Roll-to-roll chemical vapor deposition system makes long sheets of high quality graphene

MIT has combined a roll-to-roll approach — a common industrial approach for continuous processing of thin foils — with the common graphene-fabrication technique of chemical vapor deposition, to manufacture high-quality graphene in large quantities and at a high rate.

The system consists of two spools, connected by a conveyor belt that runs through a small furnace. The first spool unfurls a long strip of copper foil, less than 1 centimeter wide. When it enters the furnace, the foil is fed through first one tube and then another, in a “split-zone” design.

While the foil rolls through the first tube, it heats up to a certain ideal temperature, at which point it is ready to roll through the second tube, where the scientists pump in a specified ratio of methane and hydrogen gas, which are deposited onto the heated foil to produce graphene.

“Graphene starts forming in little islands, and then those islands grow together to form a continuous sheet,” Hart says. “By the time it’s out of the oven, the graphene should be fully covering the foil in one layer, kind of like a continuous bed of pizza.”

The researchers found that they were able to feed the foil continuously through the system, producing high-quality graphene at a rate of 5 centimeters per minute. Their longest run lasted almost four hours, during which they produced about 10 meters of continuous graphene.

They believe the system can be scaled to factories running 24 hours a day with big spools of foil feeding through, like a printing press. This end-to-end process would need to integrate more operations into the manufacturing line. The current demonstration is to generate the interest and funding needed for commercial development.

Once the researchers produced graphene using their roll-to-roll method, they unwound the foil from the second spool and cut small samples out. They cast the samples with a polymer mesh, or support, using a method developed by scientists at Harvard University, and subsequently etched away the underlying copper.

Without polymer support the Graphene will curl up.

Researchers have developed techniques to fabricate graphene membranes and precisely riddle them with tiny holes, or nanopores, the size of which can be tailored to filter out specific molecules.

Applied Material and Interfaces – A Scalable Route to Nanoporous Large-Area Atomically Thin Graphene Membranes by Roll-to-Roll Chemical Vapor Deposition and Polymer Support Casting

Scalable, cost-effective synthesis and integration of graphene is imperative to realize large-area applications such as nanoporous atomically thin membranes (NATMs). Here, they report a scalable route to the production of NATMs via high-speed, continuous synthesis of large-area graphene by roll-to-roll chemical vapor deposition (CVD), combined with casting of a hierarchically porous polymer support. To begin, they designed and built a two zone roll-to-roll graphene CVD reactor, which sequentially exposes the moving foil substrate to annealing and growth atmospheres, with a sharp, isothermal transition between the zones. The configurational flexibility of the reactor design allows for a detailed evaluation of key parameters affecting graphene quality and trade-offs to be considered for high-rate roll-to-roll graphene manufacturing. With this system, they achieve synthesis of uniform high-quality monolayer graphene (ID/IG less than 0.065) at speeds over 5 cm/min. NATMs fabricated from the optimized graphene, via polymer casting and postprocessing, show size-selective molecular transport with performance comparable to that of membranes made from conventionally synthesized graphene. Therefore, this work establishes the feasibility of a scalable manufacturing process of NATMs, for applications including protein desalting and small-molecule separations.

A video shows a custom-built roll-to-roll chemical vapor deposition (CVD) system in a laboratory at MIT, making graphene on copper foil at 1000 Celsius.

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