A Reliable Supply Pla.orm for Graphene & non- carbon 2D Materials

Transcription

1 A Reliable Supply Pla.orm for Graphene & non- carbon 2D Materials Andy Goodwin Commercial Director Advanced Materials Cambridge Graphene Technology Days rd CIR Graphene Business Conference, 6 November

2 Thomas Swan & Co. Ltd. Independently owned manufacturer of speciality chemicals. Medium sized enterprise (SME): 160 employees. ca. 25.4M revenue (2013/14). UK manufacturing base: ConseN, North East England. Export performance: UK/EU/Outside EU Commitment to highest standards.

3 Thomas Swan s CapabiliGes as an SME Established manufacturing infrastructure: Capital Engineering. Quality Control. Environmental Control. Scheduling/LogisGcs. Sales/commercial Underpinned by recognized accreditagons: ISO ISO OHSAS Responsible Care. Regulatory Affairs: Experts in nanomaterials Process Engineering: Process design and pilogng. Flexible chemistries. Proven scale- up experience.

4 Graphene by Direct Liquid ExfoliaGon

5 The high shear exfoliagon process route We selected a scalable high shear exfoliagon route: Ambient condigons. No ultra- sonicagon. No aggressive chemistry. Range of solvents including water. Range of mineral raw materials. Scalable mineral processing. Products are stabilised 2D dispersions and powders. 3D RMs Solvent Dispersant 2D material production Liquid phase exfoliagon Exfoliation of 2D from 3D by high shear. Full sciengfic details have been published: Paton, Coleman et al., Scalable producgon of large quangges of defect- free, few- layer graphene by shear- exfoliagon in liquids Nature Materials Volume: 13, Pages: (2014) Typical Rotor/Stator equipment used for preparing graphene dispersions.

6 The Challenge: Development of a full flow- sheet 2D material production 2D/3D separation Washing Polishing step Quality Assurance 3D RMs Solvent Dispersant Liquid phase exfoliagon Separator Wash unit Polishing Product TesGng 3D RMs surfactant Exfoliation of 2D from 3D by high shear. Separation and recycle of 3D RM. Modulation and control of dispersion concentration Optional fine polishing to control number of layers Product Testing & process monitoring. MulG- step process Proprietary knowledge developed by Thomas Swan Flexibility enabling a range of 2D material specificagons and pricing

7 Elicarb Premium Grade Graphene

8 Elicarb Graphene 1.0 G Graphite D/G 0.5 Intensity (a.u.) 0.5 D /L (µm -1 ) 2D D Raman Shift (cm -1 ) Raman spectra of Elicarb Graphene Powder (532 nm excitagon laser wavelength). The Raman spectrum shows high quality sp 2 network with a typical D/G rago of 0.23 and D/ D normally between 3.5 and 5. TGA to 1100 o C in air of Elicarb Graphene powder exfoliated in water/surfactant shows a small surfactant residue (loss at ca. 300 o C). Primary decomposigon of graphene at 800 o C.

9 Elicarb Graphene TEM Images TEM analysis of Elicarb Graphene Powder showing high quality graphene platelets typical of the liquid exfoliazon process.

10 Elicarb Graphene SEM Images SEM analysis of Elicarb Graphene Powder Allows analysis of larger number of flakes than typical TEM Illustrates relazve uniformity in size and shape of nanoplatelets

11 Elicarb Graphene flake size 500nm scale bar 100nm scale bar TEM analysis of Elicarb Graphene Powder shows very consistent flake size between batches. TEM Image pargcle size analysis of Elicarb Graphene Powder: average X- Y dimension is ca. 1 micron.

12 Thomas Swan Elicarb Graphene Products Sheet Resistance: 4 point probe Filtered solids 5-10 Ω/ for 25µm film Products available today: Bulk ConducZvity: > 500 Siemens/cm has been achieved on deposited films. Graphene platelet thickness: AFM analysis of mean thickness in exfoliated GNPs shows an average plate thickness between 5 and 7 carbon layers. Elicarb Graphene Powder Target applicagons include: Elicarb Graphene Dispersion (AQ) ConducGve inks & coagngs Super- capacitors & bakeries Displays & touch panels ElectrostaGc & thermal management

13 What s Next from Thomas Swan? ConGnuing collaboragve applicagon development with key customers and partners looking forward to engaging with new partners ConGnued process development and scale up as demand dictates. Product extensions Elicarb Materials Grade Graphene Powder and Elicarb Electrical Grade Graphene Dispersion. Non- carbon 2D materials from Thomas Swan, in congnuing collaboragon with Trinity College Dublin.

14 We have developed a range of products Elicarb Grade Product ProperZes ApplicaZons Elicarb Premium Grade Graphene Powder 1 Elicarb Electrical Grade Graphene Powder Elicarb Materials Grade Graphene Powder SP8073P SP8081 SP8082 Few layer graphene platelet, with typical lateral size 1µm. ConducGvity 2 =5-10 Ω/ Few layer graphene platelet, with typical lateral size 1-3 µm. ConducGvity 2 =5-10 Ω/ Few layer graphene platelet, with typical lateral size <5µm. ConducGvity 2 < 20 Ω/ Displays, sensors and device R&D. ConducGve inks, conducgve coagngs, energy storage, thermal management. ThermoplasGcs, composites - conducgvity and mechanical properges. A range of graphene products are now available Advantages Robust and scalable manufacturing process. Highly conducgve Graphene Nanoplatelets (GNPs) and graphigc carbons. Carbon sp 2 layers substangally undamaged and non- oxidised. Contaminants of non- carbon elements such as oxygen and transigon metals are low. Uniform pargcle size.

15 and are extending into other 2D Materials Thomas Swan Direct Liquid ExfoliaGon process is applicable to all 2D materials A broad array of inorganic layered materials exists depending on chemical make- up and structure Rich and versagle properges promise increased applicagon scope Examples: MoS 2 semi- conductor and catalysis. h- BN thermal interface materials, dielectric, barrier.

16 Conclusions: Thomas Swan built on its history and experience as a proven supplier of speciality & performance chemicals. We have developed a reliable scalable route to graphene and other 2D materials. We are acgvely working with customers to understand their needs and further refine our product range. We look forward to future development relagonships supported by Innovate UK and H2020 funding.

17 Advanced Materials Division Reliability and Quality in carbon nanomaterials For further informagon: Please visit our stand today and talk to Andy Goodwin and Paul Ladislaus. swan.co.uk swan.co.uk/advanced- materials

18 The Thomas Swan Commitment: Reliability and Quality in carbon nanomaterials since 2004: Elicarb brand Build on our experience and provide a high quality raw material to applicagon developers. Make R&D and prototyping materials available on commercial terms early. CollaboraZve applicazon development Work collaboragvely with customers in target sectors. Open to a range of collaboragon models and government supported projects. ConZnuing InnovaZon in Nanomaterials Launch of graphene products in 2014 and non- carbon 2D products in Responsible CommercialisaZon Monitoring and implementagon of best pracgce in nanomaterial development, manufacture and supply. Leadership in product registragon and regulatory compliance.

19 Understanding product quality C ontrol C hart - Normalised Sheet Resistance UC L= Individual Value _ X= LC L= Observation Moving Range UC L= 8.65 MR= LC L= Observation Finished product is analysed in- house using a range of techniques. Sheet- resistance used as an applicagon test. We use SPC monitoring to ensure our process remains under control.