Ceramics production: COld-cOntainer processing for Long-wavelength mid-infrared fibreoptics. (COOL)

Lead Research Organisation: University of Nottingham
Department Name: Faculty of Engineering

Abstract

We are making new types of optical fibre that transmit, and can emit, long-wavelength mid-infrared light. Why? Mid-infrared light-waves oscillate at frequencies within a range that matches the frequency-range of characteristic vibrations of molecular bonds. The molecular bond vibration increases in amplitude on (resonantly) absorbing mid-infrared light of the same frequency. For the first time, we made a record optical fibre that, on being laser pumped, emitted a record broad range of frequencies of mid-infrared light: 'a mid-infrared rainbow' called a mid-infrared supercontinuum (SC) of light [1]. Shining this broad SC of mid-infrared light onto a molecular sample, and collecting the light again after its interaction with the sample, reveals some mid-infrared frequencies are diminished in brightness, gone to stimulate particular molecular vibrations in the sample. This is called mid-infrared spectroscopy and it allows us to sense and image the molecular makeup of a molecular sample, including numerous molecular gases, liquids and solids as diverse as: greenhouse-gases, explosives, food and biological tissue.

To date, because mid-infrared light sources have been characteristically weak the source/sample/ detector have all had to be in close proximity. The new bright [1,2] mid-infrared fibre SC sources are a disruptive technology which will help establish a new paradigm in PORTABLE, REAL-TIME mid-infrared molecular sensing and imaging, opening up the mid-infrared spectral region for more general use. We are developing this new paradigm through focused development of portable fibre devices and systems which are robust, functionally designed, safe, compact and cost effective, and which are based on mid-infrared optical fibers. Hyper-pure optical fibres are required to increase the efficiency of the SC sources and to realise long-wavelength mid-infrared fibre lasers, and also for passive routeing of mid-infrared light to where it is needed.

Currently, making and purifying the long-wavelength mid-infrared optical fibres is rather intricate and takes about 8 man-weeks. This long-winded processing could be hugely cut, and hyper-purity improved, by applying the innovative processing methods to be developed in this Project.

Currently, resistive heating is used for glass-melting and purification but production times are exceedingly long. We demonstrated for the first time [3] that microwave-assisted heating can achieve high-speed glass-melting. In this Project, we will develop the microwave approach, optimise microwave-cavities and carry out rapid glass melting and follow-on rapid glass hyper-purification via microwave-heating.

Why is the microwave heating so fast? -because the microwaves directly couple to the mid-infrared glass melt and not to the container, which remains cold and uncompromised. Far higher glass-melting temperatures can be attained than normal which: (i) gives faster melt-homogenisation (0.5 h instead of 36 h) and (ii) facilitates high vapour pressures for fast multi-distillations of the glass-melt.

This Project aims to achieve novel cold-container processing to enable the unprecedented rapid manufacture of long-wavelength mid-infrared selenide and telluride chalcogenide glasses of new levels of hyper-purity needed to make new long-wavelength mid-infrared glass fibre-optic devices for disruptive portable, real-time molecular sensing and imaging.

In this Project we will demonstrate, by means of new rapid processing:

i. new hyper-pure fibres for conduiting long-wavelength mid-infrared light;
ii. new hyper-pure long-wavelength mid-infrared SC fibre sources for efficient portable molecular sensing and
iii. first time long-wavelength mid-infrared fibre lasers for pumping the fibre SC.


REFERENCES
1. Petersen, Tang, Benson, Seddon et al., NAT. PHOTON. 8 830(2014).
2. Yu et al., Opt. Lett., 40(6)1081(2015).
3. Prasad, Seddon et al., J. Non-Cryst. Solids, 356(41-42) 2134(2010).

Planned Impact

IMPACT SUMMARY

1. INTRODUCTION

This Project will help to make a new generation of portable long-wavelength mid-infrared fibre-optic devices for molecular sensing and imaging. The technological impact of these new devices will be game-changing through diverse applications across many UK sectors such as healthcare, energy, security and manufacturing.

This Project aims to achieve novel cold-container processing to enable the unprecedented rapid manufacture of long-wavelength mid-infrared selenide and telluride glasses of new levels of hyper-purity. These are needed to make the new mid-infrared glass fibre-optic devices for the new disruptive paradigm of portable, real-time molecular sensing and imaging.

This Project will assist in "greener" materials' manufacture; the energy demands of the cold-container processing will be lower than the conventional processing it replaces.

The impact in UK science/engineering will be in aspects of generating new UK business and of trained people.

