scholarly journals Silica-Polystyrene Nanocomposite Particles Synthesized by Nitroxide-Mediated Polymerization and Their Encapsulation through Miniemulsion Polymerization

2006 ◽  
Vol 2006 ◽  
pp. 1-10 ◽  
Author(s):  
Bérangère Bailly ◽  
Anne-Carole Donnenwirth ◽  
Christèle Bartholome ◽  
Emmanuel Beyou ◽  
Elodie Bourgeat-Lami
Keyword(s):  
Silica Nanoparticles ◽  
Functional Group ◽  
Silica Surface ◽  
Miniemulsion Polymerization ◽  
Molecular Weights ◽  
Transmission Electron ◽  
Shell Particles ◽  
Terminal Functional Group ◽  
Nitroxide Mediated Polymerization

Polystyrene (PS) chains with molecular weights comprised between 8000 and 64000g⋅mol-1and narrow polydispersities were grown from the surface of silica nanoparticles (Aerosil A200 fumed silica and Stöber silica, resp.) through nitroxide-mediated polymerization (NMP). Alkoxyamine initiators based on N-tert-butyl-1-diethylphosphono-2,2-dimethylpropyl nitroxide (DEPN) and carrying a terminal functional group have been synthesized in situ and grafted to the silica surface. The resulting grafted alkoxyamines have been employed to initiate the growth of polystyrene chains from the inorganic surface. The maximum grafting density of the surface-tethered PS chains was estimated and seemed to be limited by initiator confinement at the interface. Then, the PS-grafted Stöber silica nanoparticles were entrapped inside latex particles via miniemulsion polymerization. Transmission electron microscopy indicated the successful formation of silica-polystyrene core-shell particles.

Nitroxide-Mediated Polymerization of Styrene Initiated from the Surface of Silica Nanoparticles. In Situ Generation and Grafting of Alkoxyamine Initiators

2005 ◽  
Vol 38 (4) ◽  
pp. 1099-1106 ◽  
Author(s):  
C. Bartholome ◽  
E. Beyou ◽  
E. Bourgeat-Lami ◽  
P. Chaumont ◽  
F. Lefebvre ◽  
...  
Keyword(s):  
Silica Nanoparticles ◽  
In Situ Generation ◽  
Nitroxide Mediated Polymerization

Grafting of Polymers to Solid Surfaces by using Immobilized Azoinitiators

1993 ◽  
Vol 304 ◽  
Author(s):  
O. Prucker ◽  
J. Rühe
Keyword(s):  
Diffuse Reflectance ◽  
Functional Group ◽  
Solid Surfaces ◽  
Covalent Attachment ◽  
Head Group ◽  
Radical Chain ◽  
Molecular Weights ◽  
Transmission Electron ◽  
Covalently Bonded ◽  
Reflectance Ftir

AbstractThe covalent attachment of polymers such as polystyrene, polymethylmethacrylate and polyacrylonitrile to microparticulate silica and to silicon wafers through immobilized radical chain initiators (especially azocompounds) is described. The initiator is bonded to the surface using α,ω-substituted silanes, which have only one functional group at the silane head group.Up to 10 g of polymer per g of silica could be covalently bonded to the surface. The attached monolayers were characterized using diffuse reflectance FTIR spectroscopy, XPS and elemental analysis. After the cleaving off of the attached layers molecular weights up to 300.000 g/mol were measured. Transmission electron micrographs generated with an element specific imaging technique (ESI) clearly show a continuous, about 10 nm thick, polymer layer around the silica particles.

Spherical Glycopolymer Architectures using RAFT: From Stars with a ?-Cyclodextrin Core to Thermoresponsive Core–Shell Particles

2009 ◽  
Vol 62 (8) ◽  
pp. 813 ◽  
Author(s):  
Ling Zhang ◽  
Martina H. Stenzel
Keyword(s):  
Raft Polymerization ◽  
Chain Extension ◽  
Solution Temperature ◽  
Core Shell ◽  
Molecular Weights ◽  
Transmission Electron ◽  
Reversible Addition ◽  
Shell Particles ◽  
Surface Tensiometry ◽  
Block Structures

Glycopolymers with a seven-arm star architectures based on a β-cyclodextrin core (β-CD-RAFT) were successfully prepared using reversible addition–fragmentation chain transfer (RAFT) polymerization. A bimodal molecular weight distribution was observed in the early stages of the polymerization. At monomer conversions of N-acryloyl glucose (AGA) above 10% the polymerization proceeded according to a living behaviour and molecular weights of more than 200000 g mol–1 were obtained. However, the resulting star polymers did not undergo well-controlled chain extension with N-isopropyl acrylamide (NIPAAm) and the formation of block structures in each arm was prevented. Alternatively, the arm-first technique was employed. Block copolymers based on AGA and PNIPAAm were self-assembled into micelles at a solution temperature above the lower critical solution temperature. Subsequent core-crosslinking with hexan-1,6-diol diacrylate resulted in unimolecular micelles with thermoresponsive properties. Dynamic light scattering studies, surface tensiometry, and transmission electron microscopy confirmed the formation of core–shell particles.

