Edmund Seminar - Ultra Low Surface Roughness Polishing and Metrology

Ultra–Low Surface Roughness Polishing and
Metrology
Jayson Nelson and Shawn Iles
PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics®
Edmund Optics Company
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engineering
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• Over 20 years experience as
provider of custom fab and
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of Arizona
PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics® 2
What markets benefit from sub Angstrom surfaces?
Applications that require optical and energy efficiency

• Ultraviolet regime and below
• Ultra low scatter
• High power laser systems
• Metrology systems
Image from axisimagingnews.com

Image from AZO Materials Inc, shutterstock.com
Image from LLE.Rochester.edu
Images from Ultrafast Innovations GmbH

What markets benefit from sub Angstrom surfaces?
Applications that require optical and energy efficiency

• Ultraviolet regime and below
• Ultra low scatter
• High power laser systems
• Metrology systems
Medical
Image from BusinessKorea
• Eye surgery
• Imaging systems
Defense Image from WebMD Inc., 2003
Image from SPIE Paper 013402, Jan2012
• Navigation systems
Image from FoxTrotAlpha

Ultra–Low Surface Roughness
SPIE Paper 11175-05, 2019

doi: 10.1117/12.2536689 PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics® 5
Polishing Fundamentals
Traditional subtractive polishing begins

with generating the surface
• Fixed Abrasives (Blanchard, et al)
• Loose Abrasives
• Progressively finer grits
• SSD is a natural result of mechanical
material removal
Edge Grind Intermediate Final Small Tool
Shaping Grinding & Polish Polish Polish Polish
SPIE Paper 11175-05, 2019

Sub Surface Damage
Atomic level bonding is very strong
• Polishing particles have irregular shape
• Particle rips material from the substrate
Some substrate material remains bonded to
sheared material
• Irregular surface of glass fragments
• Particle pressure on glass causes fractures
Resulting surface voids created by material

removal beneath the shear plane
• Some visible, some latent (SSD)

Particle Analysis
Composition Ce O C Composition Ce O C Si
(at.%) 39.9 49.1 11 (at.%) 17.0 48.3 31.3 3.4
Sample from the top
Sample from the Bottom

Particle Analysis
✓ Silica is one of the main

components of glass and is
detected at the top of the slurry.
✓ Good suspension because of the Ceria
particle
small particle size and lower density
2.5g/cm3. 1 Hr Top 6 Hr Top
✓ Large ceria polishing powder easily

settled at the bottom owing to its
high density 7.2g/cm3.
✓ After run-in process for 4hrs, the
particle size somewhat reduced and
further decreased after 6hrs. Control Sample 1 Hr Bottom 6 Hr Bottom

“Insanity is doing the same thing over and over
and expecting different results”
SPIE Paper 11175-05, 2019

Polishing Science
Chemical Mechanical Polishing (CMP)
• Ceria, alumina, zirconia, and silica are common
polishing agents
• Water softens the glass by breaking Si-O bonds;
o SiO2 + 2(H2O) → Si(OH)4 Si
o Si-OH molecules form (Si(OH)4)

Si
Reality – aggressive removal below Beilby layer; SSD

Si
Si
*Ideally – material removal occurs when modified

Si(OH)4 layer is removed from the surface
SPIE Paper 11175-05, 2019

Polishing Science
Diffusion of H2O in SiO2
• Diffusion coefficient estimated around 10-
15 cm2/sec* (very low value)
• Measured value of diffusion depth 0.5nm ≤

d ≥12.0nm**
• Solubility of H2O in SiO2 increases
exponentially with increasing hydrostatic
pressure and compressive stress
• Diffusion coefficient decreases ↔ Therefore, control slurry density
exponentially (Lee Cook paper) and pressure on window
*”Diffusion of Water in SiO2 at Low Temperatures”, ** “Effect of Stress on Water Diffusion in Silica Glass”,
Lanford, Doremus, et al, “Advances in Materials Nogami & Tomozawa, J of Am Cer Society, 67, 1984,
Characterization II”, 1985, p203 p151
SPIE Paper 11175-05, 2019
Super Polish Fundamentals
Submersion Polishing*
• Constant input of fresh slurry
• Maintains hydrated lap at interface
• Consistent temperature
• Surface tension forms a barrier against
airborne contaminants
• Uninterrupted formation of Beilby layer
• Higher probability of particle mixing
* Essential to the creation of sub Angstrom surfaces

