Advances in LPC Monitoring in CMP Slurries

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Advances in LPC* Monitoring

in CMP Slurries
Statistics are a Bear

Mark Bumiller
Particle Sizing Systems

(*LPC = Large Particle Counts, typically > 1 µm)


LPC vs. Defects/Scratches (Yield)*

• Slurries differing in LPC


by a minimum
of 1.8×105particles/g
slurry had statistically
different predicted scratch
events at the 95%
confidence level.
• LPC from PSS AccuSizer
780
– LE400 (extinction) sensor

*Remsen, E. et al., Analysis of Large Particle Count in Fumed Silica Slurries and Its Correlation with 
Scratch Defects Generated by CMP, Journal of The Electrochemical Society, 153 (5) G453‐G461(2006)
LPC Correlates to Yield
*

**

* R. Nagahara et al, VMIC‐MIC, 1996

**from Y.‐J.Seo et al., Effects of slurry filter size on the chemical mechanical 
Polishing (CMP) defect density, Materials Letters, 58(2004) 2091‐2095
The Wish
• Please give me an ideal LPC monitor:
• Inexpensive • Yield ROI?
• Point of Use? • Yes, LPCs generated
• No Dilution? • Coincidence (statistics)
• Finds LPC’s • Statistics matter
CMP Filtration Monitoring
• Incoming slurry supply line
Supply Line; Particles/ml greater or equal to 1.01 um
• At point of use
• Change filters based on 24 hr

particle count, not just on


expected life time = better
yield, lower cost
tote              mixer           day tank     
manifold
filter

POU filter POU filter

AccuSizer Mini AccuSizer Mini

polishing tools
Effect of Pumping (Shear Stress)

Increased circulation

S/C = scratches
Effect of Pumping (Sedimentation)

• Top vs. bottom of 
tank
• Supply line LPC > 
1.01 µm
• Online FX results

New tote

• From day tank
Effect of Slurry Pumping (in the Tool)

• Real time monitoring


of LPC counts
downstream of a
peristaltic pump
provides feedback on
pump performance
and generated LPCs.

Monitoring LPC Counts of Silica Slurry in a Loop


No Dilution? Avoid Coincidence Errors
• Must avoid coincidence error for best data
• Only one particle in measurement zone
• Collimated beam: 0.5 - 400 µm 60 ml/min
• 10,000 particles/mL
Advancement: Focused Beam
• Focused beam
• ~106 particles/mL
• 103 improvement
• FX: 0.7- 20 µm
• FX Nano .15 – 10 µm
• But dilution may still
be required to avoid
coincidence
Check for Coincidence Error
• Measure at several different concentrations (dilutions)
• Should have linear response @ size of interest

Error @ 1 µm

No error @ 5 µm
Advancements in Autodilution
Internal Fluidics
2013                              2016
Dilution Fluidics:
HEADING2 Stage Dilution
Variable sample loop volume
= VL= 1, 3, or 5 mL

Volume = V1= 30 mL

Goodbye coincidence errors


Tailor Measurement to Slurry

Plus many controls fixed in firmware


Parameters saved for each slurry
Distribution Statistics: Standard Error
SE=s/(√n) where
s = standard deviation
n= number of particles counted

So n = s2/SE2

If the sample has a standard deviation of 2 and we


can live with a 2% standard error, then the number
of particles, n, that needs to be measured is:

n = 22/ (0.02)2 = 10,000


ISO 13322-1 Approach*

n* with admissible error of 5% as a function of the geometric standard deviation


GSD of the sample. Here, the probability, P, is taken as P = 0.95

*ISO 13322-1, Particle Size Analysis—Image Analysis Methods—Part 1: Static Image Analysis Methods, available at www.iso.org
H. MASUDA & K. GOTOH, Study on the sample size required for the estimation of mean particle diameter,
Advanced Powder Technol., 10(2), 1999, pp. 159-173
Experimental Confirmation

# Sized D10 (µm) D50 (µm) D90 (µm)


442 8.5 13.82 21.65 D90
D50
2579 8.3 13.82 20.99 D10
5213 8.73 13.82 21.71
11364 9.47 15.39 25.63
13196 10 16.24 25.02
16748 17.41 24.07 44.11
37688 17.14 29.42 50.45

NEED to count tens of thousands,


preferably hundreds of thousands of
particles to achieve statistical accuracy
at tails of the distribution (LPC)
?
LPC Sensitivity

• Spike silica slurry w/1 µm


PSL standard
• Dilute slurry A 200:1
• Add 1.44 mL diluted PSL
stock at 1.74 × 107/mL
• Measure on AccuSizer FX
Point of Use system
• Note increase of ~100,000
particles/mL @ expected
size = excellent recovery
Ceria CMP Slurry
• Spike ceria A slurry
w/ 106/mL 1 µm PSL

• Mix Slurry A & B

99% Ceria A + 1%
Ceria B

99% Ceria A + 1%
Ceria B

90% Ceria A +
10% Ceria B
Conclusions
• It’s worth the investment: increased yields
• Point of Use monitors detect LPCs where
they cause troubles
• Need autodilution, tailored to the slurry
• Need to measure 104 particles to always
find LPCs
• Can’t beat statistics
– Sorry, you won’t win this jackpot
Booth 1100
[email protected]

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