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PolyGraph Report Summary

Project ID: 604143
Funded under: FP7-NMP
Country: United Kingdom

Periodic Report Summary 2 - POLYGRAPH (Up-Scaled Production of Graphene Reinforced Thermosetting Polymers for Composite, Coating and Adhesive Applications)

Project Context and Objectives:
The concept of PolyGraph is to develop new production techniques, which will deliver industrial scale quantities of graphene-reinforced thermosetting polymers. These materials will be suitable for use in a number of key applications where improvements are needed in the strength, stiffness, toughness, electrical conductivity and thermal and barrier properties of polymers; such as fibre-reinforced composite resins, coatings and adhesives.

Interest in graphene and its potential uses has grown rapidly since 2004, when the material was first isolated using the now famous “Scotch tape” method by Professors Andre Geim and Konstantin Novoselov at the University of Manchester.

An area of particular significance is graphene-reinforced polymers. After several years of research in the area, it is now well known that the addition of small quantities of graphene can simultaneously provide significant improvements in strength, toughness and electrical and thermal conductivity to a number of polymers. This has raised expectation levels with many industries, such as polymer composites, coatings and adhesives, which are keen to exploit the excellent properties of graphene in order to produce high performance polymer components. However, it remains the case that there are no techniques suitable for industrial-scale production of graphene-reinforced polymers.

Specifically, the following issues remain:
• Current graphene production processes are typically low yield, energy intensive, time consuming and often use large amounts of solvent
• As a result, the cost of graphene remains prohibitively expensive for many industries
• Incorporation and uniform distribution of graphene in low-viscosity thermosetting polymers has not yet been demonstrated on an industrial scale
• Conventional composite, coating and adhesive processing techniques have not yet been optimised to ensure that graphene remains uniformly distributed during processing

PolyGraph will address these issues by developing two new routes to industrial-scale quantities of graphene-reinforced thermosetting polymers; both starting from a relatively inexpensive expanded graphite starting material. In the first route, we will develop new chemical and mechano-chemical methods to exfoliate the expanded graphite and produce graphene. Alongside this, we will develop the equipment and techniques necessary to disperse the graphene into low-viscosity thermosetting polymer resins in a uniform, consistent and scalable basis. Our second route will go a step further and will develop the equipment and techniques to enable in-situ exfoliation of the expanded graphite and dispersion of the resulting graphene in a single operation, directly in the low-viscosity thermosetting polymer resins.

A further aim is to optimise techniques for the production of fibre-reinforced composites, adhesives and coatings, to ensure that the graphene remains well distributed in the final part.

As a result, we will significantly lower the overall cost of these materials and make them viable for use in the wider composites, coatings and adhesives industries.

Project Results:
During the 2nd period of the project all the technical work packages have been active. Work Package 2 has delivered novel graphite grades suitable for subsequent exfoliation and graphene for dispersion in thermosetting polymers. Since the beginning of the project novel grades of graphite (synthetic graphite, expanded graphite and nano-graphite) and graphene (mono and few layer) platelets have been developed and produced in a reasonable scale suitable for the rest of the consortium. The production of selected materials has been optimized to increase the production capacity and to meet the needs of the tasks of the other Work Packages. Functionalization of some materials has been performed with the aim of increasing the compatibility with epoxy resin and increase dispersibility.
For Work package 3: “Development and Up-scaling of Exfoliation Techniques and Equipment”, in-situ exfoliation trials were carried out with the most promising graphite grades that were defined by the Consortium. An experiment set-up has been defined for future scale-up.
In WP4 “Formulation of Graphene and Graphite filled polymers for adhesive applications” the following has been addressed. Epoxy and PU formulations have been developed to benchmark against current adhesives in use. The formulations have been modified to enable maximum loading of Carbon.
“Formulation of Graphene and Graphite filled polymers for coating applications”.
HMG paints have incorporated and measured the effects of Graphite and Graphene into solvent based paint, the increase in viscosity expected has been mitigated by the use of hyper-dispersant. Tests are ongoing.
“Formulation of Graphene and Graphite filled polymers for composite applications” Different epoxy systems have been developed for different composite manufacturing techniques.
WP5 has been developing the adhesive, coating and composite formulations that are being developed as part of WP4 to ensure the materials are optimised and suitable for product level manufacturing processes. In task 5.1 the end-users, plus formulators and science partners have worked in collaboration to evaluate and improve the suitability of the developing adhesives, coatings and composite matrices for deployment by the end-users under representative production environments, scales and processing equipment. In tasks 5.2 improvements, optimisations and innovative solutions have been considered to ensure the highest quality and reproducibility. Appropriate testing and analysis of the mechanical, electrical and morphological characteristics have been under concurrent evaluation as part of task 5.3.

