Ee w08.1 m_ 3. renewables and the electricity industry (climate change)
About Analyzing Abrasives - Horiba 1. 0 2. 0 3. 0 4. 0 5. 0 6. 0 7. 0 8. 0 9. 0 l/b 10 20 30 40 50...
Transcript of About Analyzing Abrasives - Horiba 1. 0 2. 0 3. 0 4. 0 5. 0 6. 0 7. 0 8. 0 9. 0 l/b 10 20 30 40 50...
© 2015 HORIBA, Ltd. All rights reserved.
About Analyzing Abrasives
Jeffrey Bodycomb, Ph.D.
HORIBA Scientific
www.horiba.com/us/particle
© 2015 HORIBA, Ltd. All rights reserved.
Mechanics of abrasion
Abrasion is the interaction of a rock (the abrasive
particle) and a hard place (the work piece). Either
the abrasive gives or the work piece gives. Ideally
it is the latter.
© 2015 HORIBA, Ltd. All rights reserved.
Factors affecting abrasion
Contact force: more force causes faster abrasion
Loading: worn abrasive and cast off work material fills spaces between grains, reducing cutting efficiency while increasing friction
Use of lubricant/coolant/metal working fluid: can carry away swarf (preventing loading), transport heat (in some cases), decrease friction (with the substrate or matrix), suspend worn work material and abrasives to allow a finer finish.
© 2015 HORIBA, Ltd. All rights reserved.
Factors affecting abrasion
Difference in hardness between substances: harder abrasives cut faster and deeper.
Grain size (grit size): larger grains cut faster and deeper (and leave deeper scratches).
Grain shape: sharp corners help
Adhesion between grains, between grains and backing, and between grains and matrix determines how quickly grains are lost and how soon fresh grains (if present) are exposed.
© 2015 HORIBA, Ltd. All rights reserved.
Mohs scale
The Mohs scale is a qualitative scale built on knowing which material scratches which others. Since abrasives work by scratching, it is a handy way to think about materials.
Mohs Hardness
Material
1 talc
3 Calcium carbonate
5 enamel
7 quartz
8 emery
9 Aluminum oxide
10 diamond
© 2015 HORIBA, Ltd. All rights reserved.
Macro vs. Micro grits
Macro grits: Greater than 60 mm
Size is generally determined by sieves
Micro grits: Less than 60 mm
Traditional test by sedimentometer.
2 mm macro grit
40 mm micro grit
© 2015 HORIBA, Ltd. All rights reserved.
Table of sizes
Extracted from ANSI B74.12. See the full document for further details. This is Table 3.
Grit 100% min sieve
25% max sieve
35% min sieve
70% min sieve
5% max through sieve
16 8 14 16 16+18 25
All material through #8 sieve
No more than 25% on #14
At least 35% on #16
At least 70% on #16 and #18 combined
No more than 5% through a #25 sieve
© 2015 HORIBA, Ltd. All rights reserved.
Effect of Particle Size: Price
© 2015 HORIBA, Ltd. All rights reserved.
Size: Particle Diameter (mm) 0.01 0.1 1 10 100 1000
Colloidal
Suspensions and Slurries
DLS – SZ-100
Electron Microscope
Powders
Fine Coarse
Optical Microscopy PSA300, Camsizer
Laser Diffraction – LA-950
Acoustic Spectroscopy
Electrozone Sensing
Disc-Centrifuge
Light Obscuration
0.001
Macromolecules
Nano-Metric
Meth
od
s
Ap
ps
S
izes
Sedimentation
Sieves
© 2015 HORIBA, Ltd. All rights reserved.
Weigh % sample caught on known screen sizes
Solid particles 30 mm – 30 mm (and larger)
Advantages:
Low equipment
cost
Direct
measurement
method
No practical upper
limit
Disadvantages:
Limited lower
range
Time
Consuming
High Labor Cost
Need Large
Sample Available through www.retsch.com
Sieves
© 2015 HORIBA, Ltd. All rights reserved.
More information available through www.retsch.com
Replace Sieves
Tend to wear over time. It is difficult to tell when sieve results are “drifting” due to wear
Results depend on nature of shaking and loading leading to operator to operator variations in results.
Small number of size classes
Sieves
© 2015 HORIBA, Ltd. All rights reserved.
Digital Image Analysis
© 2015 HORIBA, Ltd. All rights reserved.
Take a picture,
analyze for size
Measurement Results
Image Analysis
© 2015 HORIBA, Ltd. All rights reserved.
