Fabrication Of Microstructures Research Articles

Xenon-plasma focused ion beam processing of photonic microstructures with GaAs-based quantum dots

So far, successful focused ion beam (FIB) based fabrication of photonic structures with quantum dots (QDs) has been limited to cases with above 1 µm thick cap, usually in a form of a distributed Bragg reflector of a vertical cavity, which simultaneously protects the active region from the destructive influence of the ion beam. Here, we propose optimized xenon-plasma FIB (Xe-PFIB) technology as a fast and cost-efficient solution alternative to the commonly used combination of electron beam lithography and etching. We demonstrate a 3D processing of GaAs-based photonic microstructures with InGaAs QDs emitting close to the telecom O-band for cylindrical mesas with different cap thicknesses (50-650 nm) obtained by using two approaches: (i) Xe-PFIB for both reducing the cap thickness as well as the in-plane microstructure size, and (ii) wet chemical etching for cap layer removal and subsequent Xe-PFIB for the in-plane milling. The latter appeared more efficient when judging by photoluminescence intensity. Utilizing an additional protecting layer of platinum or carbon was also tested. Eventually, we for the first time show successful FIB-based fabrication of photonic microstructures with bright emission from single QDs capped with only 200 nm layer, which indicates the prospects of this technology for processing of efficient QD-based single-photon sources for quantum communication.

Fabrication of CaSiO3 LTCC high aspect ratio microstructure by laser chemical assisted micro-milling

As a new generation of chip-packaging materials, CaSiO3 LTCC substrates have the characteristics of high frequency, low thermal expansion coefficient, and low dielectric loss. These materials are widely used in radar communication and other industries. However, in the condition of high heat density, it is difficult to adapt calcium silicate with a low thermal conductivity to the heat dissipation requirements. To improve the heat dissipation performance, high-aspect-ratio heat-dissipation microchannels must be prepared on the surface of the CaSiO3 LTCC substrate. In this study, a new nanosecond laser and chemical milling-assisted micro-milling (NLCAM) method is proposed. The processing mechanism of the nanosecond laser ablation of CaSiO3 is explored and the influence of the laser parameters on the depth of the etching groove, top width, and hardness of the residual modified layer are studied by establishing a laser energy superposition model and test method. The improvement of milling force and milling surface quality by laser is studied. The results demonstrate that the laser power has the most significant effect on the ablation depth and width of the top of the CaSiO3; the excess heat diffuses outside the laser irradiation area, increasing the width of the top of the CaSiO3 beyond the designed width. With an increase in the scanning speed and scanning distance, the ablation depth exhibited a decreasing trend, corresponding to the laser energy model. Nanosecond laser chemical milling (NLCM) can reduce the hardness of the material by 72.0–77.2%. The maximum reduction in the average axial milling force was 56.8%, and the fluctuation of milling force is reduced. Compared to pure micro milling, the tool wear area of NLCAM was reduced by 89.3% and the average roughness Sa of the bottom surface of the microgroove was reduced to 0.392 μm, which confirms the high-quality and efficient machining of the CaSiO3 LTCC substrate.

Selective removal of 4H-SiC porous structures caused by photoelectric chemical etching via post oxidation annealing

Low-temperature post oxidation annealing of 4H-SiC at 900 °C for 90 min after photoelectric chemical (PEC) etching in alkaline solution can eliminate the porous structures that form during the etching process, reduce the porosity, and optimize the surface morphology, which has minimal effect on unetched surfaces, allowing for selective treatment between etched and unetched surfaces. Additionally, it can improve the etching depth and enable effective repetition of the etching process. These benefits make PEC etching a valuable technique for microstructure fabrication and surface treatment.

The optimization of CuxO microwires synthesis for improvement in photoelectrochemical performance

One of the most important challenges in the fabrication of CuxO microstructures via the electrochemical method is formation of long, regular and well-packed microwires with good adhesion on the Cu substrate and to achieve better photoelectrochemical properties, which can be potentially applied in solar-driven water splitting and CO2 conversion to light hydrocarbons. In this paper, Cu2O photoelectrode has been fabricated by direct anodization of the Cu foil, then CuO microwires (MWs) was formed by calcination process. The effect of the applied potential (10–40 V), sodium fluoride content in the electrolyte (0.2–0.5% wt.) as well as calcination conditions (400–500 °C, 60–360 min) on the morphology, phase composition, optical and photoelectrochemical properties was investigated. The highest photocurrent response was −0.71 mA cm−2 for the sample 0.35%_10V_400 °C_60min with 0.83 μm length and 154 nm diameter. The mechanism of the photocurrent generation process in the presence of CuxO/Cu under UV–Vis irradiation was proposed.

