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Design and characterization of nanoparticles and their assemblies: Transmission electron microscopy investigations from atomic to mesoscopic length scales
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
2016 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Transmission electron microscopy (TEM) is a powerful and versatile tool for investigating nanomaterials. In this thesis, various transmission electron microscopy techniques are used to study the chemical and structural features of different types of inorganic nanoparticles of well-defined morphologies as well as their assemblies. The synthesis of spherical and anisotropic nanoparticles (iron oxide nanocubes and other morphologies, gadolinium orthophosphate nanorods, tungsten oxide nanowires and nanorods, palladium nanospheres, and facetted iron-manganese oxides hybrid nanoparticles) using thermal decomposition of metal complex precursors in high-boiling point organic solvents and hydrothermal process are described in details.

Electron diffraction tomography (3D EDT) is a recently developed technique that is used to investigate the 3D structure of crystalline materials. Reciprocal space volume reconstruction of 3D EDT data of thin WO3 nanowires assembled into nanorods revealed single crystal domains of hexagonal symmetry. Moreover, the use of 3D EDT enabled to identify and solve the structures of individual GdPO4 nanorods in a mixed phase powder. The use of 3D EDT was extended using small-angle diffraction mode to investigate the packing arrangements and defects in nanoparticle assemblies. A high concentration of planar defects found in different nanoparticle assemblies highlights the competition between the fcc and hcp arrangements during the assembly process.

Iron-manganese oxides hybrid nanoparticles with different three-dimensional configurations, i.e. core|shell and asymmetric facetted dimers, were investigated using a combination of several electron microscopy techniques (HRTEM, SAED, STEM-HAADF, EFTEM, EELS). The growth of the facetted cubic MnO phase onto preformed Fe3O4 seed particles occurs preferentially along the Fe3O4 nanocube edges forming a well-oriented crystalline interface despite the lattice mismatch and defects. Atomic resolution monitoring of the structural changes in Mn3O4|Fe3O4 and Fe3O4|Mn3O4 core|shell nanoparticles induced by the electron beam revealed a strain relief mechanism at the interface involving inhomogeneous diffusion of cations and defects creation.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University , 2016. , 66 p.
Keyword [en]
nanoparticles, electron microscopy
National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
URN: urn:nbn:se:su:diva-129569ISBN: 978-91-7649-405-9 (print)OAI: oai:DiVA.org:su-129569DiVA: diva2:923226
Public defence
2016-06-02, Magnéli Hall, Arrhenius Laboratory, Svante Arrhenius väg 16 B, Stockholm, 13:00 (English)
Opponent
Supervisors
Funder
Knut and Alice Wallenberg Foundation
Note

At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 4: Manuscript. Paper 5: Manuscript.

Available from: 2016-05-10 Created: 2016-04-25 Last updated: 2017-02-23Bibliographically approved
List of papers
1. WO3 Nanorods Created by Self-Assembly of Highly Crystalline Nanowires under Hydrothermal Conditions
Open this publication in new window or tab >>WO3 Nanorods Created by Self-Assembly of Highly Crystalline Nanowires under Hydrothermal Conditions
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2014 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 30, no 34, 10487-10492 p.Article in journal (Refereed) Published
Abstract [en]

WO3 nanorods and wires were obtained via hydrothermal synthesis using sodium tungstate as a precursor and either oxalic acid, citric acid, or poly(methacrylic add) as a stabilizing agent. Transmission electron microscopy images showed that the organic acids with different numbers of carboxylic groups per molecule influence the final sizes and stacking nanostructures of WO3 wires. Three-dimensional electron diffraction tomography of a single nanocrystal revealed a hexagonal WO3 structure with preferential growth along the c-axis, which was confirmed by high-resolution transmission electron microscopy. WO3 nanowires were also spin-coated onto an indium tin oxide/glass conducting substrate, resulting in the formation of a film that was characterized by scanning electron microscopy. Finally, cyclic voltammetry measurements performed on the WO3 thin film showed voltammograms typical for the WO3 redox process.