Static Image Analysis
Particles are dispersed (isolated) on a surface
Picture are taken from stationary particles
Camera or surface with particles is shifted, multiple images are taken from different positions, images are processed and evaluated
High resolution images is possible
Number of images/particles is limited (because of time limitations)
Preferred orientation of the particles on the surface (largest 2D)
HORIBA PSA300
© 2015 HORIBA, Ltd. All rights reserved.
Dynamic Image Analysis
Particles flow through the measurement volume of the instrument and the field of view of the camera
Particles are captured during movement, no other moving parts necessary
Capturing of many particle images in a short time interval
Limitations because of image rate of the camera(s)
Image quality is (a bit) worse
Particles are projected in random orientation (3D)
CAMSIZER
© 2015 HORIBA, Ltd. All rights reserved.
Data Evaluation
Binarize
Find Edges
Analyze Each Particle
Output Distribution
Raw Image
© 2015 HORIBA, Ltd. All rights reserved.
xc min
xc min
“width”
A
A‘ = A xare
a
“diameter over
projection surface”
xarea
“length”
xFe max
xFe max
Width is best suited for
comparison with sieves !
Shape parameters can be calculated!
Many Size Measures
© 2015 HORIBA, Ltd. All rights reserved.
x [mm]0.1 10
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Q3
Tinovetin-B-CA584A_BZ_xc_min_002.rdf
Syngenta-1mm-2min-Sieb.ref
Meßwertdiagramm:
D:\...-Demo-Muenchwillen\CAMSIZER-Messungen\Tinovetin-B-CA584A_BZ_xc_min_002.rdf
Meßaufgabe: Syngenta-BZ.afg
Digital Image Processing
Measuring of Width Sieving
Competing Measuring Methods
--- width measurement
-*- Sieving
comparison
CAMSIZER-measurement xc min (red) and sieving * (black)
xc min
xc min
“width”
18 © Retsch Technology GmbH
© 2015 HORIBA, Ltd. All rights reserved.
fitted result
CAMSIZER-measurement xarea (red) to sieving * (blue)
Fitting of CAMSIZER results to Sieving
19 © Retsch Technology GmbH
© 2015 HORIBA, Ltd. All rights reserved.
Shape Analysis
area of the
particle
perimeter of
the particle
circle with
same area
as particle
diameter of
circle of
same area
© 2015 HORIBA, Ltd. All rights reserved.
Shape Analysis
SPHT 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
0
10
20
30
40
50
60
70
80
90
Q3 [%]
Pharma-Product-1-30kPa-bonne-forme-_xc_min_009.rdf
Pharma-Product-1-30kPa_Vitesse-Adaption_xc_min_008.rdf
lactose-30kPa_xFemax_003.rdf
Pharma-Product-2-460_xc_min_008.rdf
© 2015 HORIBA, Ltd. All rights reserved.
Easy shape example
b/l0.4 0.5 0.6 0.7 0.8 0.90
10
20
30
40
50
60
70
80
90
Q3 [%]
A32L 2__xc_min_001.rdfA32L 2__xc_min_002.rdf
A32L 2__xc_min_003.rdfA32L 2__xc_min_004.rdfA32L 2__xc_min_005.rdf
Messwertdiagramm:C:\CAMSIZER4.4.9\CAMDAT\RT1707_Fraunhofer IZM\A32L 2__xc_min_001.rdfMessaufgabe: RT1707.afg
broken round
Length and shape numbers for single particles, from real
pictures
Precise analysis of the amount of broken particles by shape
detection
© 2015 HORIBA, Ltd. All rights reserved.
Fused Silica
2© Retsch
xc_min [mm]0.05 0.10 0.15 0.20 0.25 0.30 0.350
10
20
30
40
50
60
70
80
90
Q3 [%]
Minco50-100_BZ_fix35_10mmGS_convex_xc_min_009.rdf
RT1549_50-100_rec_sieve.ref
Graph of measurement results:
D:\...nuary\CAMDAT\Mesh-50-100\Minco50-100_BZ_fix35_10mmGS_convex_xc_min_009.rdf
Task file: RT1594_Minco30-50_convex_10mm-GS.afg
0.1 – 0.35mm
xc_min [mm]0.1 0.2 0.3 0.40
100
200
300
400
500
600
q3 [%/mm]Minco-50-100_Sample-4-05%_xc_min_001.rdf
Minco-50-100_Sample-3-05%_xc_min_006.rdf
Minco-50-100_Sample 1 Half Repeat_xc_min_005.rdf
Graph of measurement results:
C:\...-3-16\CAMDAT\Mesh-50-100-Sample-4\Minco-50-100_Sample-4-05%_xc_min_001.rdf
Task file: RT1594_Minco50-100_10mm-GS.afg
© 2015 HORIBA, Ltd. All rights reserved.