Microstructural Engineering of Flow Battery Electrodes with Non-Solvent Induced Phase Separation

Rising levels of greenhouse gases urge the decarbonization of human activities. Electrification of strategic sectors such as transport, industry, and heating necessitates affordable, safe, and dispatchable large-scale energy storage systems. Redox flow batteries (RFBs) stand as a promising long-duration and large-scale energy storage technology due to their design features[1]. Ongoing research focuses on engineering key cell components (e.g. membranes, electrodes, active materials) to improve cost competitiveness. This work focuses on the fabrication of novel porous carbon electrodes which strongly influence the performance and cost of the technology. The requirements for porous electrodes liquid-phase electrochemical reactors are contradictory: a large surface area is needed to overall exchange current density, but also minimal pressure losses to decrease pumping costs. Additionally, surface properties of the electrode dictate the reaction kinetics whereas its microstructure controls the mass transport of the reactants within the reactor area[2]. However, the current state-of-the-art porous electrodes for RFBs consists of carbon-fiber materials repurposed from other electrochemical technologies (e.g. polymer electrolyte fuel cells) which do not offer a favorable tradeoff between transport properties and surface area. Additionally, their production involves complex manufacturing processes resulting in high cost and limited morphological versatility. Therefore, there is a need to develop alternative synthetic platforms which offer tailorable microstructures and surface properties to match the requirements of emerging electrochemical applications, such as redox flow batteries. In this work, we draw inspiration from the membrane technology and employ non-solvent induced phase separation (NIPS) as a method to synthesize porous carbon electrodes for RFBs[3,4].Here, we present our latest efforts to develop a manufacturing route enabling the control of microstructural features of carbonaceous porous electrodes for RFBs. The microstructure of the carbon scaffold is determined by the nature and composition of the polymer blend used to cast the electrode precursor. We use polyacrylonitrile as scaffold precursor and polyvinylpyrrolidone as a pore forming agent, dissolved in an organic solvent (i.e., dimethylformamide, dimethylsulfoxide or N-methylpyrrolidone). The polymer blends were cast into a mold and immersed in a water coagulation bath prior to being stabilized (270 °C) and carbonized (1050 °C). Various process parameters (e.g. polymer concentration, bath temperature, solvent type) governing the final electrode properties were leveraged to control structural features, opening new opportunities for the fabrication of diverse microstructures (i.e., porosity gradient, isoporosity and with macrovoids). Electrochemical double layer capacitance and pressure drop measurements show an increased design space compared to carbon-fiber electrodes, confirming the versatility of the synthetic route. Microstructural analysis of the prepared NIPS electrodes reveals two porosity domains: large finger-like macrovoids (throat diameter >50 μm) and smaller interconnected microvoids (pore diameter 2-15 μm). Flow cell polarization and electrochemical impedance spectroscopy measurements in two common flow battery electrolytes, an Fe2+/Fe3+ single electrolyte and vanadium full cell, show improvements in performance compared to traditional electrodes. An increase in the polymer concentration of the polymer blend solution produced NIPS electrodes with smaller pores and resulted in better mass transport within the electrode. When the temperature of the coagulation bath was increased to 40 ºC, the electrode has higher electrochemically active surface area, producing a significant power increase in the sluggish vanadium electrolyte. Overall, the NIPS electrodes operate at significantly lower activation and mass transport overpotentials in all-vanadium RFBs, generating higher electrical power at the expense of a slight pressure drop increase. Although preliminary, we demonstrate the potential of NIPS to manufacture electrodes with tailorable microstructures for convection-enhanced electrochemical technologies.[1] T. M. Gür, Energy Environ. Sci. 2018, 11, 2696.[2] A. Forner-Cuenca, E. E. Penn, A. M. Oliveira, F. R. Brushett, J. Electrochem. Soc. 2019, 166, A2230.[3] R. R. Jacquemond, C. T.-C. Wan, Y.-M. Chiang, Z. Borneman, F. R. Brushett, K. Nijmeijer, A. Forner-Cuenca, Cell Reports Physical Science 2022, 3, 100943.[4] C. T.-C. Wan, R. R. Jacquemond, Y.-M. Chiang, K. Nijmeijer, F. R. Brushett, A. Forner-Cuenca, Adv. Mater. 2021, 10. Figure 1

