Hard X-ray Studies of Thin Films and nanoclusters

1. Hard X-ray Studies of Thin Films and nanoclusters Najeh M Jisrawi Birzeit University Najeh M Jisrawi

2. Hard X-ray Studies of Thin Films and nanoclusters • Overview • Hard X-ray Characteristics • In situ studies of superconductors • Studies of battery electrodes • Hydrogen in Pd/Nb multilayers and bimetallic electrodes • Hydrogenated metallic clusters

3. Hard X-ray Study of Superconductors Collaborators: T. Thurston, J. McBreen S. Mukerjee, M. Suenaga Najeh M Jisrawi

4. Penetration and Scattering Geometry T.R.Thurston et.al. J. Aqppl. Phys. 79, 3122(1996).

5. Example Development of the High Tc 2223 Phase Note that up to 10,000 coutns/sec are possible in transmission

6. LiMn2O4 Example T.R. Thurston et.al. Appl.Phys. Lett. 69, 194(1996). Industrial Prototype with X-rays going through casing and battery material

7. Details of Phase Transformation “Rocking Chair” battery transformation probed during operation.

8. Nb thin films Collaborators: M. Dornheim, A. Pundt, and R. Kirchheim B. Ocko and M. Strongin Najeh M Jisrawi

9. Hydrogen-metal phase diagram

10. Hydrogen in Metal Films octahedral tetrahedral

11. Thin Film In Situ Electrochemical Cell ECC made from Teflon Euler cradle of B2 at Hasylab

12. Hydrogen in Bimetallic Electrodes N.M. Jisrawi et.al. J. mater. Res. 12, 2091(1997). • 800 A Pd film.

13. Nb/Pd/Nb (800/200/800)

14. 800 A Nb C-axis expansion In-plane expansion

15. Phase Changes in Nb

16. Development of the b-phase

18. Y-Films Collaborators: M. Dornheim S. Kooij B. Ocko M. Strongin Najeh M Jisrawi

19. Y-H Phases Measurement X’pert machine: 6 h /scan H-Y phase diagram

22. CLUSTERS Collaborators: M. Suleiman, A. Pundt, R. Kirchheim, H. Teichler S. AbdulHadi and I. Ladadwa Najeh M Jisrawi

23. TEM Low resolution: Faceting High Resolution: Crystal Symmetery

24. Magic Numbers

25. Cuboctahedral vs Icosahedral

26. Cuboctahedral to Icosahedral Transition

28. Critical Size for Transformation

29. Hydrogen Gravimetry

30. Synchrotron X-rays

31. XRD: Structure of as-prepared clusters Experiment: As-prepared samples Theory: MD- Simulation small clusters have icosahedral structure.The number of nearest neighbours is large & the surface energy is low. large cluster has (ca. 6 nm) cubic structure. Interatomic spacing in not uniform in an ico. mechanical stresses.  M. Suleiman 6

32. In-situ XRD HASYLAB:  6 nm Cluster “cubic” ´  ´   ´  ´ • as-preparedcubic structure • lattice expansion • phase transition ( - ´ )( 26 - 36 mbar ) • reversible  9 M. Suleiman

33. In-situ XRD HASYLAB :  5.4 nm Cluster in H-Atmosphere • * Intensity change • Change in the diffractogramm • Structural change H  M. Suleiman 11

34. 8 10-4 In-situ XRD HAYSLAB: lattice parameter change for different cluster sizes • lattice parameter changes as a function of the H-partial pressure • the lattice parameter change is less than that in the bulk Pd- H system M. Suleiman 13

35. Computed Patterns

36. Clusters Simulation Collaborators: Saja Abdul Hadi Najeh M Jisrawi

37. Surface and Subsurface!

38. Click here for a Movie Saja AbdulHadi et.al.

39. Saja AbdulHadi et.al.

40. Melting Properties Saja AbdulHadi et.al.

41. Saja AbdulHadi et.al.

42. Saja AbdulHadi et.al.

43. Saja AbdulHadi et.al.

44. Melting Movie Movie by: Imad Ladadwa

45. Source: X-ray data booklet: http://xdb.lbl.gov/Section1/Periodic_Table/Pd_Web_data.htm

46. http://xdb.lbl.gov/Section1/Periodic_Table/Nb_Web_data.htm

47. http://xdb.lbl.gov/Section1/Periodic_Table/Y_Web_data.htm