Electromagnetic field controlled domain wall displacement for induced strain tailoring in BaTiO3-epoxy nanocomposite

Scientific Reports 12, 7504 (2022)


Failure in an epoxy polymer composite material is prone to initiate by the coalescence of microcracks in its polymer matrix. As such, matrix toughening via addition of a second phase as rigid or/and rubber nano/micro-particles is one of the most popular approaches to improve the fracture toughness across multiple scales in a polymer composite, which dissipates fracture energy via deformation mechanisms and microcracks arrest. Few studies have focused on tailorable and variable toughening, so-called ‘active toughening’, mainly suggesting thermally induced strains which offer slow and irreversible toughening due to polymer’s poor thermal conductivity. The research presented in the current article has developed an instantaneous, reversible extrinsic strain field via remote electromagnetic radiation. Quantification of the extrinsic strain evolving in the composite with the microwave energy has been conducted using in-situ real-time fibre optic sensing. A theoretical constitutive equation correlating the exposure energy to micro-strains has been developed, with its solution validating the experimental data and describing their underlying physics. The research has utilised functionalised dielectric ferroelectric nanomaterials, barium titanate (BaTiO3), as a second phase dispersed in an epoxy matrix, able to introduce microscopic electro-strains to their surrounding rigid epoxy subjected to an external electric field (microwaves, herein), as result of their domain walls dipole displacements. Epoxy Araldite LY1564, a diglycidyl ether of bisphenol A associated with the curing agent Aradur 3487 were embedded with the BaTiO3 nanoparticles. The silane coupling agent for the nanoparticles’ surface functionalisation was 3-glycidoxypropyl trimethoxysilane (3-GPS). Hydrogen peroxide (H2O2, 30%) and acetic acid (C2H4O2, 99.9%) used as functionalisation aids, and the ethanol (C2H6O, 99.9%) used for BaTiO3 dispersion. Firstly, the crystal microstructure of the functionalised nanoparticles and the thermal and dielectric properties of the achieved epoxy composite materials have been characterised. It has been observed that the addition of the dielectric nanoparticles has a slight impact on the curing extent of the epoxy. Secondly, the surface-bonded fibre Bragg grating (FBG) sensors have been employed to investigate the real-time variation of strain and temperature in the epoxy composites exposed to microwaves at 2.45 GHz and at different exposure energy. The strains developed due to the in-situ exposure at composite, adhesive and their holding fixture material were evaluated using the FBG. The domain wall induced extrinsic strains were distinguished from the thermally induced strains, and found that the increasing exposure energy has an instantaneously increasing effect on the development of such strains. Post-exposure Raman spectra showed no residual field in the composite indicating no remnant strain field examined under microwave powers < 1000 W, thus suggesting a reversible strain introduction mechanism, i.e. the composite retaining its nominal properties post exposure. The dielectric composite development and quantifications presented in this article proposes a novel active toughening technology for high-performance composite applications in numerous sectors.

Accelerated Testing and Reliability of FDM-Based Structural Electronics

Applied Sciences 12(3), 1110 (2022)

With the development of the miniaturization of electronic systems, heat dissipation from components has become an increasing challenge. Structural electronics represent a new approach to this problem. Instead of downsizing all the elements, in this idea, electronic parts of the device are embedded into its mechanical construction. This approach has many advantages, but the reliability of systems constructed this way has not been extensively studied so far. In this work, circuits consisting of silver ink conductive traces were printed on FDM polymer substrates, with or without 0 Ω resistors, and were subjected to accelerated aging testing. The samples were divided into three groups, and for each of them, the mean time to failure was calculated, which for the best group was 8000 h. This paper also presents the mechanism that led to the failure of these systems, as well as actions that will lead to the elimination of this phenomenon.

Electrically Conductive Nanocomposite Fibers for Flexible and Structural Electronics

Applied Sciences 12(3), 941 (2022)

The following paper presents a simple, low-cost, and repeatable manufacturing process for fabricating conductive, elastic carbon-elastomer nanocomposite fibers for applications in the textile industry and beyond. The presented method allows for the manufacturing of fibers with a diameter of 0.2 mm, containing up to 50 vol. % of graphite powder, 10 vol. % of CNT, and a mix of both fillers. As a result, resistivity below 0.2 Ωm for the 0.2 mm-diameter fibers was achieved. Additionally, conductive fibers are highly elastic, which makes them suitable for use in the textile industry as an element of circuits. The effect of strain on the change in resistance was also tested. Researches have shown that highly conductive fibers can withstand strain of up to 40%, with resistivity increasing nearly five times compared to the unstretched fiber. This research shows that the developed composites can also be used as strain sensors in textronic systems. Finally, functional demonstrators were made by directly sewing the developed fibers into a cotton fabric. First, the non-quantitative tests indicate the feasibility of using the composites as conductive fibers to power components in textronic systems and for bending detection.

