The possibility to produce and process graphene, related 2D crystals, and heterostructures in the liquid phase makes them promising materials for an ever-growing class of applications as composite materials, sensors, in flexible optoelectronics, and energy storage and conversion. In particular, the ability to formulate functional inks with on-demand rheological and morphological properties, i.e., lateral size and thickness of the dispersed 2D crystals, is a step forward toward the development of industrial-scale, reliable, inexpensive printing/coating processes, a boost for the full exploitation of such nanomaterials. Here, the exfoliation strategies of graphite and other layered crystals are reviewed, along with the advances in the sorting of lateral size and thickness of the exfoliated sheets together with the formulation of functional inks and the current development of printing/coating processes of interest for the realization of 2D-crystal-based devices.

2D-Crystal-Based Functional Inks

There are now numerous emerging flexible and wearable sensing technologies that can perform a myriad of physical and physiological measurements. Rapid advances in developing and implementing such sensors in the last several years have demonstrated the growing significance and potential utility of this unique class of sensing platforms. Applications include wearable consumer electronics, soft robotics, medical prosthetics, electronic skin, and health monitoring. In this review, we provide a state-of-the-art overview of the emerging flexible and wearable sensing platforms for healthcare and biomedical applications. We first introduce the selection of flexible and stretchable materials and the fabrication of sensors based on these materials. We then compare the different solid-state and liquid-state physical sensing platforms and examine the mechanical deformation-based working mechanisms of these sensors. We also highlight some of the exciting applications of flexible and wearable physical sensors in emerging healthcare and biomedical applications, in particular for artificial electronic skins, physiological health monitoring and assessment, and therapeutic and drug delivery. Finally, we conclude this review by offering some insight into the challenges and opportunities facing this field.

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Emerging flexible and wearable physical sensing platforms for healthcare and biomedical applications

