Witnessing the birth of a crystal nucleus by non-photochemical laser-induced nucleation

Lead Research Organisation: University of Edinburgh
Department Name: Sch of Chemistry

Abstract

Crystals appear everywhere in nature and are the silent heroes of technology: crystals make up the foundations of electronic devices (e.g., silicon wafers) and pharmaceuticals (in medicines). The initial birth of a crystal, from a molten liquid or from solution is called nucleation. It is hard to say what the events are leading-up and during to nucleation, because it happens randomly in location and in time. If we were able to choose when and where nucleation took place, we could witness the birth of a single crystal. The aim of our project is to do just that, using a new effect called non-photochemical laser-induced nucleation (NPLIN). This effect uses a short pulse of light (billionths of a second) from a laser to stimulate nucleation, and we have recently developed this technique to choose where and when this happens. Our goal is to examine NPLIN in detail to unravel the structures and motions of nuclei that occur during nucleation. We also want to be able to harness NPLIN so that it can enable synthesis and determination of the structures of new materials, such as proteins and drugs. To achieve these goals, we will build a unique microscope (a laser scattering microscope) at the UK Central Laser Facility, and we will use two beams of laser light, one to initiate and one to watch crystal nucleation as it happens. The laser light we will use to watch crystal nucleation will also allow us to measure the sizes and movements of clusters of material, some as small as 100 nm (100 billionths of a metre!) that are not ready to nucleate. We will also be able to excite these clusters and nuclei with our beam (using a technique called micro-Raman spectroscopy) to find out details of the structure of these clusters and how they change as they nucleate. Our instrument will use tweezers made of light (so-called laser tweezers ) to trap clusters of material that are ripe and have the potential to nucleate, and we will nucleate these trapped clusters with an intense pulse of light. Through our project we will be nucleating growth of another important species: one of the next generation of scientists who are trained, equipped and ready to exploit the premier national science facilities and the light sources of the future. The project student will be trained in designing, building and operating laser microscopy instruments using the latest advances in lasers and optical technology. When fully trained, this student will be an expert in crystal nucleation technology and an innovator at the forefront of science, working to position the UK at the head of a global technological economy.

Publications

10 25 50
 
Description The overarching aim of our EPSRC-funded research project was to elucidate microscopic mechanisms underlying crystal nucleation. Using pulsed lasers we demonstrated (2009) unprecedented temporal (within 5 ns) and spatial (within 100 micrometres) control of nucleation of potassium chloride salt. In 2010 we demonstrated symmetry breaking (forming left or right-handed crystals) in a molten salt, and in 2011 we showed that the system had memory, which we attributed to activation of residual seeds that survived melting and were reactivated by the laser. In 2012 we resolved the mechanism behind the effect of luminescence during crystallisation of sodium chloride salt, first observed over a century ago. With collaborators at Research Complex at Harwell, we built (in 2013) a microscope that has provided the first direct images of clusters of crystal solute in concentrated urea solutions; these clusters are believed to be the objects that trigger crystal nucleation.
Exploitation Route Crystal nucleation occurs widely in nature and is a fundamental step in many industrial processes, e.g., manufacture of fine chemicals. By its mid-point, our project had generated interest from the pharmaceutical sector and we began collaboration with the EPSRC Centre for Innovative Manufacture: Continuous Manufacture and Crystallisation (CMAC). The interest was focused on our ability to control nucleation, which can significantly alter the physical properties of the final solid, e.g., rate of solubility or suitability for tableting as a drug. Our work has stimulated other research groups, in France, Japan, and USA to develop important new methods for studying the mechanism of crystal nucleation and growth. In particular our work has stimulated new theoretical and computational models of nucleation; new collaboration as a direct outcome of the funding has recently provided (2015) the first evidence for transient clusters on a timescale commensurate with our experiments.
Sectors Agriculture, Food and Drink,Chemicals,Electronics,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology

 
Description A key outcome of the project was training of a PhD student in advanced microscopy techniques at the Central Laser Facility (CLF): after a brief period of postdoctoral research, the student is now working as a consultant for a contract research organisation, servicing primarily the pharmaceutical sector. Many children have grown crystals at home or school, as it is an ideal topic to capture the imagination. Funding from the grant allowed us to engage schools and the public, e.g., by outreach to schools in Midlothian area, with a view to widening participation in higher education. Funding allowed us to participate in public engagement events at the Midlothian Science Festival and Edinburgh International Science Festival. Key results on laser control of nucleation were picked up by the media, and our research was featured, e.g., on BBC radio and TV. We also filmed a short interview for REN tv (Russia) where we explained potential applications of control of nucleation. The research funding allowed us to engage with the pharmaceutical industry. An important outcome was development of collaborations (EPSRC Centre for Continuous Manufacture and Control), and further funding to develop application of the research in manufacturing (EPSRC Manufacturing with Light). We have recently (2015) begun to demonstrate economic impact through an Impact Acceleration Funding grant, partnered with global pharmaceutical company GSK.
First Year Of Impact 2014
Sector Chemicals,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology
Impact Types Societal,Economic

