Materials Characterization Lab
                                www.mri.psu.edu/mcl



SMALL ANGLE XRAY SCATTERING (SAXS)

...
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                                          www.mri.psu.edu/mcl




      MCL SERVICES


•   ...
Materials Characterization Lab
          www.mri.psu.edu/mcl




200 mesh




400 mesh
Materials Characterization Lab
                                                               www.mri.psu.edu/mcl
        ...
Materials Characterization Lab
                                                               www.mri.psu.edu/mcl


      ...
Materials Characterization Lab
                                      www.mri.psu.edu/mcl




What kinds of materials?




...
Materials Characterization Lab
                               www.mri.psu.edu/mcl



What kinds of materials?
Materials Characterization Lab
                               www.mri.psu.edu/mcl




What kinds of materials?
Materials Characterization Lab
                                                             www.mri.psu.edu/mcl




Exampl...
Materials Characterization Lab
                                                                  www.mri.psu.edu/mcl




E...
Materials Characterization Lab
                                                               www.mri.psu.edu/mcl




Exam...
Materials Characterization Lab
                                                           www.mri.psu.edu/mcl




Examples...
Materials Characterization Lab
    www.mri.psu.edu/mcl




 Mouse bone
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                                                           www.mri.psu.edu/mcl


          ...
Materials Characterization Lab
                                                 www.mri.psu.edu/mcl




          Common S...
Materials Characterization Lab
                                www.mri.psu.edu/mcl



Dilute Particulate models
Materials Characterization Lab
                                www.mri.psu.edu/mcl



Dilute Particulate models
Materials Characterization Lab
                                www.mri.psu.edu/mcl


Dilute Particulate Models
Materials Characterization Lab
                                          www.mri.psu.edu/mcl




          Common SAXS Mod...
Materials Characterization Lab
                                           www.mri.psu.edu/mcl




            Common SAXS ...
Materials Characterization Lab
    www.mri.psu.edu/mcl
Materials Characterization Lab
                          www.mri.psu.edu/mcl




Photoresist grating
Materials Characterization Lab
                                                      www.mri.psu.edu/mcl




             ...
Materials Characterization Lab
                                     www.mri.psu.edu/mcl




TWO IMPORTANT GENERAL MODEL RE...
Materials Characterization Lab
                                                         www.mri.psu.edu/mcl


            ...
Materials Characterization Lab
                                            www.mri.psu.edu/mcl



               GUINIER L...
Materials Characterization Lab
                                                           www.mri.psu.edu/mcl



         ...
Materials Characterization Lab
                              www.mri.psu.edu/mcl



   INSTRUMENTS FOR SAXS


•KRATKY CAME...
Materials Characterization Lab
                    www.mri.psu.edu/mcl




KRATKY CAMERA
Materials Characterization Lab
                                              www.mri.psu.edu/mcl



       INSTRUMENTS FOR...
Materials Characterization Lab
                        www.mri.psu.edu/mcl


BEAM CONDITIONING
Materials Characterization Lab
                        www.mri.psu.edu/mcl


MOLMET (PSU) SAXS
Materials Characterization Lab
    www.mri.psu.edu/mcl
Materials Characterization Lab
                                              www.mri.psu.edu/mcl



       INSTRUMENTS FOR...
Materials Characterization Lab
                     www.mri.psu.edu/mcl


Sample holders
Materials Characterization Lab
                               www.mri.psu.edu/mcl


Multi-wire Area Detector
Materials Characterization Lab
               www.mri.psu.edu/mcl




EXAMPLES
Materials Characterization Lab
                                                      www.mri.psu.edu/mcl


               ...
Materials Characterization Lab
                                                                                           ...
Materials Characterization Lab
                               www.mri.psu.edu/mcl




Core-Shell latex spheres
Materials Characterization Lab
                                                 www.mri.psu.edu/mcl


      Supercritical ...
Materials Characterization Lab
    www.mri.psu.edu/mcl
Materials Characterization Lab
    www.mri.psu.edu/mcl
Materials Characterization Lab
                                                     www.mri.psu.edu/mcl