Linear polydimethylsiloxane microstructure fabrication by electrohydrodynamic printing with cone jet

Linear polydimethylsiloxane microstructure fabrication by electrohydrodynamic printing with cone jet

Multi-Objective Optimization of Micro-Milling Parameters—The Trade-Offs between Machining Quality, Efficiency, and Sustainability in the Fabrication of Thin-Walled Microstructures

Micro-milling has found extensive applications in machining components with thin-walled microstructures, such as terahertz slow-wave structures, microfluidic chips, and micro-molds. Due to the influence of size effects, micro-milling exhibits higher specific energy consumption compared with traditional milling, implying that more energy is consumed to remove a unit volume of material, particularly in challenging-to-machine materials like Ti-6Al-4V. Historically, research on parameter optimization for micro-milling has predominantly focused on enhancing machining quality and efficiency, with limited attention given to energy efficiency. However, in the context of the “double carbon” strategy, energy conservation and emissions reduction have garnered significant attention in the manufacturing industry. Therefore, this paper proposes a micro-milling parameter-based power consumption model. Based on this, a specific energy consumption model can be obtained. Moreover, evolutionary algorithms are utilized for the optimization of micro-milling parameters, which aims to achieve comprehensive enhancements in both machinability and sustainability. The optimization objectives encompass improving surface quality, dimensional accuracy, material removal rate, and specific energy consumption during the micro-milling process for thin-walled micro-structures. Among them, NSGA-III achieves the best optimization results. Under conditions in which cutting energy consumption and processing efficiency are very close, the optimization outcomes based on NSGA-III lead to the best machining quality, including the minimum surface roughness and dimensional errors, and the largest surface fractal dimension. The optimal combination of micro-milling parameters is n = 28,800 rpm, fz = 2.6 μm/t, and ap = 62 μm.

3D Printing Hierarchically Nano-Ordered Structures.

Natural materials are composed of a limited number of molecular building blocks and their exceptional properties are governed by their hierarchical structure. However, this level of precision is unattainable with current state-of-the-art materials for 3D printing. Herein, new self-assembled printable materials based on block copolymers (BCPs) enabling precise control of the nanostructure in 3D are presented. In particular, well-defined BCPs consisting of poly(styrene) (PS) and a polymethacrylate-based copolymer decorated with printable units are selected as suitable self-assembled materials and synthesized using controlled radical polymerization. The synthesized library of BCPs are utilized as printable formulations for the fabrication of complex 3D microstructures using two-photon laser printing. By fine-tuning the BCP composition and solvent in the formulations, the fabrication of precise 3D nano-ordered structures is demonstrated for the first time. A key point of this work is the achievement of controlled nano-order within the entire 3D structures. Thus, imaging of the cross-sections of the 3D printed samples is performed, enabling the visualization also from the inside. The presented versatile approach is expected to create new avenues for the precise design of functional polymer materials suitable for high-resolution 3D printing exhibiting tailor-made nanostructures.

Employing Stencil-Assisted Laser Ablation to Simplify the Fabrication of Polymer Membrane-Suspended Microstructures on Printed Circuit Boards

Employing Stencil-Assisted Laser Ablation to Simplify the Fabrication of Polymer Membrane-Suspended Microstructures on Printed Circuit Boards

Online process monitoring of direct laser interference patterning using an infrared camera system

Direct laser interference patterning enables the fabrication of homogeneous microstructures in the sub µm range. Generally, the topography of fabricated structures is characterized ex-situ using for instance confocal microscopy or white light interferometry. These methods require at least few seconds to fulfill a measurement and therefore are not suitable for online process observation. In this study, an IR camera system is used for the first time, for capturing the average temperature during the DLIP treatment in real time. To determine a correlation between the average temperature and the topographical parameters, the treated surfaces are analyzed using confocal microscopy. A linear dependency between the applied laser fluence (in the range from 0.7 to 4.9 J/cm2) and the average measured temperature could be established. In addition, in this fluence range, significant changes in the surface roughness, skewness and kurtosis occurred, which could be associated to a certain process average temperature.

