Particle Characterization of Abrasives
Mark Bumiller
mark.bumiller@horiba.com

© 2010 HORIBA, Ltd. All rights reserved.
Factors Affecting Abrasion Mechanics
 Difference in hardness between the two
substances: a much harder abrasive will cut
...
Factors Affecting Abrasion Mechanics
 Contact force: more force causes faster abrasion
 Loading: worn abrasive & cast of...
Macro vs. Microgrits
Macrogrits:
Greater than ~ 60 µm
Traditional size test is
sieving

Microgrits:
Less than ~ 60 µm...
Macrogrits

© 2010 HORIBA, Ltd. All rights reserved.
Microgrits

© 2010 HORIBA, Ltd. All rights reserved.
ISO 6344
Macrogrits P12 to P220

© 2010 HORIBA, Ltd. All rights reserved.
Sieve Analysis
Inexpensive
Time consuming
Alternative: Dynamic
Image Analysis by
CAMSIZER
Higher throughput
Complete ...
Dynamic Image Analysis
By choosing proper size parameter,
Xc min, results can match historic sieve
Data. Also generates sh...
Sand: Round vs. “Edgy” by CAMSIZER

Sphericity

Similar in size.
Shape difference seen
in b/l and sphericity.
Edgy would m...
ISO 6344
Microgrits P240 to P1200

© 2010 HORIBA, Ltd. All rights reserved.
ISO 6344
Microgrits P1500 to P2500

© 2010 HORIBA, Ltd. All rights reserved.
Sedimentometer
 Sample is pre-wet, then placed in
settling medium at top of tube, time is
recorded
 Time is recorded whe...
Laser Diffraction
 Powders (in air) and
suspensions
 30 nm – 3000 µm
 Quick, easy,
reproducible
 Highly automated
 Mo...
Laser Diffraction Data
Diamond Abrasives
Silicon Carbide

slurry

© 2010 HORIBA, Ltd. All rights reserved.
Chemical Mechanical Polishing (CMP)
 Smooth (planarize) silicon wafer
surface with combination of
chemical & mechanical f...
Particle Sizing Techniques
Technique

Nano-Particle
Measurement

Oversize
Measurement

Analysis Speed

Dilution Required?
...
Laser Diffraction Data
Ludox colloidal slurry (31 nm)
Geltech silica (1.65 µm)
0.05 wt % Geltech in Ludox

© 2010 HORIBA, ...
Acoustics: DT-1201 Experiment
Attenuation [dB/cm/MHz]

I in
10

log
f [ MHz ]L[cm]
I out
9

Attenuation [dB/cm/MHz]

8
7...
Acoustics: DT-1201 Experiment
 Materials: Ludox colloidal silica, Geltech silica,
commercially available CMP slurries
 S...
Acoustics: DT-1201 Experiment

Attenuation spectra for single
component silica slurries

© 2010 HORIBA, Ltd. All rights re...
Acoustics: DT-1201 Experiment

Particle size distributions of silica Cabot SS25,
diluted down to 12 wt %, with various add...
Image Analysis Experiment
 Samples: small, medium,
large abrasive particles
 Measure size & shape using
static image ana...
Image Analysis Experiment
Small abrasive, high angularity (left),
low angularity (right)

Medium abrasive, high angularity...
Shape Parameters

© 2010 HORIBA, Ltd. All rights reserved.
Spike Parameter*

* Stachowiak, W., Image Analysis of Abrasive Grits, Tribology and Interface Engineering, Vol 44

© 2010 ...
PSA300 Calculation
Find sharp edges at the tips of the particles
Count number of tips (child count)
Number of tips alon...
PSA300 Calculation

© 2010 HORIBA, Ltd. All rights reserved.
PSA300 Calculation

© 2010 HORIBA, Ltd. All rights reserved.
PSA300 Calculation

© 2010 HORIBA, Ltd. All rights reserved.
Image Analysis Results

© 2010 HORIBA, Ltd. All rights reserved.
Conclusions
For particle size analysis
Laser diffraction offers many benefits over
sedimentometer
CAMSIZER offers many ...
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Particle Characterization of Abrasives