   Pt particle ...
Materials Characterization Lab
                                                       www.mri.psu.edu/mcl



Pt particle s...
Materials Characterization Lab
                                                         www.mri.psu.edu/mcl



Pt particle...
Materials Characterization Lab
                                                        www.mri.psu.edu/mcl



Pt particle ...
Materials Characterization Lab
                                               www.mri.psu.edu/mcl



      Deformation Sta...
Materials Characterization Lab
                                            www.mri.psu.edu/mcl



Come see the PSU MCL Mol...
Upcoming SlideShare
Loading in …5
×

Saxs 2005

1,137 views

Published on

Published in: Business, Technology
0 Comments
1 Like
Statistics
Notes
  • Be the first to comment

No Downloads
Views
Total views
1,137
On SlideShare
0
From Embeds
0
Number of Embeds
32
Actions
Shares
0
Downloads
59
Comments
0
Likes
1
Embeds 0
No embeds

No notes for slide

Saxs 2005

  1. 1. Materials Characterization Lab www.mri.psu.edu/mcl SMALL ANGLE XRAY SCATTERING (SAXS) AUGUST 10, 2005 Mark S. Angelone msa3@psu.edu
  2. 2. Materials Characterization Lab www.mri.psu.edu/mcl Summer Characterization Open Houses Technique Time Date Location Thermal analysis (TGA, DTA, DSC) 9:45 AM June 8 250 MRL Bldg. Transmission Electron Microscopy (TEM/STEM) 9:45 AM June 15 114 MRI Bldg Scanning electron microscopy (SEM) 9:45 AM June 22 541 Deike Bldg. Analytical SEM 11:00 AM June 22 541 Deike Bldg. X-ray Diffraction (XRD) 9:45 AM June 29 250 MRL Bldg. Dielectric Characterization (25 min lecture only) 9:45 AM July 6 250 MRL bldg. High temperature sintering lab (20 min lecture only) 10:15 AM July 6 250 MRL Bldg. Focused Ion Beam (FIB) 9:45 AM July 13 114 MRI Bldg TEM sample preparation 11:00 AM July 13 114 MRI Bldg Orientation imaging microscopy (OIM/EBSD) 9:45 AM July 20 250 MRL Bldg. Chemical analysis (ICP, ICP-MS) 9:45 AM July 27 541 Deike Bldg. Atomic Force Microscopy (AFM) 9:45 AM August 3 114 MRI Bldg Small angle x-ray scattering (SAXS) 9:45 AM August 10 541 Deike Bldg. Particle Characterization 9:45 AM August 17 250 MRL X-ray photoelectron spectroscopy (XPS/ESCA) 9:45 AM August 24 114 MRI Bldg Auger Electron Spectroscopy (AES) 11:00 AM August 24 114 MRI Bldg NOTE LOCATIONS: The MRI Bldg is in the Innovation Park near the Penn Stater Hotel; MRL Bldg. is on Hastings Road. More information: www.mri.psu.edu/mcl
  3. 3. Materials Characterization Lab www.mri.psu.edu/mcl Materials Characterization Lab Locations MRI Bldg: XPS/ESCA, FIB SIMS, TEM, HR- TEM, FE-Auger, MRL Bldg: Hosler Bldg: AFM, XRD SEM, XRD, OIM, DTA, SEM,AFM,ESEM, FE- DSC, TGA, FTIR, Penn Stater SEM, EPMA, ICP, Hotel Raman, AFM, Powder, E&ES Bldg: ICP-MS,BET, SAXS dielectric, prep, shop, SEM IC, UV-Vis Route 322 Steidle Bldg: Atherton Street Nanoindenter (322 Business) I-99 Park Ave. 0 0 0 0 0 0 0 Ave. 0 0 0 0 0 Park 0 Beaver 0 0 Stadium 0 0 0 Centre 0 0 Porter Road Community Univ Shortlidg Hospital 0 0 Burrowes Road ersi ty D e Pollock Road Road rive North Hastin Deike Bldg: gs Ro ad College Ave.
  4. 4. Materials Characterization Lab www.mri.psu.edu/mcl MCL SERVICES • Facilities/Instruments • User Training • Operators/Analyst for hire • 24/7 • Online bookings • User fees • website/contacts to get started