Highly conductive electronics circuits from aerosol jet printed silver inks

Scientific Reports 11, 18141 (2021)

Recently, low-cost electronics printed on lightweight, flexible and 3D shaped substrates are gaining importance in the markets of wearables and smart packaging. However, printed electronics do not meet the electrical performance of subtractive techniques because the resistivity of metallic printed patterns is still much higher than that of bulk material. To fulfil this need, low-resistive and easy printable inks for high resolution printed electronics techniques are needed. In this work, parameters of silver nanoparticles ink for micro-scale printed electronics technique, Aerosol Jet Printing, are being enhanced. To increase electrical conductivity and enhance printability, surfactants and dispersing agents were used to increase ultrasonic atomisation efficiency, obtain a uniform structure of printed lines, and narrow the width of printed patterns. Electrical measurements show a decrease in resistivity value in samples enhanced by cationic and non-ionic surfactants, by 95%, compared to initially prepared inks. Surfactant additions to silver nanoparticles Aerosol Jet Printing ink show promising features for application in modern electronics.

Are We Able to Print Components as Strong as Injection Molded?—Comparing the Properties of 3D Printed and Injection Molded Components Made from ABS Thermoplastic

Applied Sciences 2021, 11(15), 6946

In this paper, we are focusing on comparing results obtained for polymer elements manufactured with injection molding and additive manufacturing techniques. The analysis was performed for fused deposition modeling (FDM) and single screw injection molding with regards to the standards used in thermoplastics processing technology. We argue that the cross-section structure of the sample obtained via FDM is the key factor in the fabrication of high-strength components and that the dimensions of the samples have a strong influence on the mechanical properties. Large cross-section samples, 4 × 10 mm2, with three perimeter layers and 50% infill, have lower mechanical strength than injection molded reference samples—less than 60% of the strength. However, if we reduce the cross-section dimensions down to 2 × 4 mm2, the samples will be more durable, reaching up to 110% of the tensile strength observed for the injection molded samples. In the case of large cross-section samples, strength increases with the number of contour layers, leading to an increase of up to 97% of the tensile strength value for 11 perimeter layer samples. The mechanical strength of the printed components can also be improved by using lower values of the thickness of the deposited layers.

Printed Flexible Thermoelectric Nanocomposites Based on Carbon Nanotubes and Polyaniline

Materials 2021, 14(15), 4122

A new era of composite organic materials, nanomaterials, and printed electronics is emerging to the applications of thermoelectric generators (TEGs). Special attention is focused on carbon nanomaterials and conducting polymers, and the possibility to form pastes and inks for various low-cost deposition techniques. In this work, we present a novel approach to the processing of composite materials for screen-printing based on carbon nanotubes (CNTs) and polyaniline (PANI), supported with a dielectric polymer vehicle. Three different types of such tailor-made materials were prepared, with a functional phase consisted of carbon nanotubes and polyaniline composites fabricated with two methods: dry mixing of PANI CNT powders and in situ polymerisation of PANI with CNT. These materials were printed on flexible polymer substrates, exhibiting outstanding mechanical properties. The best parameters obtained for elaborated materials were σ=405.45 S⋅m−1, S=15.4 μV⋅K−1, and PF=85.2 nW⋅m−1K−2, respectively.

