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Loughborough University

1. Holt, James D. Silica attached polymers and ligands for the selective removal of metal ions and radionuclides from aqueous solutions.

Degree: PhD, 2014, Loughborough University

Surface functionalised silica materials have been prepared, followed by the extensive testing of their ability to remove metal ions from aqueous solutions. Modifications include ligand attachment and polymer grafting from the silica surface whilst the metals tested range from first row transition metals right through to the lanthanides and actinides. Characterisation of the materials produced has been of paramount importance for the understanding of the modification process and this is also extensively discussed. Atom transfer radical polymerisation (ATRP) has been used as the primary polymerisation method. Following polymerisation of 2-hydroxyethyl methacrylate (HEMA), post functionalisation was attempted. However, this was found to cause severe cross-linking and all attempts to attach ligands to this failed. Nonetheless, this process was transferred to grafting from silica surfaces and a novel approach to the characterisation of this material was implemented. (3-aminopropyl) triethoxysilane (APTES) was reacted with multiple forms of silica, primarily ZEOprep silica (average particle size 71.48 πm) and fumed silica (0.007 μm). This produced an amine coated surface to which 2-bromoisobutyryl bromide (BIBB) was attached, providing the required surface for radical polymerisation to proceed with a selected monomer. Solid State Nuclear Magnetic Resonance (SSNMR) has been utilised as the major characterisation technique for each step, leading to significant understanding of how this occurs. Thermogravimetric Analysis (TGA) and elemental analysis has supported this method at each stage whilst also enabling one to calculate the moles of APTES present, per gram of APTES-functionalised silica. For the ZEOprep silica this was calculated to be at up to 1.51 x 10-3 mol g-1 and for the fumed silica 1.63 x 10-3 mol g-1. As well as testing the selective nature of these materials, solutions of individual ions and radionuclides were used to measure the effectiveness of the materials for a specific ion. Rd values for these metals ions including solutions of Co(II), Ni(II), Cu(II), Cd2+, Eu(III) and [UO2]2+ have reached values ranging from 7.49 x 104 mL g-1 to as high as 2.17 x 109 mL g-1. These values are regarded as outstanding by other groups that have reported similar results and these are discussed in the report. This range includes values that were observed when competing Na+ and Ca2+ ions were present at 0.5 % and 1 % (w/w). pH testing was also investigated with the materials using a solution of europium ions to determine the most effective range and this was found to fall between pH 4 and 5. X-ray Photoelectron Spectroscopy (XPS) has been utilised to help gain an understanding of the binding between Cu(II) ions and APTES, suggesting that copper ions bind with oxygen atoms closer to the silica surface as well as the nitrogen atoms at the end of the ligand. Meanwhile STEM (Scanning Transmission Electron Microscope) has been used to show how effectively the surface area of the material is used by imaging the europium ions over a…

Subjects/Keywords: 541; Ligand; Polymer; ATRP; SI-ATRP; APTES; PHEMA; PEGMA; PGMA; Surface modification; Silica; Metal ion removal; Radionuclide; Sequestration; Remediation; Characterisation; Solid state NMR; TGA; CHN; XPS; STEM; SEM; TEM; ICP

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APA · Chicago · MLA · Vancouver · CSE | Export to Zotero / EndNote / Reference Manager

APA (6th Edition):

Holt, J. D. (2014). Silica attached polymers and ligands for the selective removal of metal ions and radionuclides from aqueous solutions. (Doctoral Dissertation). Loughborough University. Retrieved from http://hdl.handle.net/2134/16253

Chicago Manual of Style (16th Edition):

Holt, James D. “Silica attached polymers and ligands for the selective removal of metal ions and radionuclides from aqueous solutions.” 2014. Doctoral Dissertation, Loughborough University. Accessed October 24, 2020. http://hdl.handle.net/2134/16253.

MLA Handbook (7th Edition):

Holt, James D. “Silica attached polymers and ligands for the selective removal of metal ions and radionuclides from aqueous solutions.” 2014. Web. 24 Oct 2020.

Vancouver:

Holt JD. Silica attached polymers and ligands for the selective removal of metal ions and radionuclides from aqueous solutions. [Internet] [Doctoral dissertation]. Loughborough University; 2014. [cited 2020 Oct 24]. Available from: http://hdl.handle.net/2134/16253.