2. TECHNOLOGY IMPACT OF PORTABLE, REAL-TIME MID-INFRARED FIBRE-OPTIC SENSING AND IMAGING DEVICES ON UK SECTORS AND UK BUSINESS

Long-wavelength mid-infrared fibre supercontinuum sources and fibre lasers are disruptive technologies for real-time molecular sensing and imaging in: monitoring environmental quality (sensing pollutants e.g. exhaust gases from industrial plant, cars); energy-efficiency of fossil fuels (CO/CO2 balance); food security (authenticity/adulteration) and drink security (e.g. beer quality!); in agriculture (e.g. sensing ethylene gas in tomato ripening; monitoring leaf-hydration in farming); aquaculture (fish-farming: e.g. sensing bacterial contamination); real-time monitoring of manufacturing and chemical processing (e.g. distributed fibre-optic mid-infrared sensing enabling process control), including of oil fractionates/products; manufacturing pharmaceuticals and cosmetics and for medical diagnostics such as early skin cancer diagnosis through objective spectroscopic imaging of tissue in a primary-care setting.

Security and safety applications of mid-infrared fibre lasers include: mid-infrared ship-to-ship free-space communications, aircraft free-space counter-measures and collision-avoidance. Stand-off explosives' and narcotics' mid-infrared sensing, for instance at airports, will lead to better public safety.

New mid-infrared fibre lasers will exhibit better beam quality than currently available which will enable well-controlled laser cutting, machining and patterning of soft materials, like polymers and polymer-composites by analogy with currently emerging high-power near-infrared fibre lasers being exploited for laser cutting/welding of hard materials, like metals.

In the medical field, new wavelengths for laser surgery of human tissue will lead to more diverse and better matter/light interaction through resonance with protein/lipid absorption at newly available mid-infrared long-wavelengths, for better health outcomes.

Overall, portable long-wavelength mid-infrared fibre-based molecular sensing will allow greater control to be had in real-time, over many types of processes and procedures as well as being a new manufacturing tool. At a national level, National Health Service costs will be beneficially impacted, as well as patient comfort and convenience. There will be beneficial impact to UK industry, the UK energy sector, UK defence and security, UK agriculture and UK healthcare from this new technology.

3. IMPACT THROUGH PEOPLE TRAINING

During this Project, the Researcher will be equipped with skills in developing new manufacturing routes and trained in mid-infrared photonics. The future employment prospects are excellent in the 'people pipeline' in this new field. This includes the large PhD groups and undergraduate pools, of the Investigators, who will benefit directly by interacting with this major Project in new types of processing and in mid-infrared photonics.

Publications

10 25 50
 
Description 22 Feb 2018: We have discovered that the new type of glass processing we wish to develop on COOL actually has required the design and building of a specialist rig beyond what we had anticipated on writing the grant application. The specialist rig comprises a monomode microwave cavity, clam shell furnaces above the cavity to house the distillation rig and a dedicated turbo pump for open and closed vacuum processing. The whole equipment is being housed in a new large fume cupboard which is tall enough to accommodate the vertical processing rig we have designed and are now building. This is to ensure that any fumes that might escape will be neutralised. The design and building of this specialist rig has taken over 12 months and so we have been unable to start our experiments regarding the new type of glass processing yet. We anticipate that our first experiments will be in June 2018 and our first goal is as in the Research Proposal which is to make low optical loss unstructured mid-infrared optical fibre in a fraction of the time of the old type of conventional processing.
25 Feb 2021
We have now successfully made undoped, low optical background loss binary and ternary fibre.
Exploitation Route We will be able to comment on this once we have been able to carry out our first set of new glass processing, we anticipate this t take place in June 2018.

We are still progressing the outcomes. We now have evidence that this processing offers a brand new way of making low background optical loss passive transmission mid-infrared fibre. We are still investigating efficacy of making lanthanide doped fibre and these investigations are under progress.
Sectors Aerospace, Defence and Marine,Agriculture, Food and Drink,Chemicals,Electronics,Energy,Environment,Healthcare,Security and Diplomacy

 
Description Professor AB Seddon has been elected Trustee of the Royal Institution, UK, for 3 years from April 2020.
First Year Of Impact 2020
Sector Education
Impact Types Societal

 
Description 'New generation, mid-infrared (MIR) fibre lasers operating at long-wavelength. The Royal Society UK/Canada travel £12k 2019-2021
Amount £12,000 (GBP)
Funding ID IES\R3\183055 
Organisation The Royal Society 
Sector Charity/Non Profit
Country United Kingdom
Start 03/2019 
End 02/2021
 
Description British Council Newton Impact Scheme
Amount £97,000 (GBP)
Funding ID BC 623830962 
Organisation British Council 
Sector Charity/Non Profit
Country United Kingdom
Start 09/2021 
End 12/2022
 