© 2020 The Author(s). We present an overview of the main techniques for production and processing of graphene and related materials (GRMs), as well as the key characterization procedures. We adopt a 'hands-on' approach, providing practical details and procedures as derived from literature as well as from the authors' experience, in order to enable the reader to reproduce the results. Section I is devoted to 'bottom up' approaches, whereby individual constituents are pieced together into more complex structures. We consider graphene nanoribbons (GNRs) produced either by solution processing or by on-surface synthesis in ultra high vacuum (UHV), as well carbon nanomembranes (CNM). Production of a variety of GNRs with tailored band gaps and edge shapes is now possible. CNMs can be tuned in terms of porosity, crystallinity and electronic behaviour. Section II covers 'top down' techniques. These rely on breaking down of a layered precursor, in the graphene case usually natural crystals like graphite or artificially synthesized materials, such as highly oriented pyrolythic graphite, monolayers or few layers (FL) flakes. The main focus of this section is on various exfoliation techniques in a liquid media, either intercalation or liquid phase exfoliation (LPE). The choice of precursor, exfoliation method, medium as well as the control of parameters such as time or temperature are crucial. A definite choice of parameters and conditions yields a particular material with specific properties that makes it more suitable for a targeted application. We cover protocols for the graphitic precursors to graphene oxide (GO). This is an important material for a range of applications in biomedicine, energy storage, nanocomposites, etc. Hummers' and modified Hummers' methods are used to make GO that subsequently can be reduced to obtain reduced graphene oxide (RGO) with a variety of strategies. GO flakes are also employed to prepare three-dimensional (3d) low density structures, such as sponges, foams, hydro- or aerogels. The assembly of flakes into 3d structures can provide improved mechanical properties. Aerogels with a highly open structure, with interconnected hierarchical pores, can enhance the accessibility to the whole surface area, as relevant for a number of applications, such as energy storage. The main recipes to yield graphite intercalation compounds (GICs) are also discussed. GICs are suitable precursors for covalent functionalization of graphene, but can also be used for the synthesis of uncharged graphene in solution. Degradation of the molecules intercalated in GICs can be triggered by high temperature treatment or microwave irradiation, creating a gas pressure surge in graphite and exfoliation. Electrochemical exfoliation by applying a voltage in an electrolyte to a graphite electrode can be tuned by varying precursors, electrolytes and potential. Graphite electrodes can be either negatively or positively intercalated to obtain GICs that are subsequently exfoliated. We also discuss the materials that can be amenable to exfoliation, by employing a theoretical data-mining approach. The exfoliation of LMs usually results in a heterogeneous dispersion of flakes with different lateral size and thickness. This is a critical bottleneck for applications, and hinders the full exploitation of GRMs produced by solution processing. The establishment of procedures to control the morphological properties of exfoliated GRMs, which also need to be industrially scalable, is one of the key needs. Section III deals with the processing of flakes. (Ultra)centrifugation techniques have thus far been the most investigated to sort GRMs following ultrasonication, shear mixing, ball milling, microfluidization, and wet-jet milling. It allows sorting by size and thickness. Inks formulated from GRM dispersions can be printed using a number of processes, from inkjet to screen printing. Each technique has specific rheological requirements, as well as geometrical constraints. The solvent choice is critical, not only for the GRM stability, but also in terms of optimizing printing on different substrates, such as glass, Si, plastic, paper, etc, all with different surface energies. Chemical modifications of such substrates is also a key step. Sections IV-VII are devoted to the growth of GRMs on various substrates and their processing after growth to place them on the surface of choice for specific applications. The substrate for graphene growth is a key determinant of the nature and quality of the resultant film. The lattice mismatch between graphene and substrate influences the resulting crystallinity. Growth on insulators, such as SiO2, typically results in films with small crystallites, whereas growth on the close-packed surfaces of metals yields highly crystalline films. Section IV outlines the growth of graphene on SiC substrates. This satisfies the requirements for electronic applications, with well-defined graphene-substrate interface, low trapped impurities and no need for transfer. It also allows graphene structures and devices to be measured directly on the growth substrate. The flatness of the substrate results in graphene with minimal strain and ripples on large areas, allowing spectroscopies and surface science to be performed. We also discuss the surface engineering by intercalation of the resulting graphene, its integration with Si-wafers and the production of nanostructures with the desired shape, with no need for patterning. Section V deals with chemical vapour deposition (CVD) onto various transition metals and on insulators. Growth on Ni results in graphitized polycrystalline films. While the thickness of these films can be optimized by controlling the deposition parameters, such as the type of hydrocarbon precursor and temperature, it is difficult to attain single layer graphene (SLG) across large areas, owing to the simultaneous nucleation/growth and solution/precipitation mechanisms. The differing characteristics of polycrystalline Ni films facilitate the growth of graphitic layers at different rates, resulting in regions with differing numbers of graphitic layers. High-quality films can be grown on Cu. Cu is available in a variety of shapes and forms, such as foils, bulks, foams, thin films on other materials and powders, making it attractive for industrial production of large area graphene films. The push to use CVD graphene in applications has also triggered a research line for the direct growth on insulators. The quality of the resulting films is lower than possible to date on metals, but enough, in terms of transmittance and resistivity, for many applications as described in section V. Transfer technologies are the focus of section VI. CVD synthesis of graphene on metals and bottom up molecular approaches require SLG to be transferred to the final target substrates. To have technological impact, the advances in production of high-quality large-area CVD graphene must be commensurate with those on transfer and placement on the final substrates. This is a prerequisite for most applications, such as touch panels, anticorrosion coatings, transparent electrodes and gas sensors etc. New strategies have improved the transferred graphene quality, making CVD graphene a feasible option for CMOS foundries. Methods based on complete etching of the metal substrate in suitable etchants, typically iron chloride, ammonium persulfate, or hydrogen chloride although reliable, are time- and resourceconsuming, with damage to graphene and production of metal and etchant residues. Electrochemical delamination in a low-concentration aqueous solution is an alternative. In this case metallic substrates can be reused. Dry transfer is less detrimental for the SLG quality, enabling a deterministic transfer. There is a large range of layered materials (LMs) beyond graphite. Only few of them have been already exfoliated and fully characterized. Section VII deals with the growth of some of these materials. Amongst them, h-BN, transition metal tri- and di-chalcogenides are of paramount importance. The growth of h-BN is at present considered essential for the development of graphene in (opto) electronic applications, as h-BN is ideal as capping layer or substrate. The interesting optical and electronic properties of TMDs also require the development of scalable methods for their production. Large scale growth using chemical/physical vapour deposition or thermal assisted conversion has been thus far limited to a small set, such as h-BN or some TMDs. Heterostructures could also be directly grown.

Production and processing of graphene and related materials

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Fundamentals Of Analytical Chemistry

Graphene is the first 2D crystal ever isolated by mankind. It consists of a single graphite layer, and its exceptional properties are revolutionizing material science. However, there is still a lack of convenient mass-production methods to obtain defect-free monolayer graphene. In contrast, graphene nanoplatelets, hybrids between graphene and graphite, are already industrially available. Such nanomaterials are attractive, considering their planar structure, light weight, high aspect ratio, electrical conductivity, low cost, and mechanical toughness. These diverse features enable applications ranging from energy harvesting and electronic skin to reinforced plastic materials. This review presents progress in composite materials with graphene nanoplatelets applied, among others, in the field of flexible electronics and motion and structural sensing. Particular emphasis is given to applications such as antennas, flexible electrodes for energy devices, and strain sensors. A separate discussion is included on advanced biodegradable materials reinforced with graphene nanoplatelets. A discussion of the necessary steps for the further spread of graphene nanoplatelets is provided for each revised field.