SPIE Paper 11175-05, 2019
Super Polish Process Comparison
Standard Process – WLI
• Particle rips through Beilby layer and
into substrate (0.5µm ≤ Ø ≥ 1.5µm)
• Evidence of scratches, trenches, and
surface structure
• 23 Å P-V, 3 Å Ra
EOT Process – WLI

• Repeated removal of Beilby layer
• Evidenced as random surface structure,
no scratches or trenches
• 3 Å P-V, 0.25 Å Ra
SPIE Paper 11175-05, 2019

Super Polish Process Comparison
Standard Super Polish – AFM
▪ Very good surface – 1.55 Å average
roughness
▪ 29.6 Å P-V
▪ Structure still evident
EOT Super Polish – AFM

▪ Excellent surface – 1.07 Å average
roughness
▪ 3.71 Å P-V
▪ Surface wiped clean
SPIE Paper 11175-05, 2019

Roughness Parameters
𝑓2
𝑅𝑀𝑆 = න 𝑃𝑆𝐷 𝑓 𝑑𝑓
𝑓1
• Requires spatial frequency

bandwidth (SFB) to be
fully defined
SPIE Paper 11175-19, 2019

Spatial Frequency Groups
Figure Waviness Roughness
0.02 – 13 [mm ]
-1 1 – 1800 [mm ]
-1 30 – 50,000 [mm ]
-1
SPIE Paper 11175-19, 2019

Targeting Surface Characteristics
Low spatial Mid-spatial High spatial

frequency frequency frequency
SPIE Paper 11175-19, 2019

Instrument Capabilities
PSD
4” Interferometer
White Light
Interferometer
Atomic Force
Microscope
5X, 20X, 100X
10-1 100 101 102 103 104 105

Figure Waviness Roughness
Spatial Frequency [mm-1] Graph: L. Deck, C. Evens, “High performance Fizeau and scanning white-light
interferometers for mid-spatial frequency optical testing of free-form optics” SPIE (2004)
SPIE Paper 11175-19, 2019

Data Correlation
AFM Image WLI Image
Shared Spatial Frequency

Bandwidth:
60 – 512 [cycle/mm]
SPIE Paper 11175-19, 2019
Instrument Transfer Function (ITF)
New View with different optical
configurations
ITF is similar to MTF

https://www.edmundoptics.com/resources/application-
notes/optics/introduction-to-modulation-transfer-function/
Graph: L. Deck, C. Evens, “High performance Fizeau and scanning white-light


Zygo New View (Theoretical Data)
5X
Instrument Transfer Functions
• Specific for each type of equipment
20X
• Similar concept to MTF and Rayleigh
Criterion
• Important to stay within system 100X
capabilities
4” interferometer
SPIE Paper 11175-19, 2019

Spatial Frequency Filtering
• Why filter what the instrument can’t see?
• Critical for sub-Angstrom

surface roughness
• Solid line = measured data

• Dashed line = theoretical data
Graph: L. Deck, C. Evens, “High performance Fizeau and scanning white-light


Data Filtering
Pixels Pixels
Upper Boundary
Information from
Zygo MX help files
FOV FOV
Lower Boundary
SPIE Paper 11175-19, 2019

Super Polish Metrology
Setting the upper boundary

• ITF charts are great, but not
always available
• 4 pixels per line pair provides
good separation and contrast Each pixel “sees” a line pair (left)
Image is shifted (right)
Each pixel sees either black or white (l)
Each pixel sees half black and half white(r)
“What is all the hype about

resolution and mega pixels”, 2009,
PCO AG Structure is fully resolved by the pixels(l)
Structure fully resolved, but w/less sharpness(r)
SPIE Paper 11175-19, 2019

Effects of data filtering
• Over filtering decreases
roughness value
• Under filtering includes
system error in data
SPIE Paper 11175-05, 2019