Soldering of Electronics Components on 3D-Printed Conductive Substrates

Materials 2021, 14(14), 3850

Rapid development of additive manufacturing and new composites materials with unique properties are promising tools for fabricating structural electronics. However, according to the typical maximum resolution of additive manufacturing methods, there is no possibility to fabricate all electrical components with these techniques. One way to produce complex structural electronic circuits is to merge 3D-printed elements with standard electronic components. Here, different soldering and surface preparation methods before soldering are tested to find the optimal method for soldering typical electronic components on conductive, 3D-printed, composite substrates. To determine the optimal soldering condition, the contact angles of solder joints fabricated in different conditions were measured. Additionally, the mechanical strength of the joints was measured using the shear force test. The research shows a possibility of fabricating strong, conductive solder joints on composites substrates prepared by additive manufacturing. The results show that mechanical cleaning and using additional flux on the composite substrates are necessary to obtain high-quality solder joints. The most repeatable joints with the highest shear strength values were obtained using reflow soldering together with low-temperature SnBiAg solder alloy. A fabricated demonstrator is a sample of the successful merging of 3D-printed structural electronics with standard electronic components.

Printed Graphene, Nanotubes and Silver Electrodes Comparison for Textile and Structural Electronics Applications

Sensors 2021, 21(12), 4038

Figure 9. Scanning Electron Microscopy micrograph image presenting the morphology of the sample surface with printed graphene paste containing 10 wt.% GNP in PMMA organic vehicle.

Due to the appearance of smart textiles and wearable electronics, the need for electro-conductive textiles and electro-conductive paths on textiles has become clear. In this article the results of a test of developed textile electro-conductive paths obtained by applying the method of screen printing pastes containing silver nanoparticles and carbon (graphene, nanotubes, graphite) are presented. Conducted research included analysis of the adhesion test, as well as evaluation of the surface resistance before and after the washing and bending cycles. Obtained results indicated that the samples with the content of carbon nanotubes 3% by weight in PMMA on substrate made of aramid fibers (surface mass of 260 g/m2) were characterized by the best adhesion and the best resistance to washing and bending cycles. Such electro-conductive paths have potential to be used in smart clothing applications.

Carbon Nanotube-Based Composite Filaments for 3D Printing of Structural and Conductive Elements

Applied Sciences 2021, 11(3), 1272S


In this publication, we describe the process of fabrication and the analysis of the properties of nanocomposite filaments based on carbon nanotubes and acrylonitrile butadiene styrene (ABS) polymer for fused deposition modeling (FDM) additive manufacturing. Polymer granulate was mixed and extruded with a filling fraction of 0.99, 1.96, 4.76, 9.09 wt.% of CNTs (carbon nanotubes) to fabricate composite filaments with a diameter of 1.75 mm. Detailed mechanical and electrical investigations of printed test samples were performed. The results demonstrate that CNT content has a significant influence on mechanical properties and electrical conductivity of printed samples. Printed samples obtained from high CNT content composites exhibited an improvement in the tensile strength by 12.6 %. Measurements of nanocomposites’ electrical properties exhibited non-linear relation between the supply voltage and measured sample resistivity. This effect can be attributed to the semiconductor nature of the CNT functional phase and the occurrence of a tunnelling effect in percolation network. Detailed I–V characteristics related to the amount of CNTs in the composite and the supply voltage influence are also presented. At a constant voltage value, the average resistivity of the printed elements is 2.5 Ωm for 4.76 wt.% CNT and 0.15 Ωm for 9.09 wt.% CNT, respectively. These results demonstrate that ABS/CNT composites are a promising functional material for FDM additive fabrication of structural elements, but also structural electronics and sensors.

Additive manufacturing of electronics from silver nanopowders sintered on 3D printed low-temperature substrates

Advanced Engineering Materials 2021, 23(4), 2001085

Additive manufacturing is more widely used these days in aerospace, power industry, and automotive. The latest reports indicate that electronics can be produced with this technique. This approach requires the development of new materials for the fabrication of conductive metallic layers on polymers. Herein, a hybrid technique based on fused deposition modeling, direct‐write, and selective laser sintering is demonstrated, for the fabrication of structural electronics. Highly conductive paths are obtained with conductivity values up to 3.2·106 S m−1 in a single printing and sintering additive process. The influence of process parameters is evaluated with several 3D printed polymer substrates affecting the electrical conductivity of the printed conductive paths and circuits. The developed hybrid technique allows performing selective thermal sintering of metallic pastes on polymer substrates exhibiting the value of melting temperatures much lower than the sintering temperature of the silver paste. This phenomenon can be explained with the proposed hypothesis that the activation energy of the sintering process of metallic paste and degradation of polymer substrate plays a key role in obtaining functional conductive metallic paths on polymer substrates. Application of the developed process is demonstrated with a simple human interface device and a circuit with light‐emitting diodes and power source.