Description Mid-infrared power handling.
Amount £100,000 (GBP)
Funding ID ACC2028489 
Organisation Defence Science & Technology Laboratory (DSTL) 
Sector Public
Country United Kingdom
Start 04/2023 
End 02/2024
 
Description SHAPE: Ceramic SHaping: extrusion of glAss Preforms for new fibres in hEalthcare. EPSRC EP/T010762/1 £770.4k fec 2020-2024
Amount £770,400 (GBP)
Funding ID EP/T010762/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 06/2020 
End 05/2024
 
Description SHAPE Ceramic SHaping: extrusion of glAss Preforms for new fibres in hEalthcare £770.4k fec EPSRC EP/T010762/1 Partnership in the Faculty of Engineering, University of Nottingham, UK. Prof 
Organisation Glass Technology Services
Country United Kingdom 
Sector Private 
PI Contribution I am PI on this Grant Award (SHAPE Ceramic SHaping: extrusion of glAss Preforms for new fibres in hEalthcare, £770.4k fec, EPSRC EP/T010762/1) Ceramic SHaping: extrusion of glAss Preforms for new fibres in hEalthcare (SHAPE) The Aim of this Project is to achieve unprecedented advances in novel glass extrusion in order to make brand new shapes of glass preforms. These preforms are needed for drawing to next-generation structured glass fibres for two targeted healthcare applications - bioimplant glass fibre for therapeutics and MIR (mid-infrared) glass fibre lasers for cancer detection. 1. Glass extrusion What is glass extrusion? Heat glass above its glass transition temperature (Tg) and a viscous liquid forms. This liquid has treacle-like consistency and can be shaped by forcing it through a shaped metal die. For instance, a die with a hole produces a rod-shaped extrudate. The extruded rod is allowed to cool, and stiffens at Tg to form a glass-rod preform, which is taken to a draw tower and, in a separate operation, drawn to form glass fibre of the ~ diameter of a human hair. Co-extrusion, through the hole in the die, of two glass billets of different glass composition, but with matched thermal properties, forms a glass-rod preform with an internal core of different glass through it. Along part of the preform length, the internal core of glass occupies approx. constant 85 % of the diameter. When this is drawn to fibre, the fibre similarly has a large core of glass occupying 85 % of the diameter. The core/cladding interface is excellent optical quality, having mated during the extrusion itself. However, only 20% of the extruded rod preform is usable, as the core inside the rest of the preform is too tapered. Extrusion through a spider-die can produce a glass preform in the shape of a small-orificed tube. If a cane of different glass is now threaded through this tube, this whole can be drawn to fibre with a small core running through it and occupying less than ~ 20 % of the fibre diameter. Such small core fibre is vital to achieve fibre lasing. However, this processing route makes inferior optical quality core/cladding interfaces and can take several weeks. 2. MIR fibre This Project will enable straightforward manufacture of high quality small-core fibre vital for MIR-glass fibre lasers. We will extrude small-core glass-rod preforms with core less than or equal to 20 % diameter, constant over least 50 % of the preform, with core/cladding mating during extrusion to give excellent optical quality of the core/cladding interface. To achieve this breakthrough, we will invoke, for the first time, extrusion of pre-shaped glass billets, and also indirect glass extrusion - overlooked since its invention ~50 years' ago. MIR light distinguishes diseased tissue, including cancer, by detecting the molecular-makeup of the tissue. Using MIR fibre-optics will enable a new type of endoscopy so that during cancer surgery the surgeon can guide MIR fibre laser light onto the tissue and collect the reflected light to molecularly map the tissue and instantly tell if all cancer is removed. Compact MIR fibreoptic systems will be enabled by using MIR broad- and narrow-band fibre lasers; for these, small-core MIR fibre is essential and this Project will enable the new extrusion technology to make this possible. 3. Biocompatible, therapeutic fibre The human body does not reject biocompatible fibre. We will extrude new types of multi-layered and holey biocompatible glass preforms for bioimplant fibre of finely controlled dissolution rate in the body. This is for therapeutic drug and ion release from fibre at the site of body infection and for controlled dissolution fibre-biocomposites to implant in the body to support bone-healing. 4. Project synergy This Project will encourage cross-fertilisation of ideas, for instance a bio-compatible glass cladding for MIR glass fibres may be beneficial and using biocompatible glass fibres for NIR (near-infrared) light transmission has the potential to allow in situ monitoring of tissue health in vivo.
Collaborator Contribution This Project starts on 1 June 2020.
Impact The Project starts 1 June 2020. The collaboration is multidisciplinary: electromagnetic wave modelling; fabricating glass; glass structure; commercial upscale of processing
Start Year 2020
 