Environmental Errors
10X Data Averaging

• Removal of random, non-recurring
error
• P-V benefits when 10 ≤ n ≥ 20
• RMS benefits when 5 ≤ n ≥ 10
• Ra benefits when 5 ≤ n ≥ 10
PV System Error Removal PV System Error Removal PV System Error Removal
From 5 measurements From 10 measurements From 20 measurements
-2.5% -4.9% -10.8%
Ra System Error Removal Ra System Error Removal Ra System Error Removal
From 5 measurements From 10 measurements From 20 measurements
-7.7% -8.5% -7.1%
SPIE Paper 11175-05, 2019

System Errors
Error File
• Removes repeating system errors
o Scratches on objective
o Dust particles on system optics
• Typical system error file is around 0.5
Angstroms which is roughly equal to
surface being evaluated
SPIE Paper 11175-05, 2019

International Standards
ISO 10110-8 Surface Texture, Roughness

and Waviness
• Explains proper way to measure and
callout surface roughness
• Section 4.3.2 “Note that the RMS
description is incomplete without
indicating the spatial bandwidth limits.”
• Default bandwidth 12.5 to 400 cycles/mm
SPIE Paper 11175-19, 2019

Fused Silica Surfaces
Fused Silica Planar Polishing
Fused Silica Incoming Material
P-V (Å) RMS (Å) Ra (Å)
Average 183.416 7.423 5.701
Range 2089.920 18.240 11.190 • Sub Angstrom achieved in 2
Std Dev 186.88391 2.90696 1.81687
hours
• No measurable SSD
Fused Silica Final Results 2 Hr Polishing Time

P-V ( Å) RMS ( Å) Ra ( Å)
Average 7.862 0.448 0.333
Range 1.131 0.034 0.101
Std Dev 0.97763 0.02217 0.02024
SPIE Paper 11175-05, 2019

N-BK7 Surfaces
N-BK7 Planar Polishing
N-BK7 Incoming Material
P-V ( Å ) RMS (Å) Ra (Å)
Average 256.370 11.397 6.004
Range 538.988 17.017 1.989 • Sub Angstrom achieved in 2
Std Dev 205.748 7.484 0.671
hours
• Run alongside FS windows
• About 25% higher Ra than FS
• N-BK7 has SiO2, B2O3, Na2O,
N-BK7 Final Results 2 Hr Polishing Time
P-V ( Å) RMS ( Å) Ra ( Å)
Average
Range
15.887
3.392
1.095
0.065
0.839
0.047 Al2O3, other elements
Std Dev 1.70506 0.03253 0.02354
SPIE Paper 11175-05, 2019

Super Polishing - Silicon
• EO Part #68527
• Optical Grade Silicon Flats
• 25.0mm Ø, 3.0mm CT
• Continuous polisher, pitch
• Submerged process Final Results 2 Hr Polishing Time
P-V ( Å ) RMS ( Å ) Ra ( Å )
• 0.368 Å Ra Average 5.871 0.483 0.368
Range 4.435 0.093 0.074
• 5.871 Å P-V Std Dev 1.22176 0.02710 0.02125
New View, 20X Mirau, 1X Zoom, BPF, FFT Fixed,

9 - 250 mm-1, 10X Average, Sys Err Removed
Super Polishing – Calcium Fluoride
Incoming Material
AVERAGE
P-V ( Å)
163.835
RMS ( Å)
15.502
Ra ( Å)
11.729 • EO Part #47683
RANGE 734.679 15.537 10.326
STD DEV 227.9093 4.3495 3.1080 • Vacuum UV Grade CaF2
• 25.0mm Ø, 3.0mm CT
• Continuous polisher, pitch
Final Results 2 Hr Polishing Time • Submerged process
P-V ( Å ) RMS ( Å ) Ra ( Å )
Average
Range
18.274
19.657
0.964
0.213
0.713
0.121
• 0.713 Å Ra
Std Dev 5.99559 0.07277 0.04265
• 18.274 Å P-V
New View, 20X Mirau, 1X Zoom, BPF, FFT Fixed,

