© 2013 HORIBA, Ltd. All rights reserved.Mark Bumillermark.bumiller@horiba.comThe Importance ofParticle Shape
© 2013 HORIBA, Ltd. All rights reserved.Why is Shape Important?Most (all?) particles are not perfectlybehaving spheresSh...
© 2013 HORIBA, Ltd. All rights reserved.Particle ProcessesPowder flow; spheres flow easily,needles do notLiquid flow; in...
© 2013 HORIBA, Ltd. All rights reserved.Powder FlowUnderstand that spheres flow moreeasily than needlesHow to quantify? ...
© 2013 HORIBA, Ltd. All rights reserved.Powder Flow*c =hopper angleBC = outlet diameterAngle of internal friction*
© 2013 HORIBA, Ltd. All rights reserved.Powder Flow Unconfined YieldStrength Major principlestress that causesan unconfi...
© 2013 HORIBA, Ltd. All rights reserved.Powder Flow*Glass spheres CaCo3 TalcSimilar size ~ 5 µm But different shape*Bumill...
© 2013 HORIBA, Ltd. All rights reserved.Powder FlowBC: minimum outlet diameter to prevent archingc: hopper wall angle (fr...
© 2013 HORIBA, Ltd. All rights reserved.Powder Flow**Podczeck & Miah, The influence of particle size and shape on the angl...
© 2013 HORIBA, Ltd. All rights reserved.Rheology/Viscosity0.01 0.025 0.050Volume FractionViscosity100 200 300 nm Complex ...
© 2013 HORIBA, Ltd. All rights reserved.Mixing Shape affects mobility and therefore causessegregation Smaller effect tha...
© 2013 HORIBA, Ltd. All rights reserved.Powder Mixing* Ordered mixtures of powders comprising a microfineactive ingredien...
© 2013 HORIBA, Ltd. All rights reserved.Powder MixingStandarddeviationofconcentrationa achieved more slowly when mixingwi...
© 2013 HORIBA, Ltd. All rights reserved.Product PerformanceJust as shape influences processing,also changes product perfo...
© 2013 HORIBA, Ltd. All rights reserved.Glass Beads for Highway Paint Size and shape critical toreflective properties Mo...
© 2013 HORIBA, Ltd. All rights reserved.Defects from round particlesOvalSatellitesPointedAggregatesGlass Beads for Highway...
© 2013 HORIBA, Ltd. All rights reserved.Abrasion MechanicsDifference in hardness between thetwo substances: a much harder...
© 2013 HORIBA, Ltd. All rights reserved.Dynamic Image AnalysisBy choosing proper size parameter,Xc min, results can match ...
© 2013 HORIBA, Ltd. All rights reserved.Sand: Round vs. “Edgy”Similar in size.Shape difference seenin b/l and sphericity.E...
© 2013 HORIBA, Ltd. All rights reserved.Other Shape ParametersPSA 300Static Image Analysis
© 2013 HORIBA, Ltd. All rights reserved.PSA300 CalculationFind sharp edges at the tips of the particlesCount number of t...
© 2013 HORIBA, Ltd. All rights reserved.PSA300 Calculation
© 2013 HORIBA, Ltd. All rights reserved.AbrasivesSample Vol Round Comp AR AngSmall (µm)d10 16 0.5 0.8 1.1 1.2d50 38.8 0.7 ...
© 2013 HORIBA, Ltd. All rights reserved.Catalysts Size/Shape by CAMSIZERSpherical catalystsEasy, no special effortCylin...
© 2013 HORIBA, Ltd. All rights reserved.Catalysts Size/Shape by CAMSIZERTri & quadralobePossible to distinguishbetween d...
© 2013 HORIBA, Ltd. All rights reserved.Proppant Packing
© 2013 HORIBA, Ltd. All rights reserved.Shape ComparisonAspctRatio0.3 0.4 0.5 0.6 0.7 0.80102030405060708090Q3 [%]Ceramic-...
© 2013 HORIBA, Ltd. All rights reserved.ProppantsTraditional method CAMSIZER
© 2013 HORIBA, Ltd. All rights reserved.Shape Effects Size MeasurementsInherent effect since light scatteringinstruments ...
© 2013 HORIBA, Ltd. All rights reserved.Modeling/Predicting DifferencesIn particle size; choose a technique,influence the...