Description SHAPE Ceramic SHaping: extrusion of glAss Preforms for new fibres in hEalthcare £770.4k fec EPSRC EP/T010762/1 Partnership in the Faculty of Engineering, University of Nottingham, UK. Prof 
Organisation Glass Technology Services
Country United Kingdom 
Sector Private 
PI Contribution I am PI on this Grant Award (SHAPE Ceramic SHaping: extrusion of glAss Preforms for new fibres in hEalthcare, £770.4k fec, EPSRC EP/T010762/1) Ceramic SHaping: extrusion of glAss Preforms for new fibres in hEalthcare (SHAPE) The Aim of this Project is to achieve unprecedented advances in novel glass extrusion in order to make brand new shapes of glass preforms. These preforms are needed for drawing to next-generation structured glass fibres for two targeted healthcare applications - bioimplant glass fibre for therapeutics and MIR (mid-infrared) glass fibre lasers for cancer detection. 1. Glass extrusion What is glass extrusion? Heat glass above its glass transition temperature (Tg) and a viscous liquid forms. This liquid has treacle-like consistency and can be shaped by forcing it through a shaped metal die. For instance, a die with a hole produces a rod-shaped extrudate. The extruded rod is allowed to cool, and stiffens at Tg to form a glass-rod preform, which is taken to a draw tower and, in a separate operation, drawn to form glass fibre of the ~ diameter of a human hair. Co-extrusion, through the hole in the die, of two glass billets of different glass composition, but with matched thermal properties, forms a glass-rod preform with an internal core of different glass through it. Along part of the preform length, the internal core of glass occupies approx. constant 85 % of the diameter. When this is drawn to fibre, the fibre similarly has a large core of glass occupying 85 % of the diameter. The core/cladding interface is excellent optical quality, having mated during the extrusion itself. However, only 20% of the extruded rod preform is usable, as the core inside the rest of the preform is too tapered. Extrusion through a spider-die can produce a glass preform in the shape of a small-orificed tube. If a cane of different glass is now threaded through this tube, this whole can be drawn to fibre with a small core running through it and occupying less than ~ 20 % of the fibre diameter. Such small core fibre is vital to achieve fibre lasing. However, this processing route makes inferior optical quality core/cladding interfaces and can take several weeks. 2. MIR fibre This Project will enable straightforward manufacture of high quality small-core fibre vital for MIR-glass fibre lasers. We will extrude small-core glass-rod preforms with core less than or equal to 20 % diameter, constant over least 50 % of the preform, with core/cladding mating during extrusion to give excellent optical quality of the core/cladding interface. To achieve this breakthrough, we will invoke, for the first time, extrusion of pre-shaped glass billets, and also indirect glass extrusion - overlooked since its invention ~50 years' ago. MIR light distinguishes diseased tissue, including cancer, by detecting the molecular-makeup of the tissue. Using MIR fibre-optics will enable a new type of endoscopy so that during cancer surgery the surgeon can guide MIR fibre laser light onto the tissue and collect the reflected light to molecularly map the tissue and instantly tell if all cancer is removed. Compact MIR fibreoptic systems will be enabled by using MIR broad- and narrow-band fibre lasers; for these, small-core MIR fibre is essential and this Project will enable the new extrusion technology to make this possible. 3. Biocompatible, therapeutic fibre The human body does not reject biocompatible fibre. We will extrude new types of multi-layered and holey biocompatible glass preforms for bioimplant fibre of finely controlled dissolution rate in the body. This is for therapeutic drug and ion release from fibre at the site of body infection and for controlled dissolution fibre-biocomposites to implant in the body to support bone-healing. 4. Project synergy This Project will encourage cross-fertilisation of ideas, for instance a bio-compatible glass cladding for MIR glass fibres may be beneficial and using biocompatible glass fibres for NIR (near-infrared) light transmission has the potential to allow in situ monitoring of tissue health in vivo.
Collaborator Contribution This Project starts on 1 June 2020.
Impact The Project starts 1 June 2020. The collaboration is multidisciplinary: electromagnetic wave modelling; fabricating glass; glass structure; commercial upscale of processing
Start Year 2020
 
Description Visiting Professorship of Professor Angela B Seddon at Kyoto University, Japan. Host Professor Setsuhisa Tanabe 
Organisation University of Kyoto
Country Japan 
Sector Academic/University 
PI Contribution Discussions of mutual interest regarding photoluminescence.
Collaborator Contribution Discussions of mutual interest regarding photoluminescence.
Impact Still at start.
Start Year 2020