPC.
• Correlating the data generated by the new technologies to the historical data
base available from OPC’s is important for these new technologies to gain
acceptance and to understand what new and potentially insightful information
may be available using these techniques.
1. Madanshetty, Sameer, Particle profiling of UPW and suspensions, Ultrapure Water Micro 2016, Austin, TX.
2. Boj, Sylvain, et al, “Has the LIBD technique have potential for online Nano-particle detection in UPW?, Ultrapure Water Micro 2015, Portland, Oregon.
3. Blackford, David, et al, Introducing a non-optical 10 nm particle counter for ultrapure water, Ultrapure Water Micro 2014, Phoenix, AZ.
Slide 3Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Outline
• Instrumentation overview and capabilities
• Test plan
• Water system description and sampling locations
• Online instrumentation results
• Off-line analysis (SEM/EDS) results
• Key observations and recommendations
Slide 4Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Instrumentation
Lighthouse Worldwide
Solutions NC30+ OPC
Kanomax FMT
NanoParticle Nebulizer Model 9110
Aerosol Devices Model SSS110
Sequential Spot Sampler
Kanomax FMT
Liquid Nanoparticle Sizer (LNS)
Slide 5Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Theory of Operation and Capabilities -
Optical Particle Counting (OPC)
Courtesy of Noria Communications
Lighthouse Worldwide
Solutions NC30+
Sizing Channels: 30, 50, 80, 100 nm
Source: Van Schooneveld, et al., UPW Micro 2013
OPC response to mono-dispersed PSL
Slide 6Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Differential Mobility Analyzer (DMA)
Condensation ParticleCounter (CPC)Precision Nebulizer
Theory of Operation and Capabilities -
Liquid Nanoparticle Sizing (LNS)
CDA
PrecisionNebulizer
Scanning Mobility Particle Sizer (SMPS)ParticleAerosol
ChargeConditioner DMA CPC
monodispersed
aerosolIncoming sample
Slide 7Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Theory of Operation and Capabilities -
Liquid Nanoparticle Sizing (LNS)
20-125 nm PSL 8E4/mL > 30 nm
Particle Diameter (nm)
20 30 40 50 60 70 80 90 100 150 200 300
Cum
ula
tive
Co
nce
ntr
atio
n (
#/m
L)
100
101
102
103
104
105
106
LNS, diluted
NC30+
M50e
Excellent correlation observed between
LNS and OPC data using PSL.
Source: Van Schooneveld, et al., UPW Micro 2013
Slide 8Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Theory of Operation and Capabilities -
Focused Aerosol Deposition (FAD)
Kanomax FMT NanoParticleNebulizer Model 9110
Aerosol Devices Model SSS110Sequential Spot Sampler
→
CDA
UltrafineNebulizer
ParticleAerosol
Sequential Aerosol Spot Sampler
UPW
Slide 9Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Test Plan
• Measure selected points on CTA’s UPW system after
major cleaning, new component install and installation of
new final resin.
• Measure selected points for 12-24 hours before moving to
new location.*
• Eliminate first two hours of data from data analysis.
• Analyze focused aerosol deposition samples via
SEM/EDS.
* In subsequent testing, instrumentation collected data for several days at each sample point.
Slide 10Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
UPW System Sample Points
1
2
3
4
5
Operating conditions:
• 20 – 24 LPM
• 4 Bar
Ultra-HighPurityTank
185 nm UV Light
IX MixedBed (50 liter)
NRMMonitor
TOCMonitor
F4
P9 P10
P11
P12
T3
R3 PT2
ParticleCounter
High PurityWater System
20" - 20 nm cartridge filter
UF
20" - 20 nm cartridge filter
Slide 11Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Relevant Dates and Instruments
• January 26-27, 2017
– Sanitized system with Minncare® cold sanitizer.
– Installed UF Module
– Installed 2-20” filters
– Replace final polish resin.
• February 17-19, 2017
– CTA LNS#1
– Lighthouse NC30+
– Tandum KFMT Nanoparticle Nebulizer with AD Spot Sampler.
• April 5 – May 4, 2017
– CTA LNS#1
– Tandum KFMT Nanoparticle Nebulizer with AD Spot Sampler.