Different Aspect Ratio of Abrasives
b/l0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.90
10
20
30
40
50
60
70
80
90
Q3 [%]
SWSK-F24-Fraktion1_5Mess_xc_min002.rdf
SWSKL-HQ-F24-Fraktion1__xc_min001.rdf
ZWSK-F24-Fraktion1__xc_min001.rdf
ZWSK-F24-Fraktion1_5Mess_xc_min002.rdf
Meßwertdiagramm:
D:\...rklassen-Schleifmittel24\Fraktion 1\SWSK-F24-Fraktion1_5Mess_xc_min002.rdf
Meßaufgabe: Versuch Fraktion1.afg
Width/Length Aspect ratio
<= elongated/
non round
Cu
mu
late
d r
ela
tive
sa
mp
le v
olu
me
compact/ =>
round
© 2015 HORIBA, Ltd. All rights reserved.
Detection of Oversize Particles
2© Retsch
xc_min [µm]8 10 12 14 160
10
20
30
40
50
60
70
80
90
Q3 [%]
CA10 Feed 450kpa_xc_min_007.rdf
CA10 Feed 450kpa_xc_min_008.rdf
CA10 T18 C 450kpa_xc_min_004.rdf
CA10 T18 C 450kpa_xc_min_005.rdf
CA10 T18F-A 450kpa_xc_min_001.rdf
CA10 T18F-A 450kpa_xc_min_002.rdf
CA10 T18F-B 450kpa_xc_min_001.rdf
CA10 T18F-B 450kpa_xc_min_002.rdf
Graph of measurement results:
C:\...Camsizer4 3 19 XT\CAMDAT\RT1694 Microbeads\CA10 Feed 450kpa_xc_min_007.rdf
Task file: RT1694 PMMA 450.afg
Cum
ulat
ive
Dis
trib
utio
n
Particle size [µm]
4 Samples:
Red
Green
Blue
Violet xc_min [µm]13 14 15 16 17 18
99.0
99.2
99.4
99.6
99.8
100.0
Q3 [%]
CA10 Feed 450kpa_xc_min_av.rdf
CA10 T18F-B 450kpa_xc_min_av.rdf
CA10 T18 C 450kpa_xc_min_av.rdf
CA10 T18F-A 450kpa_xc_min_av.rdf
Graph of measurement results: Mean values, task RT1694 PMMA 450.afg
C:\...Camsizer4 3 19 XT\CAMDAT\RT1694 Microbeads\
CA10 Feed 450kpa_xc_min_008.rdf, CA10 Feed 450kpa_xc_min_007.rdf
Δ ~ approx 0.5% Vol.
Red with oversized particles
Green without oversize
Blue with oversized particles
Violet without oversize
© 2015 HORIBA, Ltd. All rights reserved.
width/
length =
aspect ratio
Sphericity
Symmetry
Convexity
xFe max
xc min
A P
r1
r2
S
A convex
A real
Particle Shape
maxFe
minc
x
x
P
A2
4
2
1
r
rmin1
2
1
convex
real
A
A
© 2015 HORIBA, Ltd. All rights reserved.
New (Old?) shape descriptors
CAMSIZER P4 Krumbeins Roundness and Sphericity
For proppants, sands, and other non-round, angular particles Compatible with ISO 13503-2 and API
Krumbein Sphericity SPHT_K measures the elongation of the particles (like w/l = b/l). Calculation based on W/L_perp = B/Lrec, with a different scaling
Average diameter of all corners divided by diameter of maximum inscribed circle
Krumbein Roundness RDNS_C measures the „angularity“, or „corner curvature radius“
© 2015 HORIBA, Ltd. All rights reserved.
Laser Diffraction
© 2015 HORIBA, Ltd. All rights reserved.
LA-960 Optics
© 2015 HORIBA, Ltd. All rights reserved.
Effect of Size
As diameter increases, intensity (per particle) increases
and location of first peak shifts to smaller angle.
© 2015 HORIBA, Ltd. All rights reserved.
Mixing Particles? Just Add
The result is the weighted sum of the scattering from each particle.
