Self-Assembled Iron Oxide Thin Films at the Liquid-Air Interface

Transcription

1 Self-Assembled Iron Oxide Thin Films at the Liquid-Air Interface Leandra Boucheron Candidacy Exam September 4, 2013

2 Introduction Outline Techniques and Results Grazing Incidence Diffraction (GID) X-Ray Photon Correlation Spectroscopy (XPCS) X-Ray Reflectivity (XR) and Grazing Incidence X- Ray Off-Specular (GIXOS) Future Work Magnetic Effects X-Ray Coherent Diffractive Imaging (CXDI)

3 Introduction Outline Techniques and Results Grazing Incidence Diffraction (GID) X-Ray Photon Correlation Spectroscopy (XPCS) X-Ray Reflectivity (XR) and Grazing Incidence X- Ray Off-Specular (GIXOS) Future Work Magnetic Effects X-Ray Coherent Diffractive Imaging (CXDI)

4 Introduction You do not really understand something unless you can explain it to your grandmother. Leandra, a lot of things are nanotechnology. Tennis balls are nanotechnology. Even humans are nanotechnology! 1. Explain it to my committee 2. Explain it to my grandmother

5 Ways to Look at Small Things Optical Microscopy >100nm Scanning Electron Microscopy >1nm Diffraction Limit d~λ Transmission Electron Microscopy >1Å De Broglie Wavelength λ = h p

6 Wavelength (10pm-10nm) Penetrating Non-Invasive Global, Statistical Information In situ Studies Surface Sensitivity (GID) Coherence (XPCS) Why X-Rays?

7 Interfacial Structures Optical Coatings Flexible Electronics Biomembranes 10nm iron oxide nanoparticle film during compression on liquid surface 60 m Singer, S. J., & Nicolson, G. L. (1972). Science, 175(23) There s no point in researching graphene any more, because the Nobel prize has already been awarded. O.S.

8 Liquid Surface Self Assembly 5-20nm iron oxide core Van der Waals Force Interfacial Forces Magnetic Interactions Electric Interactions 2nm oleic acid tails Nie, Z., Petukhova, A., & Kumacheva, E. (2010). Nature nanotechnology, 5(1)

9 Langmuir-Blodgett Trough chloroform pure water pressure sensor

10 Isotherms 60µm solid liquid gas 60µm

11 The Macroscopic Picture 20nm particles, Π~5mN/m 20nm particles, Π~15mN/m 20nm particles, Π~40mN/m 60µm 60µm 5nm particles, Π~40mN/m 60µm 60µm

12 Introduction Outline Techniques and Results Grazing Incidence Diffraction (GID) X-Ray Photon Correlation Spectroscopy (XPCS) X-Ray Reflectivity (XR) and Grazing Incidence X- Ray Off-Specular (GIXOS) Future Work Magnetic Effects X-Ray Coherent Diffractive Imaging (CXDI)

13 Full Characterization of Films In-Plane Structure Grazing Incidence Diffraction (GID) In-Plane Dynamics X-Ray Photon Correlation Spectroscopy (XPCS) Out-of-Plane Structure X-Ray Reflectivity (XR) and Grazing Incidence X- Ray Off-Specular (GIXOS)

14 Introduction Outline Techniques and Results Grazing Incidence Diffraction (GID) X-Ray Photon Correlation Spectroscopy (XPCS) X-Ray Reflectivity (XR) and Grazing Incidence X- Ray Off-Specular (GIXOS) Future Work Magnetic Effects X-Ray Coherent Diffractive Imaging (CXDI)

15 Grazing Incidence Diffraction (GID) ~1Å ~10nm ~0.3 n = 2d sin θ q z q x q a = 2π λ sin θ a 2 β θ ~ 0.3 α z α,β θ y x

16 General Liquid Surface Beamline Large Angular Range Experimental Location

17 Preservation of Structure

18 Preservation of Structure

19 GID During Film Compression 2Å

20 GID During Film Compression 2Å

21 GID During Film Compression 2Å

22 Particle Size Mixtures Mixing Partial Segregation

23 Particle Size Mixtures Mixing Partial Segregation

24 Continued Work Relate GID Peak Shifts to Particle Dynamics (XPCS) How is In-Plane Spacing Affected by Multilayer Formation?

25 Introduction Outline Techniques and Results Grazing Incidence Diffraction (GID) X-Ray Photon Correlation Spectroscopy (XPCS) X-Ray Reflectivity (XR) and Grazing Incidence X- Ray Off-Specular (GIXOS) Future Work Magnetic Effects X-Ray Coherent Diffractive Imaging (CXDI)

26 Leheny, R.L. (2012). Current Opinion in Colloid & Interface Science, 17(1) Coherent Speckle

27 Dynamic Light Scattering Wrong Length Scale Difficult to Couple

28 X-Ray Photon Correlation Spectroscopy (XPCS) β θ t o +3Δt t o +2Δt t o +Δt t o α z y x

29 Interparticle Dynamics g 2 Δt = I t I(t + Δt) t I(t) t 2 g 2 t = 1 + β[g 1 t ] 2 t o +2Δt t o +3Δt t o +Δt t o Brownian Motion g 2 ~ e 2t τ