9 - 250 mm-1, 10X Average, Sys Err Removed
CaF2 Before Polishing

CaF2 After Polishing

Summary
• Super Polishing is highly dependent on

slurry chemistry
• Chemistry is influenced mainly by
glass type and polishing compound
• Proper metrology is very important
when comparing results
• Near perfect surfaces that are wiped
clean of measurable SSD can be
achieved with process control
• Fused silica, NBK-7, Si, CaF2 all
demonstrated to sub Angstrom levels

Related Publications
• “Aggregation and Flow of Solids”, Sir G.T.Beilby, 1921
• “Chemical Processes in Glass Polishing”, Lee M. Cook, Journal of Non-Crystalline Solids, 120, 152
(1990)
• “Chemical Mechanical Polishing”, Mel Bartels, March 2001
• “Dissection of Preston Material Removal Rate Equation”, LLNL, Nov2014
• “Sub-surface Mechanical Damage Distributions during Grinding of Fused Silica”, LLNL, Aug2006
• “A Comparative Study on the Roles of Velocity in the Material Removal Rate during Chemical
Mechanical Polishing”, Wei-Tsu Tseng et al, Journal of Electrochemical Society, 146, 1952-1959,
1999
• “Slurry Particle Size Evolution during the Polishing of Optical Glass”, M.Cumbo, LLE Review,
Volume 61, 1995
• “Metal Oxide Chemistry and Synthesis”, Wiley & Sons Ltd., 2000, ISBN 0-471-97056-5 (English
translation of the original French text “De la Solution a l’Oxyde”, 1994)
SPIE Paper 11175-05, 2019

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Ultra–Low Surface Roughness Polishing and

Global manufacturing and

Applications that require optical and energy efficiency

Image from axisimagingnews.com

Image from LLE.Rochester.edu

Images from Ultrafast Innovations GmbH

PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics® 3

Applications that require optical and energy efficiency

PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics® 4

SPIE Paper 11175-05, 2019

Traditional subtractive polishing begins

SPIE Paper 11175-05, 2019

Resulting surface voids created by material

PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics® 7

Sample from the top

Sample from the Bottom

PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics® 8

✓ Silica is one of the main

✓ Large ceria polishing powder easily

PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics® 9

SPIE Paper 11175-05, 2019

o Si-OH molecules form (Si(OH)4)

Reality – aggressive removal below Beilby layer; SSD

*Ideally – material removal occurs when modified

SPIE Paper 11175-05, 2019

• Measured value of diffusion depth 0.5nm ≤

* Essential to the creation of sub Angstrom surfaces

EOT Process – WLI

SPIE Paper 11175-05, 2019

EOT Super Polish – AFM

SPIE Paper 11175-05, 2019

• Requires spatial frequency

SPIE Paper 11175-19, 2019

Figure Waviness Roughness

SPIE Paper 11175-19, 2019

Low spatial Mid-spatial High spatial

SPIE Paper 11175-19, 2019

5X, 20X, 100X

10-1 100 101 102 103 104 105

SPIE Paper 11175-19, 2019

Shared Spatial Frequency

ITF is similar to MTF

Graph: L. Deck, C. Evens, “High performance Fizeau and scanning white-light

PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics® 21

SPIE Paper 11175-19, 2019

• Critical for sub-Angstrom

• Solid line = measured data

Graph: L. Deck, C. Evens, “High performance Fizeau and scanning white-light

PROPRIETARY Information | www.edmundoptics.com | © Copyright Edmund Optics® 23

SPIE Paper 11175-19, 2019

Setting the upper boundary

“What is all the hype about

SPIE Paper 11175-19, 2019

SPIE Paper 11175-05, 2019

10X Data Averaging

SPIE Paper 11175-05, 2019

SPIE Paper 11175-05, 2019

ISO 10110-8 Surface Texture, Roughness

SPIE Paper 11175-19, 2019

Fused Silica Final Results 2 Hr Polishing Time

SPIE Paper 11175-05, 2019

SPIE Paper 11175-05, 2019

New View, 20X Mirau, 1X Zoom, BPF, FFT Fixed,