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Graphene Nanoplatelets-Based Advanced Materials and Recent Progress in Sustainable Applications

A novel type of a broadband flexible electromagnetic absorbing panel made of a resistive pattern printed on a dielectric spacer backed by a conducting surface is investigated in this paper. It is shown that an appropriate choice of the shape and sheet resistance of the pattern allows extending an absorption spectrum up to an octave and beyond, which is very competitive over alternative solutions. The pattern is made of ink with graphene nano-platelets, which allows achieving expected sheet resistance with decent repeatability, what is confirmed with measurements undertaken with the DC point probe and microwave dielectric resonator techniques. An exemplary sample of the proposed absorber is manufactured and characterized, indicating a very good agreement between theoretical study and experiments.

A Broadband Absorber With a Resistive Pattern Made of Ink With Graphene Nano-Platelets

This paper describes the design and measurements of a remote frequency identification (RFID) tag built of a graphene-based dipole antenna and a chip operating in the ultrahigh-frequency (UHF) band in accordance with the EPC Global Class 1 Gen 2 standard A custom-designed antenna has been designed first Then, it was used to construct several tags that have been tested with a standard RFID reader to reveal that each one is fully operational, although the interrogation range for the graphene-based circuits has been limited in comparison to copper antennas This can be attributed to increased sheet resistance of a graphene layer and—in the case of tags fabricated on paper—also to significant dielectric losses of the substrate material However, it seems that for applications where the interrogation range is not crucial the novel antenna can be an alternative to much more expensive circuits printed with silver-based inks

Graphene-Based Dipole Antenna for a UHF RFID Tag

Polymer composites with nanomaterials such as graphene nanoplatelets and carbon nanotubes are a new group of materials with high application possibilities in printed and flexible electronics. In this study such carbon nanomaterials were used as a conductive phase in polymer composites. Pastes with dispersed nanomaterials in PMMA and PVDF vehicles were screen printed on flexible substrates, and used as an active layer in pressure sensors, exploiting contact resistance phenomena. The relationship between resistance and pressure is nearly linear on a logarithmic scale for selected types of samples, and their response is several times higher than for similar sensors with graphite layers. The use of surfactants allowed us to fabricate evenly dispersed nanomaterials with different amount of nanoplatelets and nanotubes in the composites. The samples contained from 1.25 wt.% to 2 wt.% of graphene and 1 wt.% to 0.5 wt.% of nanotubes and exhibited diverse sheet resistivity. Experiments revealed the relationship between morphology and loading of functional phase in the polymer matrix and the sensors' sensitivity.

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Screen-printed resistive pressure sensors containing graphene nanoplatelets and carbon nanotubes.

Inkjet printing is an excellent printing technique and an attractive alternative to conventional technologies for the production of flexible, low-cost microelectronic devices. Among many parameters that have a significant impact on the correctness of the printing process, the most important is ink viscosity. During the printing process, the ink is influenced by different strains and forces, which significantly change the printing results. The authors present a model and calculations referring to the shear rate of ink in an inkjet printer nozzle. Supporting experiments were conducted, proving the model assumptions for two different ink formulations: initial ink and with the addition of a dispersing agent. The most important findings are summarized by the process window regime of parameters, which is much broader for the inks with a dispersing agent. Such inks exhibit preferable viscosity, better print-ability, and higher path quality with lower resistivity. Presented results allow stating that proper, stable graphene inks adjusted for inkjet technique rheology must contain modifiers such as dispersing agents to be effectively printed.

Efficient Inkjet Printing of Graphene-Based Elements: Influence of Dispersing Agent on Ink Viscosity

Purpose – New types of substrates were used for fabrication of printed electroluminescent structures. Polymer foils mainly used as substrates for such optoelectronic elements were replaced with paper and textiles. Printing on non-transparent substrate requires elaboration of printed transparent electrode, while usually polyester foils with sputtered ITO transparent electrodes are used. The paper aims to discuss these issues. Design/methodology/approach – Electroluminescent structures were fabricated with elaborated polymer compositions filled with nanomaterials, such as carbon nanotubes and graphene platelets, dielectric and luminophore nanopowders. Structures were printed as “reverse stack”, where transparent electrode is printed on top of the last luminophore layer. For that carbon nanotubes and graphene platelets filled composition was used, deposited with spray-coating technique. Findings – Main issue with new substrates is proper wetting with the use of screen-printing pastes, and much higher roughne...

Daniel Janczak

Papers

A Broadband Absorber With a Resistive Pattern Made of Ink With Graphene Nano-Platelets

Graphene-Based Dipole Antenna for a UHF RFID Tag

Screen-printed resistive pressure sensors containing graphene nanoplatelets and carbon nanotubes.

Efficient Inkjet Printing of Graphene-Based Elements: Influence of Dispersing Agent on Ink Viscosity

Electroluminescent structures printed on paper and textile elastic substrates