© 2013 HORIBA, Ltd. All rights reserved.Modeling/Predicting Differences
© 2013 HORIBA, Ltd. All rights reserved.Modeling/Predicting DifferencesMy sample is a rod, what will my instrument report?...
© 2013 HORIBA, Ltd. All rights reserved.Defining SizeMeasurement Resultsxc minxc min“width”AA‘ = Axarea“diameter overproje...
© 2013 HORIBA, Ltd. All rights reserved.x [mm]0.1 100.10.20.30.40.50.60.70.80.9Q3Tinovetin-B-CA584A_BZ_xc_min_002.rdfSynge...
© 2013 HORIBA, Ltd. All rights reserved.Laser Diffraction vs. Sieves Sieves report smaller sizeTypically 10-30% smaller...
© 2013 HORIBA, Ltd. All rights reserved.Fiber: Laser Diffraction vs. ImagesNote: both distributions widened by laser diffr...
© 2013 HORIBA, Ltd. All rights reserved.Want to Avoid Influence of Shape? Use image analysis ! Direct measurement of siz...
© 2013 HORIBA, Ltd. All rights reserved.SummaryParticle shape a critical physicalparameterAffects the product, the proce...
© 2013 HORIBA, Ltd. All rights reserved.Resources: www.horiba.com/particleNext webinarView webinarsGet information
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Importance of Particle Shape

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Mark Bumiller from HORIBA Scientific (www.horiba.com/particle) discusses how the shape of particles can be a critical physical characteristic that affects processing behavior and end product performance. Choosing the right characterization tool and data interpretation can be challenging tasks for those not familiar with the science of particle morphology. The presentation will reference dynamic image analysis and static image analysis technologies as well as the CAMSIZER and PSA300 products.

Topics covered include:
* Why particle shape is important
* Which analytical tools are available
* How to get the most from these instruments
* How to interpret results

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Importance of Particle Shape

  1. 1. © 2013 HORIBA, Ltd. All rights reserved.Mark Bumillermark.bumiller@horiba.comThe Importance ofParticle Shape
  2. 2. © 2013 HORIBA, Ltd. All rights reserved.Why is Shape Important?Most (all?) particles are not perfectlybehaving spheresShape can influence almost everythingParticle processes, making productsProduct performanceMaking measurementsSo in other words, shape can affect almosteverything
  3. 3. © 2013 HORIBA, Ltd. All rights reserved.Particle ProcessesPowder flow; spheres flow easily,needles do notLiquid flow; increased aspect ratio willincrease viscosityPowder mixing; blend time may changewith shapeAlso VERY associated with size, hardsometimes to separate size and shape
  4. 4. © 2013 HORIBA, Ltd. All rights reserved.Powder FlowUnderstand that spheres flow moreeasily than needlesHow to quantify? Need to first knowsomething about powder flow testingWon’t go into great detail in today’s talkJust show results including particleshape
  5. 5. © 2013 HORIBA, Ltd. All rights reserved.Powder Flow*c =hopper angleBC = outlet diameterAngle of internal friction*
  6. 6. © 2013 HORIBA, Ltd. All rights reserved.Powder Flow Unconfined YieldStrength Major principlestress that causesan unconfined bulkmaterial to fail inshear Directly proportionalto arching &formation of ratholes Influences by #contact pointsFrom: Johansen, Effect of Particle Shape onUnconfined Yield Strength, Material FlowSolutions,Inc.
