Automated modular platforms for the exploration and discovery of inorganic materials

Salley, Daniel (2020) Automated modular platforms for the exploration and discovery of inorganic materials. PhD thesis, University of Glasgow.

Abstract

The work presented in this thesis focuses on the development and use of automated systems for the synthesis, discovery, and study of inorganic materials, specifically polyoxometalates and gold nanoparticles. The introduction of automated systems in chemistry laboratories has had a profound impact in many areas, increasing productivity whilst reducing menial tasks. However, for many reasons the wide scale adoption of automated systems has been historically slow. Despite having received much attention in recent years, commercially available automated solutions to everyday laboratory activities still suffer from a combination of the two major drawbacks. As Chapter 1 details, the first drawback is that many systems are prohibitively expensive and the second is a lack of adaptability beyond the initial purpose of a given unit, due to a lack of modularity in the design of hardware and/or software.
Two of the three results chapters of this work demonstrate the creation of a singular modular architecture for chemical synthesis, that can range from its base unit providing simple liquid handling capabilities at a fraction the cost of commercially available alternates, to that same unit being the epicentre of a closed-loop workflow that can perform environmentally controlled reactions, obtain and learn from reaction data in order to navigate and optimise difficult synthesis. The former unit was used to combinatorically explore polyoxometalate chemistry in which it discovered new and novel species and independently reproduced known compounds. The latter was used to optimise several seed mediated syntheses of gold nanoparticle shapes using a genetic algorithm. The modular hardware and accompanying software can perform multiple reactions in parallel whilst incorporating sample removal for in-line analysis, probe-based feedback, reaction-to-reaction transfer and other capabilities.
The remaining results chapter involved the development of robotic platforms capable of collaborating over shared chemical tasks. Two such units were used to study the crystallisation process of a known polyoxometalate and optimise the specific conditions for the formation of crystals. This project was a proof of concept to help envision a future where laboratories could possess interlinked reaction apparatus for the sharing of results to combat irreproducibility of published data. Combined the three results chapters of this work utilise three different types of automation for inorganic synthesis using custom designed architectures: a combinatorial approach (chapter two), a collaborative approach (chapter 3) and an intelligent, algorithm driven approach (chapter 4).
We believe that automation of reaction and data recording processes have a significant part to play in combatting the growing reproducibility problem in chemistry as well as science generally. One fundamental goal and common theme seen throughout this work is attempts to us the systems developed here to increase the reliability and reproducibility of our published work.

• Item Type: Thesis (PhD)
• Qualification Level: Doctoral
• Keywords: Chemistry, automation, robotics, inorganic materials, nanoparticles polyoxometalates.
• Subjects: Q Science > QD Chemistry; T Technology > T Technology (General)
• Colleges/Schools: College of Science and Engineering > School of Chemistry
• Supervisor's Name: Cronin, Professor Leroy
• Date of Award: 2020
• Embargo Date: 15 October 2023
• Depositing User: Mr Daniel Salley
• Unique ID: glathesis:2020-81725
• Copyright: Copyright of this thesis is held by the author.
• Date Deposited: 28 Oct 2020 09:54
• Last Modified: 28 Oct 2020 10:35
• URI: https://theses.gla.ac.uk/id/eprint/81725