Slide 12Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Test Results
Slide 13Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Lighthouse NC30+
Date
2/18/2017 2/19/2017 2/20/2017
Cum
ula
tive
Co
nce
ntr
atio
n (
#/m
L)
0.1
1
10
100
1000
10000
> 30 nm
> 50 nm
> 80 nm
> 100 nm
Out of final filter Out of UF Out of IX Out of TOC
LampOut of pump
Liquid Nanoparticle Sizing System
Date
2/18/2017 2/19/2017 2/20/2017
Cum
ula
tive C
oncentr
ation (
> 5
nm
)
1e+6
1e+7
1e+8
1e+9
1e+10
Out of final filter Out of UF Out of IX
Out of TOCLamp
Out of pump
(lost air supply)
Test Results – LNS vs OPC
Observations:
1. Highest LNS and OPC concentrations are out of the TOC lamp.
2. Lowest OPC concentration is out of the UF/MF.
3. Lowest LNS concentration is out of the ion exchange resin
Slide 14Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Liquid Nanoparticle Sizing System
Date
2/18/2017 2/19/2017 2/20/2017
Cum
ula
tive
Co
nce
ntr
atio
n (>
5 n
m)
1e+6
1e+7
1e+8
1e+9
1e+10
Out of final filter Out of UF Out of IX
Out of TOC
Lamp
Out of pump
(lost air supply)
LNS Particle Size Distributions
Particle Diameter (nm)
5 6 7 8 9 10 12 15 20 25 30 40 50
Cum
ula
tive C
oncentr
ation (
#/m
L)
1e+5
1e+6
1e+7
1e+8
1e+9
Out of pump (-2.45)Out of TOC Lamp (-2.91)Out of IX resin (-2.44)Out of UF (-2.78)Out of final filter (-2.61)
Test Results – LNS Particle Size Distribution
Observations:
1. Increase in small particle size distribution out of the TOC reduction lamp. Could be
small particle formation/generation in the TOC lamp and/or increased level of
dissolved species (organic or silica).
2. Sharp drop in concentration after UF at 10 nm.
3. Lowest LNS concentration is after IX, not UF or MF
Slide 15Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Lighthouse NC30+
Date
Sat 18 Sun 19 Mon 20
Cum
ula
tive
Co
nce
ntr
atio
n (
#/m
L)
0.1
1
10
100
1000
10000
> 30 nm> 50 nm> 80 nm> 100 nm
Out of final filter Out of UF Out of IX Out of TOC
LampOut of pump
Ion Exchange Particle Retention (NC30+)
Channel (nm)
20 40 60 80 100 120
Pa
rtic
le R
ete
ntio
n (
%)
99.5
99.6
99.7
99.8
99.9
100.0
Lighthouse NC30+
Channel (nm)
20 30 40 50 60 80 100 150
Cu
mu
lative
Co
nce
ntr
atio
n (
#/m
L)
0.01
0.1
1
10
100
1000
10000
Out of pump (-1.79)Out of TOC lamp (-1.78)Out of IX resin (-2.96)Out of UF (-2.46)Out of final filter (-2.08)
Test Results – OPC Particle Size Distribution
Observations:
1. The ion exchange resin exhibited significant particle retention, >
99% of particles detected by OPC ≥ 30 nm.
2. Unusually flat slope (log-log < -2) out of pump and TOC lamp.
Possibly consequence of the sanitizing.
3. Flat slope out of UF/MF is also unusual. Would expect -3.5 to 4.
Possibly shedding from the UF and MF’s.
Slide 16Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Particle Size Distributions
Particle Diameter (nm)
5 10 20 30 40 50 60 80 100 120
Cum
ula
tive
Co
nce
ntr
atio
n (
#/m
L)
1e-1
1e+0
1e+1
1e+2
1e+3
1e+4
1e+5
1e+6
1e+7
1e+8
1e+9
Out of pump (LNS)Out of TOC lamp (LNS)Out of IX resin (LNS)Out of UF (LNS)Out of final filter (LNS)Out of pump (NC30+)Out of TOC lamp (NC30+)Out of IX resin (NC30+)Out of UF (NC30+)Out of final filter (NC30+)
Test Results – LNS vs OPC
Observations:
1. Sizing order different between two
techniques out IX resin. Measuring
different particles?
2. Large drop (3 orders) in concentration
after IX observed with OPC but not
observed by LNS. Why??
3. Concentration measured by LNS are 3 to 6
orders of magnitude higher than OPC.
