Instrumentation and Control of Carbon Nanotube Fibre Manufacture

Lead Research Organisation: University of Cambridge
Department Name: Engineering

Abstract

Over the past 7 years at Cambridge, a team led by Prof Windle has developed a process capable of making continuous carbon fibres in a single operation that are composed of entangled multi and single wall carbon nanotunes. The potential of this ground-breaking process for making high performance fibres has led to the opportunity of it being applied in a broad range of industrial sectors. It offers a disruptive technology that, if successfully developed through greater manufacturing innovations, is poised to replace traditional materials in a host of mechanical and electrical applications. Moreover, the current research position established by the Cambridge team offers a significant opportunity for the UK to take the lead in the development of a new materials supply chain, new manufacturing process technologies, and product innovations that are a step change from their conventional counterparts. Prof Windle's work to date has established the basic manufacturing process through a series of many process innovations. Numerous advances in reactor design, catalyst materials, and operating conditions have been explored in order to establish the manufacturing foundations. Many kilometres of fibre can now be produced in a continuous operation. However, limitations of the current laboratory production system include: variation in material characteristics such as fibre width; CNT crystal structure; mechanical strength; thermal and electrical conductivity. These issues have become a significant barrier to the consistent high volumetric production of materials with known characteristics. This project will develop advanced on-line instrumentation and manufacturing technology solutions that will enable the tightly controlled production of CNT fibre with sufficient quality and and in sufficient quantity that will allow industrial users to begin testing the materials in their new products. The new CNT fibres could find widespread applications in all sectors including power generation, aerospace, automotive, defence and consumer goods.

Planned Impact

The major research and development outputs from this programme could make significant impacts across all parts of the manufacturing value chain, society at large, and the wider economy. The proposal offers an opportunity to develop new manufacturing capabilities for the production of high volumes of low cost and high quality CNT fibre materials. The new and advanced instrumentation technology developed here will provide an important step forward in the reliable production of CNT fibres. CNT fibres will, for the first time, be produced under known and regulated conditions. Moreover, the provision of high quality CNT fibres will increase the take-up of these new materials downstream across a range of industrial sectors. The commercial private sector will benefit from the research through the availability of a new class of materials that will allow them to enhance their product offerings through more efficient designs, or lower costs. Policy makers could take advantage through the setting of standards that allow greater use of resources in materials consumption or improved health and safety measures in personal protection equipment in military or industrial applications. The wider public could see improved product performance through greater electrical and mechanical efficiencies in a wide range of products. The research could directly contribute to the nations wealth by placing the UK in the international lead in this area and establish the manufacturing value chain that delivers thousands of UK jobs in the production, supply and application of the new materials. These manufacturing breakthroughs coupled with new knowledge of the process, have the potential to allow industry to establish swathes of new products for the market, that have the potential for significant societal impacts in areas such as health-care, transport, energy generation, communications and defense. These benefits are significant and could all be realised in the next 10 years should this research be successful. The knowledge and experience gained in terms of new manufacturing technologies and production methods, and the output of leading experts in the field could be applied in the creation of new and potentially world leading companies.
 
Description We have completed the construction of a new fibre drawing tower, and implemented a feedback control system for the ferrocene catalyst injection, in addition to the use of FTIR for live analysis of the gas mixture inside the reactor. In addition, the means by which we can remotely monitor the electrical characteristics of the drawn fibre have been completed. The final stage of experiments sought to define the critical operating parameters for the production of reliable CDT fibre. Work to date has included the design, installation and testing of an optical monitoring cell for the reaction catalyst ferrocene and the testing of a commercial moisture sensor on the main gas line. Wide ranging experiments using statistical analysis tools have allowed us to establish correlations between the floating catalyst process parameters and the properties of single and multi walled carbon nanotube fibres. These findings provide greater knowledge of the floating catalysts production process, and the ability to effect greater control over the process.
Exploitation Route The findings of this programme will be taken forward by academics working in this research field. In addition, the licence holder of the floating catalyst technology is seeking access to the IP and generated in the programme
Sectors Aerospace, Defence and Marine,Digital/Communication/Information Technologies (including Software),Electronics,Energy,Manufacturing, including Industrial Biotechology,Retail

 
Title Database of fibre properties and process parameters 
Description A comprehensive database of floating catalyst process parameters linked directly with carbon nanotube fibre properties has been generated from the outputs if this work 
Type Of Material Improvements to research infrastructure 
Year Produced 2018 
Provided To Others? No  
Impact The dataset generated through this programme offers deep insight into the performance of a floating catalyst process route for the production of CNT fibres. Comprehensive analysis of the data using JMP approaches has enabled us to identify the links between major process variables and CNT fibre properties. This has led to new process recipes for targeting fibres with specific enhancement of critical properties such as electrical conductivity, tenacity, and mechanical strength. 
 
