Synthesis of CdS nanocrystals in polymeric films studied by in-situ GID and GISAXS

ABSTRACTIn this work, we describe the synthesis of CdS nanocrystals in thin polymeric films by in-situ Grazing Incidence Diffraction (GID) and Grazing Incidence Small Angle Scattering (GISAXS). The 2D GISAXS patterns indicate how the precursor structure is altered as the temperature is varied from 25°C to 300°C. At 150°C, the CdS nanocrystals start to arrange themselves in a hexagonal lattice with a lattice parameter of 27 Å. The diffraction intensity from the hexagonal lattice reaches a maximum at 170°C and decreases steadily upon further heating above 220°C indicating loss of symmetry. Correspondingly, the GID scans at 170°C show strong crystalline peaks from cubic CdS nanocrystals that are about 2 nm size. The results indicate that a temperature of 170°C is sufficient to synthesize CdS nanocrystals without degradation of the polymer matrix (Topas) in thin films (about 30nm).

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In-situ GISAXS on Nanocomposite Films of CdS Nanoparticles and Polymers

MRS Proceedings ◽

10.1557/proc-1027-d05-02 ◽

2007 ◽

Vol 1027 ◽

Author(s):

Tiziana Di Luccio ◽

Dina Carbone ◽

Anna Maria Laera ◽

Katrin Peeper ◽

Christian Mauser ◽

...

Keyword(s):

Polymer Films ◽

Grazing Incidence ◽

Nanocomposite Films ◽

Ex Situ ◽

Cds Nanoparticles ◽

Precursor Polymer ◽

X Ray Scattering ◽

Angle Scattering ◽

Precursor Structure

AbstractWe investigated the growth of CdS nanoparticles in polymer films by means of ex-situ and in-situ x-ray scattering experiments using synchrotron radiation. The CdS nanoparticles were synthesized by thermal decomposition of a Cd thiolate precursor dispersed in a cyclic olefin copolymer. The films were deposited by spin coating. Grazing incidence diffraction (GID) reveals the Bragg reflections of the CdS nanoparticles. In-situ diffraction and grazing incidence small angle scattering (GISAXS) experiments were recorded during the thermal treatment of the precursor/polymer films from room temperature up to 250°C. The diffraction curves show that the initial precursor structure is soon lost at 100°C. Correspondingly, the GISAXS data show a peak at a momentum transfer value q ∼ 0.2Å−1 that shifts towards smaller values with the temperature. Under UV excitation the films show photoluminescence in the range 400 – 700 nm.

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In Situ Grazing‐Incidence Wide‐Angle Scattering Reveals Mechanisms for Phase Distribution and Disorientation in 2D Halide Perovskite Films

Advanced Materials ◽

10.1002/adma.202002812 ◽

2020 ◽

Vol 32 (33) ◽

pp. 2002812 ◽

Cited By ~ 4

Author(s):

Justin M. Hoffman ◽

Joseph Strzalka ◽

Nathan C. Flanders ◽

Ido Hadar ◽

Shelby A. Cuthriell ◽

...

Keyword(s):

Phase Distribution ◽

Grazing Incidence ◽

Wide Angle ◽

Angle Scattering ◽

Halide Perovskite

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In-situ X-ray Measurements of the Initial Epitaxy of Fe(001) Films on MgO(001)

MRS Proceedings ◽

10.1557/proc-280-441 ◽

1992 ◽

Vol 280 ◽

Author(s):

Bruce M. Lairson ◽

A. P. Payne ◽

S. Brennan ◽

N. M. Rensing ◽

B. J. Daniels ◽

...