  5. 5. Materials Characterization Lab www.mri.psu.edu/mcl 200 mesh 400 mesh
  6. 6. Materials Characterization Lab www.mri.psu.edu/mcl Scattering ‘Live’ Demo Real Space Reciprocal Space d1 d2 = d1/2 Smaller d yields larger SD Scattered Beam (1st order) θ SOURCE Direct Beam - - - - - - - θ SD Scattered Beam (1st order) Smaller TAN θ = For Sample/Detector D SD/D Larger d
  7. 7. Materials Characterization Lab www.mri.psu.edu/mcl Bragg Scattering (WAXS-XRD) ηλ = 2 d sin θ λ = Cu Kα = 1.5401 Å q =(4π/λ) sin θ = 2 π/d d 2θ 10Å (0.001 Micron) 8.84º 0.628 A-1 0.126 A-1 50Å 1.17 º 0.063 A-1 100Å 0.88 º 0.021 A-1 300Å 0.29 º 0.010 A-1 600Å 0.15 º 0.006 A-1 1000Å 0.09 º Atomic Structures WAXS (Cu Ka, 2-160 2θ) Sub Angstrom - 10Å Nano/ Colloidal (PSU) Laboratory SAXS 10Å - 1000Å Structures Synchrotron SAXS/SANS 10Å – several 1000Å
  8. 8. Materials Characterization Lab www.mri.psu.edu/mcl What kinds of materials? Compiled by Earle Ryba
  9. 9. Materials Characterization Lab www.mri.psu.edu/mcl What kinds of materials?
  10. 10. Materials Characterization Lab www.mri.psu.edu/mcl What kinds of materials?
  11. 11. Materials Characterization Lab www.mri.psu.edu/mcl Examples from literature Polymer dendrimers dilute solns in CH3OH to get dendrite sizes dilute so dendrimers don’t correlate Alkanediols solns in water to study clustering heavy water improves contrast (sans) Water-based polymer latexes use anionic surfactant to suspend in water Macromolecular foams wafers cut & immersed in toluene to get swelling banded matls are translated in situ Microemulsions oils in water to get droplet size
  12. 12. Materials Characterization Lab www.mri.psu.edu/mcl Examples from literature CVD SiGe films µ-thin films stacked to get Ge heterogeneity Nanotubes use surfactant in water & sonicate; place in quartz cells to study nanotube aggregation Powders thin-walled capillaries Polymers study crystallization processes in situ in hot cell
  13. 13. Materials Characterization Lab www.mri.psu.edu/mcl Examples from literature Thin films on glass substrates as is, but requires grazing incidence Random crystalline block copolymers rheology study in situ in rotating parallel disk cell to get crystal alignment and grain rotations Splat-cooled glass in situ annealing study to follow pptn of PbTe nano-crystals
  14. 14. Materials Characterization Lab www.mri.psu.edu/mcl Examples from literature Blown polymer films special cell for in situ studies Liq. Crystals special magnetic cell for molecule rotation Ionomers cell w/ kapton windows Hi pressure studies diamond windows
  15. 15. Materials Characterization Lab www.mri.psu.edu/mcl Mouse bone
  16. 16. Materials Characterization Lab www.mri.psu.edu/mcl Reciprocal Space Reciprocal Space Real Space Real Space I(q) ⏐A⏐ Γ (r) ⏐A⏐2 ρ (r) I.F.T. F.T. 1/r (q) q r r 1/r (q) Not Possible By Direct Calc Calc – Scattering Theory – F.T. Calc – Auto Correlation Function of ρ (r) Large r Correlation function, radial Large r Amplitude/Phase distribution Observed scattering Particulate shapes Spectra of scattering intensity- Phase mix from individual scatters Small r Noise/truncation Large period structures (continuous/discrete) Pair (Radial) distribution: Short effects range atomic ordering Small r (amorphous materials) Atomic positions •Crystals Large r (SAXS) Diffuse scatter Patterson function: Interatomic •amorphous Small r (WAXS) Diffraction dominates vectors (crystals) for xtals, diffuse scatter for liquids, amorphous solids
