CHE.525 Laboratory Course Technical Chemistry II (CHE.525) Nanostructural characterisation by small-angle X-ray scattering (SAXS)

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1 Meeting point: NTEG250 Stremayrgasse 9 Ground floor, XRD Lab Supervisor: Manfred Kriechbaum manfred.kriechbaum@tugraz.at Institut für Anorganische Chemie Tel: CHE.525 Laboratory Course Technical Chemistry II (CHE.525) Nanostructural characterisation by small-angle X-ray scattering (SAXS) WS 2014/15

2 Objective: To characterize the lattice type and lattice spacing of the nanostructure of the templates and of the deposits on the goldcoated foils by the method of SAXS(small-angle-X-ray scattering). In particular, we will measure the nanostructure of a detergent solution (Brij56, diluted with water 1:1), the Pt and/or Pd template and the deposit on a gold-coated foil and on a solid support in order to investigate the nanostructural alignment on the solid surface.

3 3 What sizes does SAXS probe? SAXS is not a spectroscopic (it is elastic scattering of X-rays) but a direct imaging method in reciprocal space (not in real space like optical microscopy). (D)LS

4 X-ray detector X-ray source sample Illustration of the SAXS method and SAXS camera used in this lab-course (to the right) (SAXSess from A.Paar, Graz)

5 Principle of Small-Angle Scattering: Samples don t have to be necessarily crystalline, but can also be amorphous or liquid solutions. Measured signal: Scattered X-ray intensities at small angles: (2 θ: 0 to ~ 5 10 deg) Isolated nano-particles In solution or in a matrix Amorphous or porous samples (polymers, coal ) Crystals or liquid crsytals 1D-, 2D- or 3D-crystalline samples

6 Size-ranges covered by SAXS (small-angle) and WAXS (wide-angle) λ 0.1 nm X-ray 2θ: 0 5 SAXS Nanosized objects (1-100 nm) 2θ: > 5 Bragg s law: sin θ = λ / 2d WAXS/XPD X-ray powder-diffraction Atomic structure: (1-0.1nm) small θ large θ large d small d

7 7 Real space Reciprocal space

8 8 Relation between scattering angle 2θ(deg) and momentum transfer or magnitude of the scattering vector q ([Å -1 ] or [nm -1 ]) SAXS in transmission mode: 80 k i = k s = 2π/λ q..[å -1 ] or [nm -1 ] d..[å] or [nm] q (1/nm) λ=0.154 nm theta Calibration of the angular scale is usually done with a sample with a precisely known lamellar repeat-spacing, usually silver-behenate: CH 3 -(CH 2 ) 20 -COO-Ag: d = nm

9 9 Lattice type, lattice constants (d) and electron density ρ(r). I(q) D-lamellar d ρ( r z ) d ρ n max ( rz ) = n= 1 F n 2πnr cos d z q D-hexagonal d I(q) 20 SAXS-spectra q I(q) D-cubic q

10 1-D lamellar und 2-D hexagonal lattices and their respective SAXS-patterns a a q1 Equidistant diffraction peaks at: 1, 4, 9, 16, 25,.. a=2*π/q1 q1 Diffraction peaks at: 1, 3, 4, 7, 9,.. a=(2*π/q1)*2/ 3

11 11 GISAXS Illustration by Zhang Jiang (APS) Illustration by Gilles Renaud

12 12 GISAXS Source : Dr. A. Fromsdorf, Univ. Hamburg, D, D.-M. Smilgies, CHESS, Cornell Univ., Ithaka, NY, USA,

13 GISAXS 2. BP Oriented multilayer LS SB 1. BP Isotropic liposome + PB α f Ω- scan α i Information on ordering/orientation and on the lateral nanostructure of surfaces or of thin films.

14 X-Ray Transmission (Absorption) Absorption coefficient depends on the used wavelength! If a thickness d of a sample with the transmission T (0<T<1) is increased by a factor n, the transmission decreases to T n. If the satistics of a SAXS measurements is to be increased by a factor of n, the exposure time t has to be increased by a factor of n 2. Transmission of 1 mm water: at λ= nm: 0.37 I = I 0 *e (-µ*d) I o =intensity without sample µ= mass absorption coefficient d= thickness

15 15 X-Ray Transmission (Absorption) calculated for H 2 0 using X-rays of wavelength λ= nm.

16 16 The following samples will be measured with the SAXSess camera, operating at 2 kw X-ray tube power, using Cu-K α -radiation in the transmission (T) or GI-SAXS-mode. Exposure times will be typically 300 s. Evaluate the lattice type and unit cell-spacing from the SAXS-spectra using the programs SGI (Space Group Indexing) and FIT2D. Sample SAXS-mode Lattice type Unit cell spacing Brij/H 2 O (1:1) Pt-template Pd-template Pt-deposit on foil Pd-deposit on foil Pt-deposit on glass Pd-deposit on glass T T T T T GI GI Remarks

17 Calculate the X-ray transmission (using the utility at the webpage: ) for a 100 µm Mylar foil and for a 0.5 mm thick quartz-glass plate (SiO 2, density 2.2 g/cm 3 ) and also the (total) transmission when coated with a 1 µm Au-film (assuming a density of 19.3 g/cm 3 ) at two different wavelengths: and 0.07 nm, respectively. Which wavelength is better suited for biological and polymer samples (elements mostly C,H,O, N) and which one for metals and alloys? Wavelength(X-rays) Mylar Mylar+Au Glass Glass+Au nm 0.07 nm

18 Books for small-angle scattering (SAS): The SAXS Guide by H.Schnablegger and Y. Singh (2011), A.Paar GmbH (Getting acquainted with the principles) Stribeck N. "X-Ray Scattering of Soft Matter" Springer, Heidelberg (2007)

19 Webresources for small-angle scattering (SAS): SAXS: GISAXS: More SA(X)S-related weblinks:

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