nanoparticles automated systems for nanoparticle synthesis Syrris - High quality, control and precision in nanochemistry

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1 nanoparticles automated systems for nanoparticle synthesis Syrris - High quality, control and precision in nanochemistry

2 Why choose Syrris for nanoparticle synthesis? Syrris offers a wide range of innovative batch and flow reactors for nanoparticle synthesis. The award-winning systems, designed by chemists for chemists, present multiple benefits: nanoparticles Narrow particle size distribution: Excellent mixing and temperature control leads to improved homogeneity of particle size Rapid nanoparticle optimization: Process conditions such as temperature, time, mixing, reagent ratios and concentrations can be quickly varied Reproducibility and automation: Additions, mixing, temperature, etc. can be fully controlled in automated fashion for seamless reproducibility Easy to use: All products can be assembled, maintained and cleaned without tools Simple scale up: Large range of reactor sizes (batch) and flow rates (continuous flow) provides the tools for moving from small scale process optimization to production Nanoparticles not possible by other means: Nanoparticles previously unseen using batch techniques can be obtained in microreactors due to the high level of control Types of nanoparticles 4 Overview of nanochemistry 6 Key options for nanoparticle synthesis 8-9 Batch chemistry systems 10 Flow chemistry systems 11 Case studies Nickel nanocubes, pyramids and tetrapods 12 Gold nanoparticle synthesis 13 Quantum dots (iron oxide core with gold shell) 14 Platinum nanoparticle synthesis 15

3 Examples of nanoparticles The list below shows a selection of nanoparticles synthesized in Syrris reactor systems and the unique advantages they have offered: Nickel nanocubes: Ability to accurately select desired shape. High quality material obtained. Cadmium selenide quantum dots: Synthesis, capping and functionalization done in one continuous process. Large scale synthesis. Silver nanowires: Excellent monodispersity. Improved electric conductivity property. Superparamagnetic iron nanoparticles: Small particle size. Fast throughput. Gold nanocrystals: Smaller average particle size obtained in flow. Easy process optimization. Nickel tetrapods: Previously unreported shape. Only seen in microreactors. Silica beads: Narrow size distribution. High reproducibility. Titanium oxide nanoparticles: Faster synthesis. Excellent yields. Platinum nanoparticles deposited on carbon fibers: And many more... Synthesis and deposition performed in one cycle. Control of the size by varying flow rate. For more examples, visit:

4 overview of nanoparticle synthesis Nanochemistry includes the synthesis, characterization and reaction of materials at nanoscale. Nanoparticles can offer a wide range of advantages over regular materials including unique or superior properties such as magnetic, optical, physical, electric, etc. Control of process parameters in nanochemistry is essential to ensure the desired shape, size, composition, surface structure and thus desired properties. Key synthesis parameters include temperature, mixing, concentrations and reaction time.

5 Key options for nanoparticle synthesis Technique Description Advantages Systems BATCH Classic way to do chemistry Reagents are loaded into the reactor, mixed and left to react The products are collected at the end, after the reaction has been completed and worked-up. Batch rectors Multiple sensors can be used for control (temperature, ph, turbidity, etc...), No particle size restrictions Easy scale-up globe reactions made easy Key factors: concentration, mixing, temperature, reaction time For more advantages in batch synthesis, visit: Atlas Chemical Reactors A range of modular, fully automated chemistry systems for processes in jacketed reactors, flasks or vials Globe Jacketed Reactors A jacketed chemical reactor system from 50ml to 5L that saves time, money and space FLOW New technique Reagent streams are continuously pumped into the flow reactor Reagents mix and react in the flow reactor The product leaves the reactor as a continuous stream Flow reactors Fast and reproducible mixing Excellent heat transfer and accurate temperature control Suitable for optimization and product on same system Asia Flow Chemistry The future of flow chemistry. An award winning modular system. africa automated flow chemistry Key factors: residence time (flow rates), mixing, pressure, temperature For more advantages in flow synthesis, visit: Africa Flow Chemistry A fully automated, flexible and easy-to-use microreactor system

6 Atlas is a revolutionary range of modular products, which can form a wide range of lab reactors. Atlas offers manual or automated control of one or many reactions at a time with volumes from 5 litres to 1ml in jacketed reactors, flasks or vials. Asia is an award-winning range of flow chemistry products from Syrris. It has been designed by chemists for chemists to enable the widest variety of chemical reactions and ultimate ease of use. Experiments can be manually controlled or fully automated. Example Atlas Systems Learn more at Self-aligning overhead stirring up to 800 rpm Stacking Dry Bath for heating of flasks from 50ml to 2L Temperature control with Hotplate up to +350 C Wide range of sensors available: temperature, ph, pressure, turbidity, FTIR Pressures from vacuum to 3 bar (glass) or 200 bar (metal) Full data logging The intelligent base allows direct control, automated experiments without a PC or full software control Capability to run step by step process Temperature control from -90 C to +250 C Safety auto shutdown, alarms and controls based on sensors Jacketed reactors from 50ml to 5L from process optimization to small-scale production Wide range of stirrer shapes with speeds up to 2000 rpm Accurate automated dosing and sampling of liquids Example Asia System Learn more at Asia Pressurized Input Store This enables the use of air sensitive reagents and eliminates bubbles when pumping Asia Pump Flow rate: 1μl - 10ml/min Smooth pumping for accurate control of stoichiometry and residence time Automated blockage detection and shut down Tube reactors Fluoropolymer or stainless steel 4ml, 16ml Up to 250 C Ideal for scale-up Asia Reagent Injector Fast process optimization using small samples Asia Product Collector Continuous collection of one or many nanoparticle samples Glass microreactors 62.5μl, 250μl, 1ml Controlled from -15 C to +250 C Excellent reproducible mixing and heat transfer Asia Pressure Controller Automatically pressurizes the reaction up to 20 bar allowing temperatures C above atmospheric boiling point