  17. 17. Materials Characterization Lab www.mri.psu.edu/mcl Analytical Interpretation Model ρ(r) → calculate I(q) → fit to observed I(q) Or Model ρ(r) → calculate Γ(r) → fit to F.T. of observed I(q) (models cast in parameters of size, shape, dispersity, thermo mixing energy, etc.)
  18. 18. Materials Characterization Lab www.mri.psu.edu/mcl Common SAXS Models DILTUE PARTICULATE SYSTEM •Mono or poly dispersed •No interparticle scattering effects SAXS Interpretation yields •Size/dispersity for known shapes •Rg for unknown shapes •Can incorporate dense packing effects into model
  19. 19. Materials Characterization Lab www.mri.psu.edu/mcl Dilute Particulate models
  20. 20. Materials Characterization Lab www.mri.psu.edu/mcl Dilute Particulate models
  21. 21. Materials Characterization Lab www.mri.psu.edu/mcl Dilute Particulate Models
  22. 22. Materials Characterization Lab www.mri.psu.edu/mcl Common SAXS Models Non Particulate 2 Phase System •2 intermixed phases without host or matrix SAXS Interpretation yields •Phase volume fraction, domain size, •information on interphase boundary (sharp or diffuse)
  23. 23. Materials Characterization Lab www.mri.psu.edu/mcl Common SAXS Models Periodic Systems •Lamellar stacks, ordered copolymers, biologic Periodic and ordered structures WAXS methods apply but with emphasis on deviations from ordered structures
  24. 24. Materials Characterization Lab www.mri.psu.edu/mcl
  25. 25. Materials Characterization Lab www.mri.psu.edu/mcl Photoresist grating
  26. 26. Materials Characterization Lab www.mri.psu.edu/mcl Common SAXS Models Soluble Blend System •Single disordered phase dissolved molecularly with density inhomogeneity (miscible polymers, block copolymers, polymer solns) SAXS Interpretation yields •Solution properties (could be treated as dilute system but blend model formulated for more direct treatment of thermodynamic properties rather than size and shape)
  27. 27. Materials Characterization Lab www.mri.psu.edu/mcl TWO IMPORTANT GENERAL MODEL RESULTS (some interpretation without models) •GUINIER LAW •POROD LAW
  28. 28. Materials Characterization Lab www.mri.psu.edu/mcl GUINIER LAW •Even for unknown, irregular or ‘non-describable shapes; scattering has predictable form at low q
  29. 29. Materials Characterization Lab www.mri.psu.edu/mcl GUINIER LAW Valid for •q << 1/Rg •Dilute system •Isotropic (random particle orientation) •Solvent scattering subtracted
  30. 30. Materials Characterization Lab www.mri.psu.edu/mcl POROD LAW •Predictable relationship between I(q) and total interface area in 2 phase systems at high q •Can obtain total interface area for absolute intensities or specific surface area (S/V) for relative measure of scattered intensity •Deviations from Porod Law indicate and give information on diffuse interphase boundaries •
  31. 31. Materials Characterization Lab www.mri.psu.edu/mcl INSTRUMENTS FOR SAXS •KRATKY CAMERA •PINHOLE CAMERA •LABORATORY SOURCES •SYNCHROTRON SOURCES
  32. 32. Materials Characterization Lab www.mri.psu.edu/mcl KRATKY CAMERA
  33. 33. Materials Characterization Lab www.mri.psu.edu/mcl INSTRUMENTS FOR SAXS •Scattering in transmission mode •1-2mm ideal thickness for polymers/organics •Source is critical •Monochromatic •Intense •Collimated •Small cross section (pinhole)