Title Raman and TGA data supporting Kaniyoor et al. "High throughput production of single-wall carbon nanotube fibres independent of sulfur-source" 
Description Supporting data for Raman spectra and Thermogravimetric Analysis (TGA) data given in Kaniyoor et al. "High throughput production of single-wall carbon nanotube fibres independent of sulfur-source". The folder contains Raman spectroscopy and Thermogravimetry data for the various samples analysed in the work. Raman spectra were obtained using a Bruker Raman Senterra microscope with laser lines 532 (2.33 eV, 5 mW), 633 (1.96 eV, 5 mW), and 785 nm (1.58 eV, 10 mW). For every sample at least five different locations are sampled under a x20 objective, and averaged in the Bruker OPUS software. The raw data is presented in the Raman folder, named as Date synthesised_Sample name_Microscope Objective_Laser Wavelength_Laser Power_Accumulation time_Number of additions. Each data file has two columns which are Raman shift (in cm-1) and Intensity (counts). Please refer to the excel/.csv file in this folder to link the sample names to the flow rate, sulfur source (thiophene, carbon disulphide (CS2), elemental sulfur) and molar concentration (Low = 0.76 S:Fe, high = 1.52 S:Fe) under which the samples were synthesised. To obtain graphs presented in the paper, the data must be baseline corrected by asymmetric least squares method, and all intensities must be normalized to the respective G band intensity maximum. G:D values are calculated by taking the area of the G and D peaks. These analyses can easily be performed in Origin software. Thermogravimetry was performed using a TA Instruments Q500 under a dynamic ramp rate to 1000 8C with synthetic air. The data presented were obtained directly from the TA instruments software. The naming protocol is as follows: Sample synthesized date_Sample number_sulfur concentration and source hydrogen flow rate. Each data file has several columns of data. The important columns are 2nd- temperature (in celcius), 3rd ñ mass of the sample at different temperatures (in mg), 6th ñ derivate mass loss data. Information such as amorphous carbon content and residual catalyst can be obtained from the mass loss curves. Integrating different peaks in the derivative curves gives the amount of species that burn at that peak. 
Type Of Material Database/Collection of data 
Year Produced 2019 
Provided To Others? Yes  
 
Description CNT Instrumentation 
Organisation Dyson
Country United Kingdom 
Sector Private 
PI Contribution We have maintained the partnerships with Dyson and Tortech developed at the beginning of the project. Once the system is complete we will establish the direct engagement of the partners to develop an impact strategy for the research outputs.
Collaborator Contribution Q-Flow will explore the development of the instrumentation technology outputs from the core research programme in an effort to advance the state of their CNT fibre production technology. Dyson will seek to look for applications of the CNT fibres in the development of their future products
Impact Completion of new CNT fibre floating catalysis drawing tower Improved electrical conductivity of CNT fibres drawn from the floating catalysis tower. Improved monitoring of ferrocene catalyst concentration levels. Better understanding the the reaction kinetics within the tower. A technique for remote monitoring of the electrical conductivity of the drawn fibres.
Start Year 2016
 
Description CNT Instrumentation 
Organisation Tortech Nanofibre
Country Israel 
Sector Private 
PI Contribution We have maintained the partnerships with Dyson and Tortech developed at the beginning of the project. Once the system is complete we will establish the direct engagement of the partners to develop an impact strategy for the research outputs.
Collaborator Contribution Q-Flow will explore the development of the instrumentation technology outputs from the core research programme in an effort to advance the state of their CNT fibre production technology. Dyson will seek to look for applications of the CNT fibres in the development of their future products
Impact Completion of new CNT fibre floating catalysis drawing tower Improved electrical conductivity of CNT fibres drawn from the floating catalysis tower. Improved monitoring of ferrocene catalyst concentration levels. Better understanding the the reaction kinetics within the tower. A technique for remote monitoring of the electrical conductivity of the drawn fibres.
Start Year 2016