30 Experimental Location Beam Coherence Better Angular Resolution

31 Glassy or Jammed State Inhomogeneous Dynamics Stretched Exponential (Kohlrausch- Williams-Watts) Isotherm Compression at constant speed Relaxation at constant area Single Exponential (non-glassy) Stretched Exponential (glassy) g 2 e t τ g 2 e t τ α Williams, G., & Watts, D.C. (1970). Transactions of the Faraday Society, 66

32 Glassy or Jammed State Inhomogeneous Dynamics Stretched Exponential (Kohlrausch- Williams-Watts) Isotherm Single Exponential (non-glassy) Stretched Exponential (glassy) g 2 e t τ g 2 e t τ α Williams, G., & Watts, D.C. (1970). Transactions of the Faraday Society, 66

33 Glassy or Jammed State Inhomogeneous Dynamics Stretched Exponential (Kohlrausch- Williams-Watts) Isotherm Diffraction Pattern Shows Short-Range/Local Ordering Single Exponential (non-glassy) Stretched Exponential (glassy) g 2 e t τ g 2 e t τ α Williams, G., & Watts, D.C. (1970). Transactions of the Faraday Society, 66

34 Viscoelasticity g 2 time Δt 1, Δt 2 = I t + Δt 1 I(t + Δt 2 ) t I(t) 2

35 Timescale-Pressure Dependence τ 30mN/m = 120s τ 40mN/m = 220s

36 ADVANCEMENT Jacob Professor

37 Q-Dependence of Timescale Brownian Motion x 2 = 2Dt x 2 = 2π q 2 t = τ τ = 2π2 q 2 D ln τ = 2 ln q + C

38 Q-Dependence of Timescale Non-Brownian Motion x 2 = 2Dt n x 2 = 2π q 2 t = τ τ = 2π2 q 2 D ln τ = 2 ln q + C n

39 To Be Continued Framework for Stretched Exponential + Anomalous Diffusion Order in Glassy Systems Hydrodynamic Interactions H(q) D ε q S(q) D 0 Kurchan, J., & Levine, D. (2011). Journal of Physics A, 44.

40 Introduction Outline Techniques and Results Grazing Incidence Diffraction (GID) X-Ray Photon Correlation Spectroscopy (XPCS) X-Ray Reflectivity (XR) and Grazing Incidence X- Ray Off-Specular (GIXOS) Future Work Magnetic Effects X-Ray Coherent Diffractive Imaging (CXDI)

41 X-Ray Reflectivity (XR) η η z y x

42 X-Ray Reflectivity (XR) γ Fresnel Reflectivity R q z q c 2q z 4 e iq zz dρ dz dz 2 Surface Structure Factor γ z y x

43 Reflectivity Analysis

44 Grazing Incidence X-Ray Off-Specular (GIXOS) θ 0 Guard Slits α z y x

45 Advantages of GIXOS Faster Data Collection Less Sample Damage No Sample Motion Required Static X-Ray Footprint Dai, Y., et. al. (2011). Journal of Applied Physics, 110.

46 GIXOS During Compression

47 GIXOS During Compression

48 GIXOS During Compression

49 Analyze GIXOS Data Correlate Intensity Drop with GID Signal Continued Work Effect of Compression Speed on Multilayer Formation

50 Introduction Outline Techniques and Results Grazing Incidence Diffraction (GID) X-Ray Photon Correlation Spectroscopy (XPCS) X-Ray Reflectivity (XR) and Grazing Incidence X- Ray Off-Specular (GIXOS) Future Work Magnetic Effects X-Ray Coherent Diffractive Imaging (CXDI)

51 Magnetic Field Application No External Field External Field B B x x+δx Thorek, D.L.J., et. al. (2006). Annals of Biomedical Engineering, 34(1).

52 SEM Measurements Directed Self-Assembly? Field On During Deposition Field Off During Deposition

53 Dynamics Measurements B Kinge, S., Crego-Calama, M., & Reinhoudt, D.N. (2008). ChemPhysChem, 9(1). Cheng, G., et al, (2005). Langmuir 21(26).

54 Introduction Outline Techniques and Results Grazing Incidence Diffraction (GID) X-Ray Photon Correlation Spectroscopy (XPCS) X-Ray Reflectivity (XR) and Grazing Incidence X- Ray Off-Specular (GIXOS) Future Work Magnetic Effects X-Ray Coherent Diffractive Imaging (CXDI)

55 Butterfly Wing Coloration Saranathan, V., et al. (2010). Proceedings of the National Academy of Sciences, 107 (26).

56 X-Ray Coherent Diffractive Imaging (XCDI)

57 X-Ray Coherent Diffractive Imaging (XCDI)

58 Acknowledgements Jacob Stanley Yeling Dai Sean You (U. Chicago) Chris Parzyck Jim Wingert Oleg Shpyrko Binhua Lin (APS/S15/U Chicago) Mati Meron (APS/S15/U Chicago) Zhang Jiang (APS/S8) Suresh Narayanan (APS/S8) Alec Sandy (APS/S8)

59 Thank You!

60 Backup Slides

61 Langmuir-Blodgett Trough

62 Liquid Surface Spectrometer

63 In-Plane Film Structure Nearest Neighbor Spacing 10 1 st 2 nd 3 rd 4 th Hexagonal Close Packed Experiment

64 Radiation Damage hard core soft coating

65 Radiation Damage X-Ray Beam hard core soft coating

66 Radiation Damage

67 Intensity Intensity Radiation Damage GID Peak After Successive 500s Exposures Specular Reflectivity dθ Time (s)