  7. 7. © 2013 HORIBA, Ltd. All rights reserved.Powder Flow*Glass spheres CaCo3 TalcSimilar size ~ 5 µm But different shape*Bumiller, et. al., A Preliminary Investigation Concerning the Effect of Particle Shape on a Powder’s FlowProperties, Proceeding from WCPT4, July 2002
  8. 8. © 2013 HORIBA, Ltd. All rights reserved.Powder FlowBC: minimum outlet diameter to prevent archingc: hopper wall angle (from verticle) to achieve mass flowCritical flow rate: predicted flow from outlet: effective angle of internal friction
  9. 9. © 2013 HORIBA, Ltd. All rights reserved.Powder Flow**Podczeck & Miah, The influence of particle size and shape on the angle of internal friction and the flow factor ofunlubricated and lubricated powders, International Journal of Pharmaceutics 144 (1996) 187 194AR
  10. 10. © 2013 HORIBA, Ltd. All rights reserved.Rheology/Viscosity0.01 0.025 0.050Volume FractionViscosity100 200 300 nm Complex relationshipbetween size/shape andrheology More spherical shape =lower viscosity Small particle size = higherviscosity Wider particle sizedistribution = lower viscosityspherescubesfibers
  11. 11. © 2013 HORIBA, Ltd. All rights reserved.Mixing Shape affects mobility and therefore causessegregation Smaller effect than size Shape differences but be substantial*Koller et. al.,Continuous quantitative monitoring of powder mixing dynamics by near-infrared spectroscopyPowder Technology, Volume 205, Issues 1–3, 10 January 2011, Pages 87–96*
  12. 12. © 2013 HORIBA, Ltd. All rights reserved.Powder Mixing* Ordered mixtures of powders comprising a microfineactive ingredient adsorbed onto coarser particles ofan excipient offer significant advantages in themanufacture of pharmaceutical solid drug deliverysystemsLactose/calcium carbonate mixtures•Wong & Pilpel, Effect of Particle Shape on the Mixing of Powders,J. Pham. Phamacol. 1990,42: 1-6
  13. 13. © 2013 HORIBA, Ltd. All rights reserved.Powder MixingStandarddeviationofconcentrationa achieved more slowly when mixingwith shape SL and SH (higher shapecoefficient) and BM and CH (lowershape coefficient)
  14. 14. © 2013 HORIBA, Ltd. All rights reserved.Product PerformanceJust as shape influences processing,also changes product performanceSome products perform better whenmore sphericalGlass beads for highway paintProppantsSome products perform better whenless sphericalAbrasives
  15. 15. © 2013 HORIBA, Ltd. All rights reserved.Glass Beads for Highway Paint Size and shape critical toreflective properties More round = morereflectivity back to source CAMSIZER uses b/l ratio toquantify roundnessDry In paint
  16. 16. © 2013 HORIBA, Ltd. All rights reserved.Defects from round particlesOvalSatellitesPointedAggregatesGlass Beads for Highway PaintQuantified by Camsizer
  17. 17. © 2013 HORIBA, Ltd. All rights reserved.Abrasion MechanicsDifference in hardness between thetwo substances: a much harderabrasive will cut faster and deeperGrain size (grit size): larger grainswill cut faster as they also cutdeeperGrain shape: sharp corners helpsome mechanismsCompactness helps in others
  18. 18. © 2013 HORIBA, Ltd. All rights reserved.Dynamic Image AnalysisBy choosing proper size parameter,Xc min, results can match historic sieveData. Also generates shape data provenTo correlate with abrasive performance.
  19. 19. © 2013 HORIBA, Ltd. All rights reserved.Sand: Round vs. “Edgy”Similar in size.Shape difference seenin b/l and sphericity.Edgy would makebetter abrasive.SphericityBreadth/length (b/l)
  20. 20. © 2013 HORIBA, Ltd. All rights reserved.Other Shape ParametersPSA 300Static Image Analysis
  21. 21. © 2013 HORIBA, Ltd. All rights reserved.PSA300 CalculationFind sharp edges at the tips of the particlesCount number of tips (child count)Number of tips alone not sufficient, longparticles w/2 tips not as good as hexagonw/6 tipsDefine angularity roundness as child countx roundnessThus triangle w/3 points less angular thanoctagon of 4 sharp edges & 4 roundededges
  22. 22. © 2013 HORIBA, Ltd. All rights reserved.PSA300 Calculation
