3D characterization of asymmetric microfiltration membranes
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3D characterization of asymmetric microfiltration membranes

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By Armin Zankel (Institute for Electron Microscopy, Graz University of Technology)

By Armin Zankel (Institute for Electron Microscopy, Graz University of Technology)

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3D characterization of asymmetric microfiltration membranes 3D characterization of asymmetric microfiltration membranes Presentation Transcript

  • MicroPES®2FHerbert Reingruber Armin Zankel May 30th, 2012 Institute for Electron Microscopy and Fine Structure Research 1
  • 3D Visualization of the membrane structure• Experimental Setup• Sample Preparation• Image Processing• Results Conclusion Institute for Electron Microscopy and Fine Structure Research 2
  • SEMHigh vacuum in the sample chamber necessary ~ 10-4 Torr ESEM E(nvironmental) SEM additional variable pressure range: 0.1 - 20 Torr Institute for Electron Microscopy and Fine Structure Research 3
  • The Environmental Scanning ESEM Quanta 600 FElectron Microscope (ESEM) A Microlab for Science and Industry Institute for Electron Microscopy and Fine Structure Research 4
  • The Environmental ScanningElectron Microscope (ESEM) ESEM: Environmental SEM LV-CSEM: Low Vacuum Conventional SEM CSEM: Conventional SEM Institute for Electron Microscopy and Fine Structure Research 5
  • The Environmental ScanningElectron Microscope (ESEM) Institute for Electron Microscopy and Fine Structure Research 6
  • http://www.gatan.com/sem/3dmicrotomy.htmlhttp://www.pubmedcentral.nih.gov/articlerender.fcgi?artid=524270 Institute for Electron Microscopy and Fine Structure Research 7
  • Experimental setup in situ ultramicrotomy Institute for Electron Microscopy and Fine Structure Research 8
  • Experimental setup in situ ultramicrotomyHistory: Stephen B. Leighton, 1981 Institute for Electron Microscopy and Fine Structure Research 9
  • Institute for Electron Microscopy and Fine Structure Research 10
  • Experimental setup in situ ultramicrotomyPreparation and Positioning of the SpecimenEmbedding in resin, stainingPrecutting with ultramicrotomePositioning with light microscope and CCD-Camera Institute for Electron Microscopy and Fine Structure Research 11
  • First steps: paper Institute for Electron Microscopy and Fine Structure Research 12
  • First steps: paper coatPreparation:Embedding in resinNo staining: intrinsicmaterial contrast fibersPrecutting resin Institute for Electron Microscopy and Fine Structure Research 13
  • First steps: paper 1. cut 50. cut 100. cut100 cuts of a paper specimen (thickness of the slices: 200nm, micrograph: BSE) are assembledinto a three dimensional (3D) model (unit: µm). Institute for Electron Microscopy and Fine Structure Research 14
  • First steps: paper3D model of the fillerparticles of the paper 3D model of the fibers in the paper Institute for Electron Microscopy and Fine Structure Research 15
  • air side roll side DuraPES®200 20 µm 20 µm MicroPES®2F 20 µm 20 µm Institute for Electron Microscopy and Fine Structure Research 16
  • Institute for Electron Microscopy and Fine Structure Research 17
  • 0.5 mm Diamond knife Sample mounted on the rivet 100 µm Institute for Electron Microscopy and Fine Structure Research 18
  • Institute for Electron Microscopy and Fine Structure Research 19
  • DuraPES®450 a b 10µm10µm 10µm 10µm 10µm11.4µm Stack#2 (30.7 x 61.4 x 10.6) µm Stack #2 Stack #3 c d approx. 150µm 10µm 10µm 10µm 3.6µm Stack #1 Stack#1 (39.5 x 163.0 x 45.0) µm Stack#3 (37.5 x 25.6 x 10.0) µm Institute for Electron Microscopy and Fine Structure Research 20
  • [µm] a b 10µm10µm 10µm 10µm 10µm11.4µm [µm][µm] Institute for Electron Microscopy and Fine Structure Research 21
  • a b c da b c [µm] d [µm] [µm] [µm] 30 25 25 30 20 [µm] 12,5 12,5 20 [µm] 10 [µm][µm] 10 10 10 10105 5 5 5 0 0 0 0 5 5 4 5 10 10 [µm] 10 [µm] 8 [µm] [µm] Institute for Electron Microscopy and Fine Structure Research 22
  • MicroPES®4F DuraPES®450 Sartorius 15406surface A surface A surface A(air side) (air side) (air side) 10µm 10 µm 10 µm 10 µm Institute for Electron Microscopy and Fine Structure Research 23
  • specifically measuredInstitute for Electron Microscopy and Fine Structure Research 24
  • MicroPES®4F DuraPES®450 Sartorius 15406 air side air side air sideimages reconstructions SEM 3D 5 µm 5 µm 5 µm roll side roll side roll sidereconstructions 3D images SEM 5 µm 10 µm 5 µm Institute for Electron Microscopy and Fine Structure Research 25
  • 3D reconstruction SEM image Institute for Electron Microscopy and Fine Structure Research 26
  • Resultssub porous structure Institute for Electron Microscopy and Fine Structure Research 27
  • 3D model of the membrane structureCalculation of the absolute permeability Calculation of the pure water flux Institute for Electron Microscopy and Fine Structure Research 28
  • Calculation of the pure water flux: some equations pA pB Q Q A l Darcy´s Law: Ohm‘s Law: with Institute for Electron Microscopy and Fine Structure Research 29
  • MicroPES®4F DuraPES®450 Sartorius 15406surface A surface A surface A(air side) (air side) (air side) 10µm 10 µm 10 µm 10 µm Institute for Electron Microscopy and Fine Structure Research 30
  • specifically measuredInstitute for Electron Microscopy and Fine Structure Research 31
  • • 3D reconstructions reproduce the surface morphology, the pore structures etc.• The gained parameter profiles give quantitative values of the inner pore structure• The results of the fluid simulations are in agreement with the experiment Institute for Electron Microscopy and Fine Structure Research 32
  • [1] W. Denk, H. Horstmann.  Serial Block‐Face Scanning Electron Microscopy to Reconstruct Three‐Dimensional Tissue Nanostructure.  PLoS Biol, 2 (2004) e329.  [2] M. Ulbricht, O. Schuster, W. Ansorge, M. Ruetering, and P. Steiger. Influence of the strongly anisotropic cross‐section morphology of a novel polyethersulfone microfiltration membrane on filtration performance.  Separation and Purification Technology, 57 (2007) 63.  [3] R. Ziel, A. Haus, and A. Tulke.  Quantification of the pore size distribution (porosity profiles) in microfiltration membranes by SEM, TEM and computer image analysis.  J.Membr.Sci., 323 (2008) 241.  [4] H. Reingruber, A. Zankel, C. Mayrhofer, and P. Poelt.  Quantitative characterization of microfiltration membranes by 3D reconstruction.  J.Membr.Sci. 372 (2011) 66‐74.  Institute for Electron Microscopy and Fine Structure Research 33
  • Ing. Claudia Mayrhofer PD Dipl.-Ing. Dr. Peter Pölt Institute for Electron Microscopy and Fine Structure Research 34
  • Dipl.-Ing. Herbert ReingruberThank you for your attention! Time for Discussion Institute for Electron Microscopy and Fine Structure Research 35