WP7 has focused on the identification of potential hazards and exposure routes associated with the materials, tasks and activities within the scope of the PolyGraph project. Information gained will be used to inform the in vitro study design (Task 7.2) and to identify a set of exposure scenarios for further assessment (Task 7.3). To achieve these objectives the task was split into three distinct sub-tasks: Exposure Scenarios Review, Workplace Questionnaire and a Hazard Review. Findings from the literature review and workplace questionnaire were combined and appraised to inform an overall identification of exposure-prone activities and tasks.
Screening Comparative LCI to Support the Selection of New Graphene Polymer Formulations: An initial comparative screening of material, energy used, and impact from cradle to gate was performed in accordance with Provision 6.10 V in the ICLD handbook to consider environmental impact in the selection of graphene types, thermosetting polymers, and graphene production technologies. The data used in this screening was collected from the project partners via a questionnaire and follow-up questions, together with database records and scientific literature.
In WP8 (dissemination & exploitation): A visual identity was created and the main project website at is updated as information is made available. Several new pages were added to the website including a News section, an Aims & Objectives section, and an overview of the Industrial Stakeholder group.
Other dissemination materials were produced which detail the aims, objectives, development and expected outcomes of the project.
Task 8.4 (Screening Comparative Life Cycle Costing (LCC) Analysis): In this screening LCC, graphene flakes and SWNT were assessed.

Potential Impact:
The ultimate aim of PolyGraph is to develop a process in which graphene can be produced and dispersed “in-situ” within thermosetting polymer resins, using relatively inexpensive expanded graphite as a starting material.

To achieve this a staged approach will be used to reach this ambitious goal, starting with production of graphene via new chemical and mechano-chemical methods and its subsequent dispersion in thermosetting resins. This will then be followed by further development and modification of existing mixing and dispersion equipment to enable the exfoliation of expanded graphite to be carried out directly in thermosetting polymers.

A further aim is to optimise techniques for the production of fibre-reinforced composites, adhesives and coatings, to ensure that the graphene remains well distributed in the final part.

As a result, we will significantly lower the overall cost of these materials and make them viable for use in the wider composites, coatings and adhesives industries

To achieve this the following specific objectives have been set:
• Produce grades of specially designed graphite suitable for subsequent processing
• Use the new graphite to produce graphene via chemical and mechano-chemical methods
• Develop the equipment and processes to exfoliate and disperse graphene in thermosetting resins
• Utilise state of the art methods to monitor the dispersion process
• Develop, optimise and test the resin formulations for use in composites, adhesives and coatings
• Optimise fibre-reinforced composite, coating and adhesive production techniques such that the graphene remains well-dispersed during component production
• Scale-up of the novel equipment and production techniques
• Produce and test four demonstrator parts for key sectors (e.g. aerospace and automotive)
• Carry out health, environmental, and economic assessment in a life cycle context for the newly developed materials and processes
• Close the price-performance gap which currently exists for commercially available graphene

These breakthroughs will allow the adoption of graphene functionalised thermosetting resins in composites, coatings and adhesives across a broad spectrum of industry sectors and will place European businesses at the forefront of this technology allowing them to access new and emerging markets.

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