  23. 23. © 2013 HORIBA, Ltd. All rights reserved.AbrasivesSample Vol Round Comp AR AngSmall (µm)d10 16 0.5 0.8 1.1 1.2d50 38.8 0.7 0.9 1.3 2.3d90 63.1 0.9 0.9 1.8 3.6Mediumd10 140 0.3 0.5 1.2 1d50 211.8 0.5 0.7 1.6 1.9d90 319.9 0.7 0.8 2.5 3.3Larged10 332.9 0.6 0.7 1.1 2.1d50 375.2 0.7 0.8 1.3 3.4d90 421.4 0.8 0.9 1.5 5Angularity Roundness: count sharptips, create child areasAR: roundness x child area
  24. 24. © 2013 HORIBA, Ltd. All rights reserved.Catalysts Size/Shape by CAMSIZERSpherical catalystsEasy, no special effortCylindrical catalystsLength, widthBended extrudatesUse other parameters 2min2max )()( cFelength xxx mincstretchxAx 
  25. 25. © 2013 HORIBA, Ltd. All rights reserved.Catalysts Size/Shape by CAMSIZERTri & quadralobePossible to distinguishbetween differentdiametersShorter greendistribution = lengthTaller maroondistribution= widthSize helps defineshapeQuadralobe catalystsTrilobe catalysts
  26. 26. © 2013 HORIBA, Ltd. All rights reserved.Proppant Packing
  27. 27. © 2013 HORIBA, Ltd. All rights reserved.Shape ComparisonAspctRatio0.3 0.4 0.5 0.6 0.7 0.80102030405060708090Q3 [%]Ceramic-Prop-EP-20-40-Mesh-40.rdfCeramic-Prop-SB-20-40-Mesh1.rdfCeramic-Prop-SG-V-1.rdfSand-Prop-SIB-20-40-MIS-9.rdfNatural-Brown-Sand-C-20-40.rdfWhite-Sand-Prop-UNF-20-40-17.rdfWhite-Sand-Prop-SIB-20-40-CHF-10.rdfWhite-Sand-Prop-UNF-20-40-1.rdfWhite-Sand-Prop-UNF-20-40-8.rdflwShape comparison between natural sand proppants and ceramic proppants.There are two clearly different ranges of Aspect Ratio (Krumbein’s Sphericity).Analysis of other shape parameters are possible as well (Convexity for ceramic beadtwins, Symmetry for good and broken ceramic beads, Krumbein’s Roundnessetc.)
  28. 28. © 2013 HORIBA, Ltd. All rights reserved.ProppantsTraditional method CAMSIZER
  29. 29. © 2013 HORIBA, Ltd. All rights reserved.Shape Effects Size MeasurementsInherent effect since light scatteringinstruments report equivalent sphericaldiameterSieve vs. laser diffraction vs. imageanalysisConsider cylinder vs. sphere=V = r2h V = 4r33Sieve = 50 mmLaser = 72 mmIA = full description
  30. 30. © 2013 HORIBA, Ltd. All rights reserved.Modeling/Predicting DifferencesIn particle size; choose a technique,influence the answerWell explained in this paperPresented at the Spring Meeting of the Parenteral Drug Association in Philadelphia, June 1977
  31. 31. © 2013 HORIBA, Ltd. All rights reserved.Modeling/Predicting Differences
  32. 32. © 2013 HORIBA, Ltd. All rights reserved.Modeling/Predicting DifferencesMy sample is a rod, what will my instrument report?Coulter counter: 52 µm, laser diffraction: 81µm
  33. 33. © 2013 HORIBA, Ltd. All rights reserved.Defining SizeMeasurement Resultsxc minxc min“width”AA‘ = Axarea“diameter overprojection surface”xarea“length”xFemaxxFe maxCAMSIZER resultsarecompatiblewithsieve analysis
  34. 34. © 2013 HORIBA, Ltd. All rights reserved.x [mm]0.1 100.10.20.30.40.50.60.70.80.9Q3Tinovetin-B-CA584A_BZ_xc_min_002.rdfSyngenta-1mm-2min-Sieb.refWidth  Sieving--- width measurement-*- SievingcomparisonCAMSIZER-measurement xc min (red)and sieving * (black)xc minxc min“width”
  35. 35. © 2013 HORIBA, Ltd. All rights reserved.Laser Diffraction vs. Sieves Sieves report smaller sizeTypically 10-30% smaller Depends on shape Options to correlate Shift reported results 50% passes 325 mesh (44 µm) D50 by diffraction = 53 µm Report value @ 53 µm ads pass 325mesh result LA-950 correlation tools
  36. 36. © 2013 HORIBA, Ltd. All rights reserved.Fiber: Laser Diffraction vs. ImagesNote: both distributions widened by laser diffractionlengthwidth
  37. 37. © 2013 HORIBA, Ltd. All rights reserved.Want to Avoid Influence of Shape? Use image analysis ! Direct measurement of size + shape Get not only size but also shape distributionCAMSIZER PSA300
  38. 38. © 2013 HORIBA, Ltd. All rights reserved.SummaryParticle shape a critical physicalparameterAffects the product, the process and labmeasurementsUnderstand how shape affects yourbusinessUnderstand how shape influences yourmeasurements
  39. 39. © 2013 HORIBA, Ltd. All rights reserved.Resources: www.horiba.com/particleNext webinarView webinarsGet information

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