  1. 1. Particle Characterization of Abrasives Mark Bumiller mark.bumiller@horiba.com © 2010 HORIBA, Ltd. All rights reserved.
  2. 2. Factors Affecting Abrasion Mechanics  Difference in hardness between the two substances: a much harder abrasive will cut faster and deeper  Grain size (grit size): larger grains will cut faster as they also cut deeper  Grain shape: sharp corners help  Adhesion between grains, between grains and backing, between grains and matrix: determines how quickly grains are lost from the abrasive and how soon fresh grains, if present, are exposed © 2010 HORIBA, Ltd. All rights reserved.
  3. 3. Factors Affecting Abrasion Mechanics  Contact force: more force causes faster abrasion  Loading: worn abrasive & cast off work material fill spaces between abrasive grains, reducing cutting efficiency while increasing friction  Use of lubricant/coolant/metalworking fluid: Can carry away swarf (preventing loading), transport heat (may affect physical properties of the workpiece or the abrasive), decrease friction (with the substrate or matrix), suspend worn work material and abrasives allowing for a finer finish, conduct stress to the workpiece. © 2010 HORIBA, Ltd. All rights reserved.
  4. 4. Macro vs. Microgrits Macrogrits: Greater than ~ 60 µm Traditional size test is sieving Microgrits: Less than ~ 60 µm Traditional testing is sedimentometer © 2010 HORIBA, Ltd. All rights reserved. 2 mm 40 µm
  5. 5. Macrogrits © 2010 HORIBA, Ltd. All rights reserved.
  6. 6. Microgrits © 2010 HORIBA, Ltd. All rights reserved.
  7. 7. ISO 6344 Macrogrits P12 to P220 © 2010 HORIBA, Ltd. All rights reserved.
  8. 8. Sieve Analysis Inexpensive Time consuming Alternative: Dynamic Image Analysis by CAMSIZER Higher throughput Complete distribution Shape information Particle images Size and shape from 30 µm – 30 mm © 2010 HORIBA, Ltd. All rights reserved.
  9. 9. Dynamic Image Analysis By choosing proper size parameter, Xc min, results can match historic sieve Data. Also generates shape data proven To correlate with abrasive performance. © 2010 HORIBA, Ltd. All rights reserved.
  10. 10. Sand: Round vs. “Edgy” by CAMSIZER Sphericity Similar in size. Shape difference seen in b/l and sphericity. Edgy would make better abrasive. Breadth/length (b/l) © 2010 HORIBA, Ltd. All rights reserved.
  11. 11. ISO 6344 Microgrits P240 to P1200 © 2010 HORIBA, Ltd. All rights reserved.
  12. 12. ISO 6344 Microgrits P1500 to P2500 © 2010 HORIBA, Ltd. All rights reserved.
  13. 13. Sedimentometer  Sample is pre-wet, then placed in settling medium at top of tube, time is recorded  Time is recorded when the first material reaches the collecting tube  Times are recorded as sample reaches various graduations in settling tube  Example: If the 2mm height was reached in 4 minutes, that means 8% of the material is 39.8 microns and coarser  Still in use, but being replaced by newer technology (laser diffraction) © 2010 HORIBA, Ltd. All rights reserved.
  14. 14. Laser Diffraction  Powders (in air) and suspensions  30 nm – 3000 µm  Quick, easy, reproducible  Highly automated  Most popular particle sizing technique  LA-950 highest performance available but workhorse dependability © 2010 HORIBA, Ltd. All rights reserved. Dry powder feeder
  15. 15. Laser Diffraction Data Diamond Abrasives Silicon Carbide slurry © 2010 HORIBA, Ltd. All rights reserved.
  16. 16. Chemical Mechanical Polishing (CMP)  Smooth (planarize) silicon wafer surface with combination of chemical & mechanical forces  Uses abrasive & corrosive colloidal slurry, polishing pad, and retainer ring  CMP slurry contains small abrasive particles  Large particles in slurry cause scratches (defects)  Want to know mean size + presence of larger particles © 2010 HORIBA, Ltd. All rights reserved.