scholarly journals Magnetic Behaviour of Mn12-Stearate Single-Molecule Magnets Immobilized on the Surface of 300 nm Spherical Silica Nanoparticles

Materials ◽  
2020 ◽  
Vol 13 (11) ◽  
pp. 2624 ◽  
Author(s):  
Magdalena Laskowska ◽  
Oleksandr Pastukh ◽  
Piotr Konieczny ◽  
Mateusz Dulski ◽  
Marcin Zalsiński ◽  
...  
Keyword(s):  
Silica Nanoparticles ◽  
Single Molecule ◽  
Silica Surface ◽  
Magnetic Measurements ◽  
Magnetic Behaviour ◽  
Silica Spheres ◽  
Squid Magnetometry ◽  
Single Molecule Magnets ◽  
Transmission Electron ◽  
Spherical Silica

The magnetic behaviour of Mn 12 -stearate single-molecule magnets (SMMs) ([ Mn 12 O 12 ( CH 3 ( CH 2 ) 16 CO 2 ) 16 ] · 2 CH 3 COOH · 4 H 2 O ) on the surface of 300 nm spherical silica nanoparticles were investigated. The SMMs were bonded at the silica surface with the assumed number of anchoring points, which influenced on their degree of freedom and distribution. In order to check the properties of Mn 12 -stearate molecules separated on the silica surface, and check their interactions, the samples containing four different concentration of spacers per single anchoring unit and variously bonded Mn 12 -stearate particles were prepared. The materials have been examined using Raman spectroscopy, transmission electron microscopy, and SQUID magnetometry. The results of magnetic measurements showed a correlation between the way of single-molecule magnets immobilization onto the silica spheres and the magnetic properties of the obtained hybrid materials.

The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
Author(s):  
R. E. Herfert
Keyword(s):  
Surface Characterization ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Depth Of Penetration ◽  
X Ray ◽  
The Past ◽  
Transmission Electron ◽  
Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

Transmission Electron Microscopy of Protein Macromolecules

1971 ◽  
Vol 29 ◽  
pp. 424-425
Author(s):  
Henry S. Slayter
Keyword(s):  
Biological Systems ◽  
Metal Vapor ◽  
Resolving Power ◽  
Electron Microscopic ◽  
Chemical Methods ◽  
Molecular Weights ◽  
The Past ◽  
Physical Chemical ◽  
Transmission Electron

Electron microscopic methods have been applied increasingly during the past fifteen years, to problems in structural molecular biology. Used in conjunction with physical chemical methods and/or Fourier methods of analysis, they constitute powerful tools for determining sizes, shapes and modes of aggregation of biopolymers with molecular weights greater than 50, 000. However, the application of the e.m. to the determination of very fine structure approaching the limit of instrumental resolving power in biological systems has not been productive, due to various difficulties such as the destructive effects of dehydration, damage to the specimen by the electron beam, and lack of adequate and specific contrast. One of the most satisfactory methods for contrasting individual macromolecules involves the deposition of heavy metal vapor upon the specimen. We have investigated this process, and present here what we believe to be the more important considerations for optimizing it. Results of the application of these methods to several biological systems including muscle proteins, fibrinogen, ribosomes and chromatin will be discussed.

In situ REM imaging of surface processes on ceramic bulk crystals from 300 to 1670 K in a conventional TEM

1991 ◽  
Vol 49 ◽  
pp. 660-661
Author(s):  
Z. L. Wang ◽  
J. Bentley
Keyword(s):  
High Temperatures ◽  
Image Resolution ◽  
Atomic Processes ◽  
Crystal Surfaces ◽  
Beam Radiation ◽  
Surface Areas ◽  
Transmission Electron ◽  
Reflection Electron Microscopy ◽  
Gas Reactions

Studying the behavior of surfaces at high temperatures is of great importance for understanding the properties of ceramics and associated surface-gas reactions. Atomic processes occurring on bulk crystal surfaces at high temperatures can be recorded by reflection electron microscopy (REM) in a conventional transmission electron microscope (TEM) with relatively high resolution, because REM is especially sensitive to atomic-height steps.Improved REM image resolution with a FEG: Cleaved surfaces of a-alumina (012) exhibit atomic flatness with steps of height about 5 Å, determined by reference to a screw (or near screw) dislocation with a presumed Burgers vector of b = (1/3)<012> (see Fig. 1). Steps of heights less than about 0.8 Å can be clearly resolved only with a field emission gun (FEG) (Fig. 2). The small steps are formed by the surface oscillating between the closely packed O and Al stacking layers. The bands of dark contrast (Fig. 2b) are the result of beam radiation damage to surface areas initially terminated with O ions.