Why??
Particle Size Distributions
Particle Diameter (nm)
30 40 50
Cum
ula
tive
Co
nce
ntr
atio
n (
#/m
L)
1e+5
1e+6
1e+7
Out of pump (LNS)Out of TOC lamp (LNS)Out of IX resin (LNS)Out of UF (LNS)Out of final filter (LNS)
Slide 17Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
PSD change with run-time (6 weeks)
LNS Particle Size Distributions(February 17 - 19, 2017)
Particle Diameter (nm)
5 6 7 8 9 10 12 15 20 25 30 40 50
Cu
mu
lative
Co
nce
ntr
atio
n (
#/m
L)
1e+5
1e+6
1e+7
1e+8
1e+9
Out of pump (-2.45)Out of TOC Lamp (-2.91)Out of IX resin (-2.44)Out of UF (-2.78)Out of final filter (-2.61)
LNS Particle Size Distributions(April 5, 2017 to May 4, 2017)
Particle Diameter (nm)
5 6 7 8 9 10 12 15 20 25 30 40 50
Cum
ula
tive C
oncentr
ation (
#/m
L)
1e+5
1e+6
1e+7
1e+8
1e+9
Out of PumpOut of TOC lampOut of IX resinOut of UFOut of final filter
Observations:
1. Little change in PSD prior to IX (after pump and TOC lamp).
2. Cleanup observed in IX, UF and final filter. Small particle (< 20 nm)
concentration are similar post IX.
3. Trend in large particles (> 20 nm) are consistent with prior OPC data.
Clean up of UF and
final filter
Slide 18Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Focused Aerosol Deposition
SEM/EDS Analysis
Slide 19Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Spot Sampler SEM/EDS Analysis
Collection Location: Out of IX resin
Collection Time: 41 hrs
Collection Date: 4/7/2017
1mm
Slide 20Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Spot Sampler SEM/EDS Analysis
Slide 21Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
10 - 50nm silica
1000nm organic particles
Spot Sampler SEM/EDS Analysis
Elements Detected:
• Carbon
• Oxygen
• Silicon
• Sulphur
• Zinc
• Magnesium
Slide 22Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Spot Sampler SEM/EDS Analysis
Slide 23Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Spot Sampler SEM/EDS Analysis
Primarily organic
with silica inter-dispersed
Elements Detected:
• Carbon
• Oxygen
• Sulphur
• Sodium
• Magnesium
• Silicon
Slide 24Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Estimated Spot Size – OPC vs LNS
Lighthouse NC30+
Date
Sat 18 Sun 19 Mon 20
Cum
ula
tive
Co
nce
ntr
atio
n (
#/m
L)
0.1
1
10
100
1000
10000
> 30 nm> 50 nm> 80 nm> 100 nm
Out of final filter Out of UF Out of IX Out of TOC
LampOut of pump
LNS Particle Size Distributions(April 5, 2017 to May 4, 2017)
Particle Diameter (nm)
5 6 7 8 9 10 12 15 20 25 30 40
Cu
mu
lative
Co
nce
ntr
atio
n (
#/m
L)
1e+5
1e+6
1e+7
1e+8
1e+9
Out of IX resin
Approach:• Integrate differential size data.
• Only consider particles > 7 nm.
• Extrapolate OPC PSD to 7 nm using power
law: 𝑓 𝑥 = 𝐾 ∗ (1/dn) where n=3.
• Assume that the OPC measurements from
February are still valid.
• Assume 1% packing efficiency.
• Assume 2D packing only.
Slide 25Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Lighthouse NC30+
Date
Sat 18 Sun 19 Mon 20
Cum
ula
tive
Co
nce
ntr
atio
n (
#/m
L)
0.1
1
10
100
1000
10000
> 30 nm> 50 nm> 80 nm> 100 nm
Out of final filter Out of UF Out of IX Out of TOC
LampOut of pump
LNS Particle Size Distributions(April 5, 2017 to May 4, 2017)
Particle Diameter (nm)
5 6 7 8 9 10 12 15 20 25 30 40
Cu
mu
lative
Co
nce
ntr
atio
n (
#/m
L)
1e+5
1e+6
1e+7
1e+8
1e+9
Out of IX resin
Projected spot diameter based
on integrated OPC data – 0.004 mm
Estimated Spot Size – OPC vs LNSApproach:
• Integrate differential size data.