  17. 17. Particle Sizing Techniques Technique Nano-Particle Measurement Oversize Measurement Analysis Speed Dilution Required? Laser Diffraction Very good Excellent Excellent Yes Dynamic Light Scattering Excellent Very poor Very good Yes Acoustic Spectroscopy Very good Excellent Good No Light Obscuration Very good Good Poor Yes Disc Centrifuge Very good Excellent Very poor Yes Microscopy (SEM, TEM) Excellent Very poor (statistics) Very poor No © 2010 HORIBA, Ltd. All rights reserved.
  18. 18. Laser Diffraction Data Ludox colloidal slurry (31 nm) Geltech silica (1.65 µm) 0.05 wt % Geltech in Ludox © 2010 HORIBA, Ltd. All rights reserved.
  19. 19. Acoustics: DT-1201 Experiment Attenuation [dB/cm/MHz] I in 10  log f [ MHz ]L[cm] I out 9 Attenuation [dB/cm/MHz] 8 7 6 5 4 3 2 diameter 1 micron diameter 0.5 micron 1 0 0 10 10 1 Frequency [MHz] © 2010 HORIBA, Ltd. All rights reserved. 10 2
  20. 20. Acoustics: DT-1201 Experiment  Materials: Ludox colloidal silica, Geltech silica, commercially available CMP slurries  Spike SS25 CMP slurry with Geltech silica  Note: all measurements made with no dilution, major benefit of acoustics © 2010 HORIBA, Ltd. All rights reserved.
  21. 21. Acoustics: DT-1201 Experiment Attenuation spectra for single component silica slurries © 2010 HORIBA, Ltd. All rights reserved. Corresponding particle size distributions
  22. 22. Acoustics: DT-1201 Experiment Particle size distributions of silica Cabot SS25, diluted down to 12 wt %, with various additions of silica Geltech 0.5 © 2010 HORIBA, Ltd. All rights reserved.
  23. 23. Image Analysis Experiment  Samples: small, medium, large abrasive particles  Measure size & shape using static image analysis (PSA300)  Prepare sample using Sampler Disperser  Calculate size, shape, custom calculation to define angularity © 2010 HORIBA, Ltd. All rights reserved.
  24. 24. Image Analysis Experiment Small abrasive, high angularity (left), low angularity (right) Medium abrasive, high angularity (left), low angularity (right) Large abrasive, high angularity (left), low angularity (right) © 2010 HORIBA, Ltd. All rights reserved.
  25. 25. Shape Parameters © 2010 HORIBA, Ltd. All rights reserved.
  26. 26. Spike Parameter* * Stachowiak, W., Image Analysis of Abrasive Grits, Tribology and Interface Engineering, Vol 44 © 2010 HORIBA, Ltd. All rights reserved.
  27. 27. PSA300 Calculation Find sharp edges at the tips of the particles Count number of tips (child count) Number of tips alone not sufficient, long particles w/2 tips not as good as hexagon w/6 tips Define angularity roundness as child count x roundness Thus triangle w/3 points less angular than octagon of 4 sharp edges & 4 rounded edges © 2010 HORIBA, Ltd. All rights reserved.
  28. 28. PSA300 Calculation © 2010 HORIBA, Ltd. All rights reserved.
  29. 29. PSA300 Calculation © 2010 HORIBA, Ltd. All rights reserved.
  30. 30. PSA300 Calculation © 2010 HORIBA, Ltd. All rights reserved.
  31. 31. Image Analysis Results © 2010 HORIBA, Ltd. All rights reserved.
  32. 32. Conclusions For particle size analysis Laser diffraction offers many benefits over sedimentometer CAMSIZER offers many advantages over sieves DT-1201 for undiluted size and zeta potential For particle size and shape CAMSIZER for 30 µm – 30 mm PSA300 for 0.5 µm – 2000 µm View at any time at: www.horiba.com/us/particle © 2010 HORIBA, Ltd. All rights reserved.

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