  34. 34. Materials Characterization Lab www.mri.psu.edu/mcl BEAM CONDITIONING
  35. 35. Materials Characterization Lab www.mri.psu.edu/mcl MOLMET (PSU) SAXS
  36. 36. Materials Characterization Lab www.mri.psu.edu/mcl
  37. 37. Materials Characterization Lab www.mri.psu.edu/mcl INSTRUMENTS FOR SAXS •Scattering in transmission mode •1-2mm ideal thickness for polymers/organics •Source is critical •Monochromatic •Intense •Collimated •Small cross section (pinhole) •Evacuated beam path •Sample holders •Detectors •Film, plates, PSD, Area
  38. 38. Materials Characterization Lab www.mri.psu.edu/mcl Sample holders
  39. 39. Materials Characterization Lab www.mri.psu.edu/mcl Multi-wire Area Detector
  40. 40. Materials Characterization Lab www.mri.psu.edu/mcl EXAMPLES
  41. 41. Materials Characterization Lab www.mri.psu.edu/mcl Silver Behenate Standard r Calibrates center and q on 58.37 A d-space
  42. 42. Materials Characterization Lab www.mri.psu.edu/mcl Polyelectrolytes in Solution SAXS of 60PMVP-I in NMF 500 60PMVP-I/EG Correlation length, ξ ( Angstrom) 3500 concentration: I(q), normalized intensity, (A.U.) 60PMVP-I/NMF 2.5 mg/ml 3000 5.0mg/ml 10.0mg/ml 20.0 mg/ml 2500 100 Slope = -0.4 2000 1500 1000 0.00 0.02 0.04 0.06 0.08 0.10 0.01 0.1 1 -1 q, (Angstrom ) Concentration, c (M) Shichen Dou; PSU Colby group
  43. 43. Materials Characterization Lab www.mri.psu.edu/mcl Core-Shell latex spheres
  44. 44. Materials Characterization Lab www.mri.psu.edu/mcl Supercritical Fluid Treatment of Polymers Poly(aryl ether ether ketone) PEEK high performance thermoplastic with high impact strength, tensile yield strength and thermal and chemical resistance Group studied methyl substituted PEEK annealed in air and supercritical CO2 to control crystallization and reduce processing costs. unpublished Queen’s University, Ontario
  45. 45. Materials Characterization Lab www.mri.psu.edu/mcl
  46. 46. Materials Characterization Lab www.mri.psu.edu/mcl
  47. 47. Materials Characterization Lab www.mri.psu.edu/mcl Pt particle size in carbon-supported Pt electrocatalysts for fuel cell applications Random pore model; three supports Stevens, et al, CARBON 41 (2003)
  48. 48. Materials Characterization Lab www.mri.psu.edu/mcl Pt particle size in carbon-supported Pt electrocatalysts for fuel cell applications SAXS: Pt loadings by mass/ 2 supports Stevens, et al, CARBON 41 (2003)
  49. 49. Materials Characterization Lab www.mri.psu.edu/mcl Pt particle size in carbon-supported Pt electrocatalysts for fuel cell applications Pt Size Distribution: Pt loadings by mass/ 2 supports Stevens, et al, CARBON 41 (2003)
  50. 50. Materials Characterization Lab www.mri.psu.edu/mcl Pt particle size in carbon-supported Pt electrocatalysts for fuel cell applications •This study used moderately small angle so that size agreed with WAXS/Scherrer but SAXS best at smaller size •Generally, WAXS/Scherrer not effective in large sizes (no line broadening, xtal domain vs. grain domain, no distribution info) •TEM/SEM: specific areas vs. average important to catalyst properties Stevens, et al, CARBON 41 (2003)
  51. 51. Materials Characterization Lab www.mri.psu.edu/mcl Deformation Stage SAXS unstressed stressed Toughened Polystyrene
  52. 52. Materials Characterization Lab www.mri.psu.edu/mcl Come see the PSU MCL Molmet SAXS Room 6/7 Hosler

×