Council of Science Editors:

Holt JD. Silica attached polymers and ligands for the selective removal of metal ions and radionuclides from aqueous solutions. [Doctoral Dissertation]. Loughborough University; 2014. Available from: http://hdl.handle.net/2134/16253

2. Galabura, Yuriy. SYNTHESIS AND CHARACTERIZATION OF NANOSCALE POLYMER FILMS GRAFTED TO METAL SURFACES.

Degree: PhD, Materials Science and Engineering, 2014, Clemson University

Anchoring thin polymer films to metal surfaces allows us to alter, tune, and control their biocompatibility, lubrication, friction, wettability, and adhesion, while the unique properties of the underlying metallic substrates, such as magnetism and electrical conductivity, remain unaltered. This polymer/metal synergy creates significant opportunities to develop new hybrid platforms for a number of devices, actuators, and sensors. This present work focused on the synthesis and characterization of polymer layers grafted to the surface of metal objects. We report the development of a novel method for surface functionalization of arrays of high aspect ratio nickel nanowires/micronails. The polymer 'grafting to' technique offers the possibility to functionalize different segments of the nickel nanowires/micronails with polymer layers that possess antagonistic (hydrophobic/hydrophilic) properties. This method results in the synthesis of arrays of Ni nanowires and micronails, where the tips modified with hydrophobic layer (polystyrene) and the bottom portions with a hydrophilic layer (polyacrylic acid). The developed modification platform will enable the fabrication of switchable field-controlled devices (actuators). Specifically, the application of an external magnetic field and the bending deformation of the nickel nanowires and micronails will make initially hydrophobic surface more hydrophilic by exposing different segments of the bent nanowires/micronails. We also investigate the grafting of thin polymer films to gold objects. The developed grafting technique is employed for the surface modification of Si/SiO2/Au microprinted electrodes. When electronic devices are scaled down to submicron sizes, it becomes critical to obtain uniform and robust insulating nanoscale polymer films. Therefore, we address the electrical properties of polymer layers of poly(glycidyl methacrylate) (PGMA), polyacrylic acid (PAA), poly(2-vinylpyridine) (P2VP), and polystyrene (PS) grafted to the Si/SiO2/Au microprinted electrodes. The polymer layers insulated under normal ambient conditions can display a significant increase in conductivity as the environment changes. Namely, we demonstrate that the in-plane electrical conductivity of the grafted polymer layers grafted to Au and SiO2 surfaces can be changed by at least two orders of magnitude upon exposure to water or organic solvent vapors. The conductive properties of all the grafted polymer films under study are also significantly enhanced with temperature increase. The observed phenomenon makes possible the chemical design of polymer nanoscale layers with reduced or enhanced sensitivity to anticipated changes in environmental conditions. Finally, we show that the observed effects can be used in a micron-sized conductometric-transducing scheme for the detection of volatile organic solvents. This research also includes the study of nanoscale-level actuation with grafted polymer films and polymer/gold nanoparticles systems-grafted composites. First, we investigate the nanoscale-level… Advisors/Committee Members: Dr. Igor Luzinov, Dr. Stephen H. Foulger, Dr. O. Thompson Mefford, Dr. Scott M. Husson, Dr. Ruslan Burtovyy.

Subjects/Keywords: modification; nanoscale; Nickel; Gold; PGMA; polymer film; surface; Materials Science and Engineering

…94 5.3.5 Surface functionalization of nickel micronails with PGMA and PAA nanoscale polymer… …151 7.2.1 Synthesis, characterization and actuation of PGMA and PS/PGMA nanofoams… …151 7.2.2 Synthesis, characterization and actuation of the PGMA/gold nanoparticles composite… …156 7.3.1. Synthesis and characterization of PGMA nanofoam .........................156… …7.3.2. Actuation of the PGMA nanofoam… 

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APA · Chicago · MLA · Vancouver · CSE | Export to Zotero / EndNote / Reference Manager

APA (6th Edition):

Galabura, Y. (2014). SYNTHESIS AND CHARACTERIZATION OF NANOSCALE POLYMER FILMS GRAFTED TO METAL SURFACES. (Doctoral Dissertation). Clemson University. Retrieved from https://tigerprints.clemson.edu/all_dissertations/1300

Chicago Manual of Style (16th Edition):

Galabura, Yuriy. “SYNTHESIS AND CHARACTERIZATION OF NANOSCALE POLYMER FILMS GRAFTED TO METAL SURFACES.” 2014. Doctoral Dissertation, Clemson University. Accessed October 24, 2020. https://tigerprints.clemson.edu/all_dissertations/1300.

MLA Handbook (7th Edition):

Galabura, Yuriy. “SYNTHESIS AND CHARACTERIZATION OF NANOSCALE POLYMER FILMS GRAFTED TO METAL SURFACES.” 2014. Web. 24 Oct 2020.

Vancouver:

Galabura Y. SYNTHESIS AND CHARACTERIZATION OF NANOSCALE POLYMER FILMS GRAFTED TO METAL SURFACES. [Internet] [Doctoral dissertation]. Clemson University; 2014. [cited 2020 Oct 24]. Available from: https://tigerprints.clemson.edu/all_dissertations/1300.

Council of Science Editors:

Galabura Y. SYNTHESIS AND CHARACTERIZATION OF NANOSCALE POLYMER FILMS GRAFTED TO METAL SURFACES. [Doctoral Dissertation]. Clemson University; 2014. Available from: https://tigerprints.clemson.edu/all_dissertations/1300

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