National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-107980 (URN)10.1021/la5025907 (DOI)000341230100041 ()
Note

AuthorCount:9;

Available from: 2014-10-09 Created: 2014-10-06 Last updated: 2017-12-05Bibliographically approved
2. Phase Identification and Structure Solution by Three-Dimensional Electron Diffraction Tomography: Gd-Phosphate Nanorods
Open this publication in new window or tab >>Phase Identification and Structure Solution by Three-Dimensional Electron Diffraction Tomography: Gd-Phosphate Nanorods
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2014 (English)In: Inorganic Chemistry, ISSN 0020-1669, E-ISSN 1520-510X, Vol. 53, no 10, 5067-5072 p.Article in journal (Refereed) Published
Abstract [en]

Hydrothermal synthesis of GdPO4 in the presence of poly(methacrylic acid) yields nanorods with a diameter of 15 nm and an aspect ratio of 20. Powder X-ray diffraction patterns showed that the GdPO4 nanorods display peaks characteristics for both monoclinic and hexagonal structures. Three-dimensional electron diffraction tomography (3D EDT) was used to determine the structures ab initio on the basis of reciprocal volume reconstruction of electron diffraction data sets collected from single nanorods. The crystal structure of the monoclinic form was shown to be P2(1)/n, corroborating previous work. We were able to solve the 3D structure of the hexagonal P6(2)22 form, which has not been reported previously. Our work shows that 3D EDT is a powerful method that can be used for solving structures of single nano crystals.

National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-105199 (URN)10.1021/ic500056r (DOI)000336240400033 ()
Funder
Swedish Research CouncilKnut and Alice Wallenberg Foundation
Note

AuthorCount:6;

Available from: 2014-07-04 Created: 2014-06-24 Last updated: 2017-12-05Bibliographically approved
3. Probing planar defects in nanoparticle superlattices by 3D small-angle electron diffraction tomography and real space imaging
Open this publication in new window or tab >>Probing planar defects in nanoparticle superlattices by 3D small-angle electron diffraction tomography and real space imaging
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2014 (English)In: Nanoscale, ISSN 2040-3364, E-ISSN 2040-3372, Vol. 6, no 22, 13803-13808 p.Article in journal (Refereed) Published
Abstract [en]

We demonstrate how the acquisition and processing of 3D electron diffraction data can be extended to characterize structural features on the mesoscale, and show how lattice distortions in superlattices of self-assembled spherical Pd nanoparticles can be quantified by three-dimensional small-angle electron diffraction tomography (3D SA-EDT). Transmission electron microscopy real space imaging and 3D SA-EDT reveal a high density of stacking faults that was related to a competition between fcc and hcp arrangements during assembly. Information on the orientation of the stacking faults was used to make analogies between planar defects in the superlattices and Shockley partial dislocations in metallic systems.

National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-129567 (URN)10.1039/C4NR04156A (DOI)000344836800063 ()
Funder
Knut and Alice Wallenberg Foundation
Available from: 2016-04-25 Created: 2016-04-25 Last updated: 2017-11-30Bibliographically approved
4. Strain and defects in asymmetric Fe-Mn oxides hybrid nanoparticles
Open this publication in new window or tab >>Strain and defects in asymmetric Fe-Mn oxides hybrid nanoparticles
(English)Manuscript (preprint) (Other academic)
National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-129565 (URN)
Available from: 2016-04-25 Created: 2016-04-25 Last updated: 2016-04-26Bibliographically approved
5. Probing the metastability of core|shell nanoparticle systems at atomic resolution
Open this publication in new window or tab >>Probing the metastability of core|shell nanoparticle systems at atomic resolution
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(English)Manuscript (preprint) (Other academic)
National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-129564 (URN)
Available from: 2016-04-25 Created: 2016-04-25 Last updated: 2016-06-22Bibliographically approved

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