MicroPES®2FHerbert Reingruber  Armin Zankel  May 30th, 2012          Institute for Electron Microscopy and Fine Structure ...
3D Visualization of the membrane structure• Experimental Setup• Sample Preparation• Image Processing• Results Conclusion  ...
SEMHigh vacuum in the sample chamber           necessary             ~ 10-4 Torr            ESEM        E(nvironmental) SE...
The Environmental Scanning ESEM Quanta 600 FElectron Microscope (ESEM) A Microlab for Science and Industry                ...
The Environmental ScanningElectron Microscope (ESEM) ESEM: Environmental SEM LV-CSEM: Low Vacuum Conventional SEM CSEM: Co...
The Environmental ScanningElectron Microscope (ESEM)              Institute for Electron Microscopy and Fine Structure Res...
http://www.gatan.com/sem/3dmicrotomy.htmlhttp://www.pubmedcentral.nih.gov/articlerender.fcgi?artid=524270                 ...
Experimental setup in situ ultramicrotomy             Institute for Electron Microscopy and Fine Structure Research       ...
Experimental setup           in situ ultramicrotomyHistory: Stephen B. Leighton, 1981                            Institute...
Institute for Electron Microscopy and Fine Structure Research                                                             ...
Experimental setup              in situ ultramicrotomyPreparation and Positioning of the SpecimenEmbedding in resin, stain...
First steps: paper          Institute for Electron Microscopy and Fine Structure Research                                 ...
First steps: paper                                                                      coatPreparation:Embedding in resin...
First steps: paper                   1. cut                           50. cut                                      100. cu...
First steps: paper3D model of the fillerparticles of the paper   3D model of the fibers in the paper                      ...
air side                                                                    roll side               DuraPES®200       20 µ...
Institute for Electron Microscopy and Fine Structure Research                                                             ...
0.5 mm         Diamond knife         Sample mounted on the rivet                                      100 µm            In...
Institute for Electron Microscopy and Fine Structure Research                                                             ...
DuraPES®450                                     a                                                  b                      ...
[µm]                           a                                                  b                          10µm10µm 10µm...
a                                                   b                              c                            da        ...
MicroPES®4F                           DuraPES®450                                    Sartorius 15406surface A             ...
specifically measuredInstitute for Electron Microscopy and Fine Structure Research                                        ...
MicroPES®4F            DuraPES®450                            Sartorius 15406                                  air side   ...
3D reconstruction   SEM image                                Institute for Electron Microscopy and Fine Structure Research...
Resultssub porous structure           Institute for Electron Microscopy and Fine Structure Research                       ...
3D model of the membrane structureCalculation of the absolute permeability  Calculation of the pure water flux            ...
Calculation of the pure water flux: some equations      pA                                                                ...
MicroPES®4F                           DuraPES®450                                    Sartorius 15406surface A             ...
specifically measuredInstitute for Electron Microscopy and Fine Structure Research                                        ...
• 3D reconstructions reproduce the surface   morphology, the pore structures etc.• The gained parameter profiles give quan...
[1] W. Denk, H. Horstmann.                    Serial Block‐Face Scanning Electron Microscopy to Reconstruct Three‐Dimensio...
Ing. Claudia Mayrhofer   PD Dipl.-Ing. Dr. Peter Pölt                         Institute for Electron Microscopy and Fine S...
Dipl.-Ing. Herbert ReingruberThank you for your attention!                        Time for Discussion                     ...
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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)

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3D characterization of asymmetric microfiltration membranes

  1. 1. MicroPES®2FHerbert Reingruber Armin Zankel May 30th, 2012 Institute for Electron Microscopy and Fine Structure Research 1
  2. 2. 3D Visualization of the membrane structure• Experimental Setup• Sample Preparation• Image Processing• Results Conclusion Institute for Electron Microscopy and Fine Structure Research 2
  3. 3. 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
  4. 4. The Environmental Scanning ESEM Quanta 600 FElectron Microscope (ESEM) A Microlab for Science and Industry Institute for Electron Microscopy and Fine Structure Research 4
  5. 5. 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
  6. 6. The Environmental ScanningElectron Microscope (ESEM) Institute for Electron Microscopy and Fine Structure Research 6
  7. 7. http://www.gatan.com/sem/3dmicrotomy.htmlhttp://www.pubmedcentral.nih.gov/articlerender.fcgi?artid=524270 Institute for Electron Microscopy and Fine Structure Research 7
  8. 8. Experimental setup in situ ultramicrotomy Institute for Electron Microscopy and Fine Structure Research 8
  9. 9. Experimental setup in situ ultramicrotomyHistory: Stephen B. Leighton, 1981 Institute for Electron Microscopy and Fine Structure Research 9
  10. 10. Institute for Electron Microscopy and Fine Structure Research 10
  11. 11. 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
  12. 12. First steps: paper Institute for Electron Microscopy and Fine Structure Research 12
  13. 13. First steps: paper coatPreparation:Embedding in resinNo staining: intrinsicmaterial contrast fibersPrecutting resin Institute for Electron Microscopy and Fine Structure Research 13
  14. 14. 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
  15. 15. 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
  16. 16. 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
  17. 17. Institute for Electron Microscopy and Fine Structure Research 17
  18. 18. 0.5 mm Diamond knife Sample mounted on the rivet 100 µm Institute for Electron Microscopy and Fine Structure Research 18
  19. 19. Institute for Electron Microscopy and Fine Structure Research 19
  20. 20. 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
  21. 21. [µm] a b 10µm10µm 10µm 10µm 10µm11.4µm [µm][µm] Institute for Electron Microscopy and Fine Structure Research 21
  22. 22. 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
  23. 23. 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
  24. 24. specifically measuredInstitute for Electron Microscopy and Fine Structure Research 24
  25. 25. 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
  26. 26. 3D reconstruction SEM image Institute for Electron Microscopy and Fine Structure Research 26
  27. 27. Resultssub porous structure Institute for Electron Microscopy and Fine Structure Research 27
  28. 28. 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
  29. 29. 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
  30. 30. 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
  31. 31. specifically measuredInstitute for Electron Microscopy and Fine Structure Research 31
  32. 32. • 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
  33. 33. [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
  34. 34. Ing. Claudia Mayrhofer PD Dipl.-Ing. Dr. Peter Pölt Institute for Electron Microscopy and Fine Structure Research 34
  35. 35. Dipl.-Ing. Herbert ReingruberThank you for your attention! Time for Discussion Institute for Electron Microscopy and Fine Structure Research 35
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