Keyword(s):

Elasticity Theory ◽

Grazing Incidence ◽

Lattice Parameter ◽

X Ray ◽

X Ray Scattering ◽

Monolayer Coverage ◽

Continuum Elasticity ◽

Ray Scattering

ABSTRACTWe have studied die evolution of the lattice parameter of epitaxial Fe(001) on MgO(001) vs. thickness between 1 and 200 monolayers using Grazing Incidence X-ray Scattering. We show that an interaction exists between the islanded film and the substrate, which allows the film to be incommensurate, even when the islands are too small to allow full dislocations to exist. For the conditions studied, the Fe lattice parameter increases toward the MgO lattice parameter with increasing thickness in the 1–10 monolayer coverage regime, and then relaxes back toward the bulk Fe lattice parameter at greater thicknesses. We employ a model for the interaction between film islands and the substrate which explains large changes in the lattice parameter of the Fe in the 1–10 monolayer thickness range. Relaxation at larger thicknesses is described by continuum elasticity theory.

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Strain and Shape in Self-Assembled Quantum Dots Studied by X-Ray Grazing Incidence Diffraction

MRS Proceedings ◽

10.1557/proc-524-89 ◽

1998 ◽

Vol 524 ◽

Author(s):

I. Kegel ◽

T. H. Metzger ◽

J. Peisl ◽

P. Fratzl ◽

A. Lorke ◽

...

Keyword(s):

Quantum Dots ◽

Grazing Incidence ◽

Lattice Parameter ◽

Reciprocal Space Mapping ◽

X Ray ◽

Surface Reflection ◽

Grazing Incidence Diffraction ◽

Shape Effects ◽

Outer Perimeter ◽

Highly Strained

ABSTRACTWe have developed a method to determine the relationship between strain and lateral size of coherent self-organized quantum dots. In our approach, X-ray grazing incidence diffraction is used to collect information on strain and shape effects in the vicinity of a prominent surface reflection. We demonstrate that for highly strained nano-scale islands it is possible to separate strain-induced and form factor-induced scattering without comparing different reflections. Experimental data from InAs on GaAs(100) quantum dots is discussed with respect to this model. Reciprocal space mapping around the (220) surface reflection shows a linear relationship between relaxation from the substrate lattice parameter and the outer perimeter of the dot. In addition, the functional form of the gradient of relaxation is found to be nonmonotonous and rapidly increasing towards the tip of the dot.

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Structure of the Near-Surface Waveguide Layers Produced by Diffusion of Titanium in Lithium Niobate

MRS Proceedings ◽

10.1557/proc-590-213 ◽

1999 ◽

Vol 590 ◽

Author(s):

Y. Avrahami ◽

E. Zolotoyabko ◽

W. Sauer ◽

T. H. Metzger ◽

J. Peisl

Keyword(s):

Thin Film ◽

Lithium Niobate ◽

Grazing Incidence ◽

Lattice Parameter ◽

High Temperature Phase ◽

Temperature Phase ◽

Near Surface ◽

Structural Modifications ◽

Grazing Incidence Diffraction ◽

Surface Waveguide

ABSTRACTTitanium-induced structural modifications in thin waveguide layers of lithium niobate have been investigated by grazing incidence diffraction and complementary thin film techniques. The study was focused on the high-temperature phase transformation in this system and its influence on the lattice parameter changes, depending on the annealing time.

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In situmonitoring by synchrotron radiation of the formation of ZnO nanoparticles by aqueous chemical growth

Journal of Applied Crystallography ◽

10.1107/s0021889809023310 ◽

2009 ◽

Vol 42 (5) ◽

pp. 815-819 ◽

Cited By ~ 4

Author(s):

S. Fall ◽

O. Konovalov ◽

M. Maaza ◽

A. C. Beye ◽

A. Gibaud

Keyword(s):

Synchrotron Radiation ◽

Zno Nanoparticles ◽

Grazing Incidence ◽

Hexagonal Structure ◽

Growth Technique ◽

Grazing Incidence Diffraction ◽

Aqueous Chemical Growth ◽

Cell Scattering ◽

First Results

Synchrotron radiation experiments were carried out during thein situgrowth of ZnO nanoparticles by the aqueous chemical growth technique. The first results of this exploratoryin situgrazing-incidence diffraction (GID) experiment are reported, with emphasis on the difficulties encountered. In particular, it is shown that, whenin situGID experiments are carried out in a 25 mm-long cell, scattering by the solvent dominates. This impedes the observation of the formation of ZnO nanoparticles during the early stages of the growth process. Nevertheless, it is clearly shown that the wurzite hexagonal structure is present in the solution. At a specific concentration, it is shown how the peak intensities and widths of the Bragg peaks evolve as a function of time.