 
Description Royal Society Small Research Grant
Amount £5,000 (GBP)
Organisation The Royal Society 
Sector Charity/Non Profit
Country United Kingdom
Start  
 
Title SHG microscopy 
Description In collaboration with researchers at Rutherford Appleton Laboratory (STFC Research Complex Harwell) we have developed new method for Second Harmonic (SH) Scattering microscopy applied to transient detection of SH active particles in solution. 
Type Of Material Improvements to research infrastructure 
Year Produced 2014 
Provided To Others? Yes  
Impact The techniques used are available to users of the Lasers for Science Facility at the Central Laser Facility at Harwell. M. R. Ward, S. W. Botchway, A. D. Ward, A. J. Alexander, Faraday Discussions 167, 441-454 (2013):"Second-harmonic scattering in aqueous urea solutions: evidence for solute clusters?". doi:10.1039/C3FD00089C 
 
Description CMAC 
Organisation EPSRC Centre for Innovative Manufacturing for Continuous Manufacturing and Crystallisation (CMAC)
Country United Kingdom 
Sector Public 
PI Contribution Exchange of knowledge, engagement with industry. I was a member of the CMAC academic committee from October 2013 - December 2016. Since January 2017 I have been an associated academic of the CMAC Future Manufacturing Research Hub.
Collaborator Contribution Exchange of knowledge, sharing of expertise, facilities and equipment.
Impact The following published works are associated with the collaboration (within the discipline of the award) DOI: 10.1021/acs.cgd.5b00854 Martin Ward, PhD thesis, University of Edinburgh, 2014 Alasdair Mackenzie, PhD thesis, University of Edinburgh, 2017 DOI: 10.1021/acs.cgd.6b00882 DOI: 10.1039/c6cp07997k DOI: 10.1039/c7cp03146g DOI: 10.1063/1.5079328
Start Year 2013
 
Title NanoTrackJ contribution 
Description The software plugin was written by Thorsten Wagner, Martin Wiemann and Hans-Gerd Lipinski Software was tested using data generated from our research project, including exchange of ideas and knowledge for development. 
Type Of Technology Software 
Year Produced 2013 
Open Source License? Yes  
Impact Details of the collaboration are noted in the PhD Thesis of Martin Ward, University of Edinburgh, 2014. 
URL http://dx.doi.org/10.6084/m9.figshare.805052
 
Description Lasers for crystal storage (media coverage) 2009 
Form Of Engagement Activity A broadcast e.g. TV/radio/film/podcast (other than news/press)
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Public/other audiences
Results and Impact Press release on outcome of research: Lasers for Crystal Storage. Live interview with Peter Allen and Anita Anand on BBC Radio 5 Live (19/10/09); Recorded television interview on BBC Reporting Scotland (broadcast 21/10/09); various online and newspaper articles.

We received a number of contacts from public, academic, industrial sectors about our work. Contact from Russian television station (RT) to record interview in my laboratory for documentary on economic importance of salts.
Year(s) Of Engagement Activity 2009
URL http://news.bbc.co.uk/1/hi/scotland/edinburgh_and_east/8312286.stm
 
Description Midlothian Science Festival 2013 
Form Of Engagement Activity Participation in an activity, workshop or similar
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Public/other audiences
Results and Impact Martin Ward participated in drop-in workshop for Midlothian Science Festival (at Lasswade Centre) primarily aimed at schoolchildren and families, where he was able to discuss his research.
Year(s) Of Engagement Activity 2013
 
Description REN tv interview 2013 
Form Of Engagement Activity A broadcast e.g. TV/radio/film/podcast (other than news/press)
Part Of Official Scheme? No
Geographic Reach International
Primary Audience Public/other audiences
Results and Impact Recorded TV interview for Russian Television station REN TV documentary. Interview was on production of crystals by laser-induced nucleation, and possible applications of the method.
Year(s) Of Engagement Activity 2013
 
Description St Martins 2013-15 
Form Of Engagement Activity Engagement focused website, blog or social media channel
Part Of Official Scheme? No
Geographic Reach Local
Primary Audience Schools
Results and Impact Web based Question+Answer sessions from multiple primary school groups at St Martins primary school, East Lothian.
Year(s) Of Engagement Activity 2013,2014,2015