Note how the first peak from the 2 micron particle is suppressed since it
matches the valley in the 1 micron particle.
© 2015 HORIBA, Ltd. All rights reserved.
Why 2 Wavelengths?
30, 40, 50, 70 nm
latex standards
Data from very small particles.
© 2015 HORIBA, Ltd. All rights reserved.
Diamond
High refractive index: 2.41
0
50
10
20
30
40
0.010 50000.100 1.000 10.00 100.0 10000
100
20
40
60
80q
(%
)
Diameter (µm)
Un
ders
ize (
%)
Run D50 microns
1 30.80
2 30.44
3 30.49
4 30.53
Avg. 30.6
Std. Dev.
0.16
© 2015 HORIBA, Ltd. All rights reserved.
Silicon Carbide
High refractive index: 2.65
0
50
10
20
30
40
0.010 50000.100 1.000 10.00 100.0 10000
100
20
40
60
80
q (
%)
Diameter (µm)
Un
ders
ize (
%)
D50 microns
Dry 9.44
Wet 9.21
© 2015 HORIBA, Ltd. All rights reserved.
CMP Slurry (detect oversize)
Can detect added oversize particles!
Median Size : 1.65 µm
Colloidal Silica
Median Size : 0.031 µm
Median (Peak 1) : 0.031 µm Median (Peak 2) : 1.75 µm
Larger Silica
Mixture to check
sensitivity to
impurities
© 2015 HORIBA, Ltd. All rights reserved.
10 ml 35 ml 200 ml powders
•Wide range of sample cells depending on application
•High sensitivity keeps sample requirements at minimum
•Technology has advanced to remove trade-offs
Flexible Sample Handlers
© 2015 HORIBA, Ltd. All rights reserved.
How much sample (wet)?
Larger, broad distributions require larger sample volume
Lower volume samplers for precious materials or solvents
LA-950 Sample Handlers
Dispersing Volume (mL)
Aqua/SolvoFlow 180 - 330
MiniFlow 35 - 50
Fraction Cell 15
Small Volume Fraction Cell
10
Median (D50): 35 nm
Sample Amount: 132 mg
Median (D50): 114 µm
Sample Amount: 1.29 mg
Median (D50): 9.33 µm
Sample Amount: 0.165 mg
Note: Fraction cell has only
magnetic stir bar, not for
large or heavy particles
Bio polymer Colloidal silica Magnesium stearate
It depends on sample, but here
are some examples.
© 2015 HORIBA, Ltd. All rights reserved.
How much sample (dry)?
Larger, broad distributions require larger sample quantity
Can measure less than 5 mg (over a number of particle sizes).
Median (D50): 35 nm
Sample Amount: 132 mg
Median (D50): 114 µm
Sample Amount: 1.29 mg
Median (D50): 9.33 µm
Sample Amount: 0.165 mg
Bio polymer Colloidal silica Magnesium stearate
It depends on sample …..
wet wet wet
© 2015 HORIBA, Ltd. All rights reserved.
Measurement Workflow
Measurement
Click “Measure” button
– Hardware measures scattered light distribution
– Software then calculates size distribution
© 2015 HORIBA, Ltd. All rights reserved.
Instrument to instrument variation
Sample CV D10 CV D50 CV D90
PS202 (3-30µm) 2% 1% 2%
PS213 (10-100µm) 2% 2% 2%
PS225 (50-350µm) 1% 1% 1%
PS235 (150-650µm) 1% 1% 2%
PS240 (500-2000µm) 3% 2% 2%
These are results from running polydisperse standards on 20 different instruments
20 instruments, 5 standards
© 2015 HORIBA, Ltd. All rights reserved.
Instrument to instrument variation
Industrial Samples
4 instruments, real sample
© 2015 HORIBA, Ltd. All rights reserved.
The Benefits
Wide size range Most advanced analyzer measures from 10 nano to 5 milli
Flexible sample handlers Powders, suspensions, emulsions, pastes, creams
Very fast Allows for high throughput, 100’s of samples/day
Easy to use Many instruments are highly automated with self-guided
software
Good design = Excellent precision Reduces unnecessary investigation/downtime
First principle measurement No calibration necessary
Massive global install base/history
© 2015 HORIBA, Ltd. All rights reserved.
Q&A
Ask a question at [email protected]
Keep reading the monthly HORIBA Particle e-mail newsletter!
Visit the Download Center to find the video and slides from this webinar.
www.horiba.com/us/particle
Jeff Bodycomb, Ph.D.
P: 866-562-4698