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High-Resolution Lattice Parameter Measurement by X-Ray Grazing Incidence Diffraction

phys stat sol (a) ◽

10.1002/(sici)1521-396x(199908)174:2<395::aid-pssa395>3.0.co;2-# ◽

1999 ◽

Vol 174 (2) ◽

pp. 395-402

Author(s):

T. H. Metzger ◽

U. Pietsch ◽

E. Gartstein

Keyword(s):

High Resolution ◽

Grazing Incidence ◽

Lattice Parameter ◽

Parameter Measurement ◽

Lattice Parameter Measurement ◽

X Ray ◽

Grazing Incidence Diffraction

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Full reciprocal-space mapping up to 2000 K under controlled atmosphere: the multipurpose QMAX furnace

Journal of Applied Crystallography ◽

10.1107/s160057672000432x ◽

2020 ◽

Vol 53 (3) ◽

pp. 650-661

Author(s):

René Guinebretière ◽

Stephan Arnaud ◽

Nils Blanc ◽

Nathalie Boudet ◽

Elsa Thune ◽

...

Keyword(s):

Strain Relaxation ◽

Structural Phase ◽

Grazing Incidence ◽

Sample Surface ◽

Space Mapping ◽

Reciprocal Space ◽

Reciprocal Space Mapping ◽

Time Resolved ◽

Angle Scattering

A furnace that covers the temperature range from room temperature up to 2000 K has been designed, built and implemented on the D2AM beamline at the ESRF. The QMAX furnace is devoted to the full exploration of the reciprocal hemispace located above the sample surface. It is well suited for symmetric and asymmetric 3D reciprocal space mapping. Owing to the hemispherical design of the furnace, 3D grazing-incidence small- and wide-angle scattering and diffraction measurements are possible. Inert and reactive experiments can be performed at atmospheric pressure under controlled gas flux. It is demonstrated that the QMAX furnace allows monitoring of structural phase transitions as well as microstructural evolution at the nanoscale, such as self-organization processes, crystal growth and strain relaxation. A time-resolved in situ oxidation experiment illustrates the capability to probe the high-temperature reactivity of materials.

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Grazing exit small angle X-ray scattering on grain formation in polycrystalline metal films

Zeitschrift für Kristallographie - Crystalline Materials ◽

10.1524/zkri.2007.222.11.601 ◽

2007 ◽

Vol 222 (11/2007) ◽

Cited By ~ 2

Author(s):

Wei Zhang ◽

Ian K. Robinson

Keyword(s):

Thin Film ◽

Small Angle ◽

Ostwald Ripening ◽

Grazing Incidence ◽

Metal Films ◽

Nanostructured Thin Film ◽

X Ray Scattering ◽

Angle Scattering ◽

In Situ Diffraction

We recently proposed a new grazing exit geometry for measuring the small-angle scattering from thin film materials, which we call GESAXS, to contrast with the successful grazing incidence version, GISAXS. The technique is particularly useful for probing nanostructured thin film materials, especially when the coherence properties of the beam are employed. Here we demonstrate the application of GESAXS to evaporated metal films, prepared using an in-situ diffraction chamber, to investigate how their structure evolves upon annealing. Contrasting behavior is seen for Au, which preserves a roughly exponential distribution of domain sizes, and Fe for which the size distribution narrows by an Ostwald ripening process.

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