Author Type

Graduate Student

Date of Award

Fall 12-8-2025

Document Type

Thesis

Publication Status

Version of Record

Submission Date

December 2025

Department

Biomedical Engineering

College Granting Degree

Engineering and Computer Science

Department Granting Degree

Biomedical Engineering

Degree Name

Master of Science (MS)

Thesis/Dissertation Advisor [Chair]

Vivian Merk

Abstract

This study presents a detailed exploration of the synthesis, morphological tuning, and physicochemical characterization of nickel nanoparticles (NiNPs) engineered for catalytic applications in aqueous environments. Using a modified polyol method adapted from Couto et al., nanoparticles were synthesized under controlled thermal and chemical conditions with nickel chloride hexahydrate, polyvinylpyrrolidone (PVP), and sodium borohydride in ethylene glycol according to a modified version of this synthesis protocol.1 The reaction temperature and reactivity of the reducing agent were found to significantly influence particle size. Reaction temperatures were varied between 120° C and 170° C, resulting in nanoparticle sizes between 23 ± 7 nm and 13 ± 4 nm. Potent NaBH₄ enabled rapid burst nucleation, yielding uniform NiNPs in < 25 nm size range. Post-synthesis processing included rigorous washing and sonication to minimize residual contaminants and enhance colloidal stability. The morphological and chemical characterization of NiNPs was conducted using transmission electron microscopy (TEM), dynamic light scattering (DLS), zeta potentials, energy-dispersive X-ray spectroscopy (EDS), electron energy loss spectroscopy (EELS), alternating gradient magnetometry (AGM), and high-angle annular dark field (HAADF) scanning TEM imaging. DLS and zeta potential measurements confirmed the role of surface charge in providing nanoparticle stability2. STEM-EELS mappings was used to quantify the level of surface oxidation occurring at various reaction temperatures, which can affect the catalytic activity of NiNPs. It was found that surface oxidation increased with the reaction temperature. AGM was used to obtain hysteresis curve measurements to quantify the magnetic properties of the NiNPs. The saturation magnetization was found to increase with the reaction temperature. The findings provide a systematic foundation for engineering nanoparticle synthesis and surface chemistry towards CO2 remediation in freshwater and saltwater, an environmentally relevant aqueous-phase application. The work highlights the importance of surfactant selection and reaction temperature as controllable levers for engineering size, dispersion, stability, and magnetic recoverability — critical factors for future integration into aqueous-phase systems and nanomaterial-based environmental technologies.

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