• Only consider particles > 7 nm.
• Extrapolate OPC PSD to 7 nm using power
law: 𝑓 𝑥 = 𝐾 ∗ (1/dn) where n=3.
• Assume that the OPC measurements from
February are still valid.
• Assume 1% packing efficiency.
• Assume 2D packing only.
Slide 26Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Lighthouse NC30+
Date
Sat 18 Sun 19 Mon 20
Cum
ula
tive
Co
nce
ntr
atio
n (
#/m
L)
0.1
1
10
100
1000
10000
> 30 nm> 50 nm> 80 nm> 100 nm
Out of final filter Out of UF Out of IX Out of TOC
LampOut of pump
LNS Particle Size Distributions(April 5, 2017 to May 4, 2017)
Particle Diameter (nm)
5 6 7 8 9 10 12 15 20 25 30 40
Cu
mu
lative
Co
nce
ntr
atio
n (
#/m
L)
1e+5
1e+6
1e+7
1e+8
1e+9
Out of IX resin
Projected spot diameter based
on LNS data – 0.63 mm
Projected spot diameter based
on integrated OPC data – 0.004 mm
Estimated Spot Size – OPC vs LNSApproach:
• Integrate differential size data.
• Only consider particles > 7 nm.
• Extrapolate OPC PSD to 7 nm using power
law: 𝑓 𝑥 = 𝐾 ∗ (1/dn) where n=3.
• Assume that the OPC measurements from
February are still valid.
• Assume 1% packing efficiency.
• Assume 2D packing only.
Slide 27Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Lighthouse NC30+
Date
Sat 18 Sun 19 Mon 20
Cum
ula
tive
Co
nce
ntr
atio
n (
#/m
L)
0.1
1
10
100
1000
10000
> 30 nm> 50 nm> 80 nm> 100 nm
Out of final filter Out of UF Out of IX Out of TOC
LampOut of pump
LNS Particle Size Distributions(April 5, 2017 to May 4, 2017)
Particle Diameter (nm)
5 6 7 8 9 10 12 15 20 25 30 40
Cu
mu
lative
Co
nce
ntr
atio
n (
#/m
L)
1e+5
1e+6
1e+7
1e+8
1e+9
Out of IX resin
Projected spot diameter based
on LNS data – 0.63 mm
Projected spot diameter based
on integrated OPC data – 0.004 mm
Estimated Spot Size – OPC vs LNS
Focused Aerosol Deposition SEM results
seem to correlate better with LNS data than
OPC data in this particular study.
Additional work will be required to validate
this observation in other locations within the
UPW system.
Slide 28Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Key Observations
• While particle concentrations varying significantly between the LNS and OPC,
trends were consistent except out of the IX resin.
• Focused Aerosol Deposition with SEM/EDS appear to support the higher
concentrations measured by the LNS.
• The vast majority of the material deposited by the AD Spot Sampler were
organics and silica. Some organics materials are more difficult to detect by
light scattering due to their refractive index being close to water. Same is true
for silica. This may be one of the reasons for the differences observed
between the instruments.
• The TOC reduction lamp was a significant contributor to sub-20 nm
contamination. It is uncertain if these are particles, dissolved material or both.
Further analysis using Focused Aerosol Deposition may help to determine the
nature of these particles.
• The mixed-bed IX resin used in this test has significant particle removal
capability, especially greater than 30 nm, except for silica.
CTAssociatesinc.com
Slide 29Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Recommendations
• Continue developing our understanding of the differences
between aerosol-based and light-scattering particle
measurement techniques:
– Conduct parallel testing with aerosol-based and light scattering
instruments.
– Include alternate technology instruments as they become available.
– Utilize new tools such as Focused Aerosol Deposition to collect
and analyze the nanoparticles found in modern UPW systems.
– Work to establish a quantitative correlation between FAD, aerosol-
based and OPC results.
– Continue controlled testing to measure the response of the
instruments to nanoparticles of varied compositions.
Slide 30Van Schooneveld, et al., Ultrapure Water Micro 2017 – Portland, Oregon
Acknowledgements
• University of Minnesota’s Materials Charactization Lab
for the use of the Hitachi SU 8230 FE/SEM and Thermo
Noran System 7 Spectral Imaging (EDS) instruments.
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