7 Case study 1: Fast synthesis of nickel nanocubes, pyramids and tetrapods Case study 2: Gold nanoparticle synthesis for biotechnology application Bar Ilan University, a world leader in nanotechnology, uses Syrris Asia and microreactor technology for the synthesis of nickel nanoparticles in a continuous flow fashion. Biotechnology company Midatech Biogune is taking advantage of Syrris Atlas Potassium reactor systems to produce custom-made functionalized gold nanoparticles for medical use. Flow Chemistry System Asia 210 is an ideal flow chemistry system for the synthesis of nanoparticles Nickel nanoparticles are synthesized by thermal decomposition of a of Ni(COD) 2 in the presence of 1-hexadecylamine in a Syrris glass microreactor. The accurate control of mixing, residence time and temperature control achieved in a Syrris microreactor enables selective synthesis of different shapes of nickel nanocrystals (spheres, rod, triangles, cubes, tetrapods). Midatech use a Brust like method where a solution of HAuCl 4 is reduced by addition of NaBH 4. The Atlas system enables accurate temperature and ph control with automatic addition of the reducing agent using an Atlas Pump. This ensures excellent reproducibility and complete automation. Batch Chemistry System Atlas jacketed reactors plus the Atlas syringe pump are used to enable accurate temperature and ph control for gold nanoparticle synthesis Our Atlas Potassium reactors, with ph control and an Atlas Syringe Pump XL, have allowed us to scale-up production, enabling variables such as ph and temperature to be tightly controlled. Each route has the ability to yield a preferential shape based on kinetic control of crystal growth. Tetrapods are obtained only in a microfluidic reactor. It is a reliable and reproducible reactor system that is well assembled, compact and portable, and performs exactly as we were told it would. Meital Shviro and David Zitoun, RSC Adv., 2013, 3, Justin Barry, CEO of Midatech Biogune

8 Case Study 3: Quantum dots (Iron oxide core with gold shell) Argentinian National Institute of Industrial Technologies was investigating the ideal technology for synthesizing quantum dots. They were interested in controlling the size of the iron oxide nanoparticle core as this is a critical parameter which dictates the paramagnetic properties of the particles. Case Study 4: Platinum nanoparticle synthesis and deposition on carbon fibers AGH University of Science and Technology in Poland used Syrris flow chemistry technology to perform several steps in one continuous process allowing synthesis, stabilization and deposition of nanoparticles in one cycle. The Fe 2 O 3 nanoparticles were synthesized by oxidation of a Fe 3 O 4 solution using ammonium hydroxide. The reaction was performed on a Syrris Asia 310 system in a glass microreactor, enabling precise control and reproducibility of reaction temperature and mixing. The second step of the process (encapsulating in gold shell) can be subsequently performed using a second microreactor in completely automated and continuous fashion. A glass microreactor is used for making platinum nanoparticles with a 3.5-5nm diameter. The starting mixture of Pt (IV) is reduced with sodium borohydride then polvinyl alcohol stabilizer is added and finally the particles are deposited on active carbon fibers. The effortless control of reaction temperature and residence time allows to selectively form nanoparticles of either 3.5nm or 5nm average size. See this reaction being performed, visit: We trialled our nanoparticle experiments on the Asia flow chemistry system during a visit to Syrris UK facilities, and immediately placed an order for our own system to optimize the speed and results of our synthesis workflow. Paulina Lloret, Researcher at INTI The synthesis of PtNPs and their deposition on ACFs is possible in a short time, in one cycle. The use of a microreactor, besides making easier catalyst production, also has many advantages compared to the batch system, such as better mixing, mass and heat transport. Magdalena Luty-Blocho, Marek Wojnicki, Krzysztof Paclawski & Krzysztof Fitzner, Chemical Engineering Journal 226, 2013, 46-51

9 Syrris chemistry systems and micromixers are ideally suited to nanochemistry, including nanoparticle synthesis. Syrris network of offices in the UK, USA, Japan, India and Brazil plus over 35 distributors worldwide offer local service and support. Contact us now at: John Morris Scientific e: t: Freecall AUS t: Freecall NZ Authorised Australian Distributor: Syrris Ltd. (Europe and Rest of World) T: +44 (0) E: W: Syrris Japan, Inc. T: E: W: Syrris India T: E: W: Syrris Inc. (North America) T: E: W: Syrris Brasil T: E: W: V1.0