Role of boundaries in the crystallization of amorphous films

1988 ◽  
Vol 46 ◽  
pp. 626-627
Author(s):  
D. A. Smith
Keyword(s):  
Low Temperature ◽  
Amorphous State ◽  
Nucleation And Growth ◽  
Amorphous Films ◽  
Island Nucleation ◽  
Surface Steps ◽  
Transmission Electron ◽  
Component Systems ◽  
Temperature Deposition

The nucleation and growth processes which lead to the formation of a thin film are particularly amenable to investigation by transmission electron microscopy either in situ or subsequent to deposition. In situ studies have enabled the observation of island nucleation and growth, together with addition of atoms to surface steps. This paper is concerned with post-deposition crystallization of amorphous alloys. It will be argued that the processes occurring during low temperature deposition of one component systems are related but the evidence is mainly indirect. Amorphous films result when the deposition conditions such as low temperature or the presence of impurities (intentional or unintentional) preclude the atomic mobility necessary for crystallization. Representative examples of this behavior are CVD silicon grown below about 670°C, metalloids, such as antimony deposited at room temperature, binary alloys or compounds such as Cu-Ag or Cr O2, respectively. Elemental metals are not stable in the amorphous state.

In situ observations of electromigration induced void behavior

1995 ◽  
Vol 53 ◽  
pp. 244-245
Author(s):  
T. Marieb ◽  
J. C. Bravman ◽  
P. Flinn ◽  
D. Gardner ◽  
M. Madden
Keyword(s):  
Electron Microscopy ◽  
Void Nucleation ◽  
Plan View ◽  
Transmission Electron ◽  
Nucleation Sites ◽  
Microelectronics Industry ◽  
In Situ Observations ◽  
Backscatter Electron Detector ◽  
Voltage Scanning

Electromigration and stress voiding have been active areas of research in the microelectronics industry for many years. While accelerated testing of these phenomena has been performed for the last 25 years[1-2], only recently has the introduction of high voltage scanning electron microscopy (HVSEM) made possible in situ testing of realistic, passivated, full thickness samples at high resolution.With a combination of in situ HVSEM and post-testing transmission electron microscopy (TEM) , electromigration void nucleation sites in both normal polycrystalline and near-bamboo pure Al were investigated. The effect of the microstructure of the lines on the void motion was also studied.The HVSEM used was a slightly modified JEOL 1200 EX II scanning TEM with a backscatter electron detector placed above the sample[3]. To observe electromigration in situ the sample was heated and the line had current supplied to it to accelerate the voiding process. After testing lines were prepared for TEM by employing the plan-view wedge technique [6].

A TEM study of the microstructure of avian eggshells

1992 ◽  
Vol 50 (2) ◽  
pp. 1102-1103
Author(s):  
S. Q. Xiao ◽  
S. Baden ◽  
A. H. Heuer
Keyword(s):  
Electron Microscope ◽  
Calcium Carbonate ◽  
Nucleation And Growth ◽  
Growth Mechanisms ◽  
Shell Surface ◽  
Thin Sections ◽  
Polycrystalline Metals ◽  
Transmission Electron ◽  
Nucleation And Growth Mechanisms

The avian eggshell is one of the most rapidly mineralizing biological systems known. In situ, 5g of calcium carbonate are crystallized in less than 20 hrs to fabricate the shell. Although there have been much work about the formation of eggshells, controversy about the nucleation and growth mechanisms of the calcite crystals, and their texture in the eggshell, still remain unclear. In this report the microstructure and microchemistry of avian eggshells have been analyzed using transmission electron microscope (TEM) and energy dispersive spectroscopy (EDS).Fresh white and dry brown eggshells were broken and fixed in Karnosky's fixative (kaltitanden) for 2 hrs, then rinsed in distilled H2O. Small speckles of the eggshells were embedded in Spurr medium and thin sections were made ultramicrotome.The crystalline part of eggshells are composed of many small plate-like calcite grains, whose plate normals are approximately parallel to the shell surface. The sizes of the grains are about 0.3×0.3×1 μm3 (Fig.l). These grains are not as closely packed as man-made polycrystalline metals and ceramics, and small gaps between adjacent grains are visible indicating the absence of conventional grain boundaries.

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