Additive Manufacturing of SiOC, SiC, and Si3N4 Ceramic 3D Microstructures

Herein, the fabrication of hard ceramic SiOC 3D microstructures by precursor synthesis, laser lithography, and pyrolysis combination is proposed. Precursors are hybrid organosilicon materials prepared via sol–gel method using trimethoxymethylsilane and 3‐(trimethoxysilyl)propyl methacrylate, which has an acrylate functional group enabling laser photopolymerization process. Hard 3D ceramic structures (hardness up to ≈15 GPa, reduced elastic modulus ≈105 GPa) from soft organometallic derivatives are obtained after high‐temperature pyrolysis under nitrogen atmosphere. The advantage of the proposed method is the absence of shrinkage defects leading to a uniform repetitive decrease in the volume of printed microstructures. In contrast to slurry‐based printing technology, the proposed method is focused on homogeneous monolithic molecular resins resulting in visual smooth surfaces of prepared microstructures. Moreover, the printing resolution of the proposed method is substantially improved through the absence of predispersed ceramic microparticles in mixtures, which is a necessary element in a slurry‐based technology.

Martensite decomposition under thermal-mechanical coupling conditions to fabricate an ultrafine-grained Ti6Al4Mo4Zr1W0.2Si alloy

The fabrication of ultrafine-grained microstructures (grain size below 1 μm) in titanium alloys is beneficial for improving their mechanical properties at room temperature and medium temperatures (400–550 °C). However, a long-standing challenge involves the low-cost manufacturing of bulk ultrafine-grained titanium alloys. In this work, we developed a facile strategy through martensite decomposition at thermal-mechanical coupling conditions, to fabricate an equiaxed microstructure in a Ti6Al4Mo4Zr1W0.2Si model alloy with an average α grain size of 315 ± 62 nm. The formation of the ultrafine-grained microstructure was because the lattice strain stored in the martensitic initial microstructure enhanced the nucleation rate of dynamic recrystallization, meanwhile, the pinning role of martensite decomposition products β and (Ti, Zr)5Si3 phases suppressed grain coarsening at high temperatures. Compared to conventional (α+β) alloys, the tensile strength of this alloy improved by 20%–30% at both room temperature and 550 °C, without decreasing its ductility. In situ SEM observations revealed that the ultrafine-grained microstructure would not only suppress dislocation motions but also contribute to the homogenous deformation in the matrix of the material, therefore, it resulted in higher mechanical performance. The research results may be of great significance to the development of next-generation aviation titanium alloys.

Analytical modeling of subsurface damage and material removal energy in elliptical vibration cutting of micro-structures on brittle materials

Elliptical vibration cutting (EVC) is a promising technique for the fabrication of micro-structures on brittle materials. In this work, the surface quality and material removal energy in ultra-precision machining of micro-structures on brittle materials by EVC were investigated. Theoretical models were first established for predicting subsurface damage and specific cutting energy (SCE) based on the intermittent material removal characteristics of EVC. The models correlated cutting parameters with the tool vibration trajectory parameters, target surface geometry parameters, and material removal modes. Furthermore, the material removal behaviors in the nominal cutting direction and the feeding direction were comprehensively considered. To verify the model, the experiments of EVC and ordinary cutting (OC) were performed on single crystal silicon, and the surface morphology and cutting force were characterized. The results indicated that, compared with OC, the maximum subsurface damage depth is reduced by 61.82% and the SCE stability value is reduced to 45.87% by applying EVC to fabricate micro-structures. EVC could significantly improve the machining quality and reduce energy consumption. In addition, increasing the vibration amplitude in the depth of cut direction could further save energy, but a larger amplitude would increase subsurface damage. This work not only promotes the recognition of the material removal mechanism of EVC, but also presents effective guidance for achieving high-quality and sustainable machining of micro-structured surfaces.

An Integrated Simulation of Multiple-Pass U-10Mo Alloy Hot Rolling and Static Recrystallization

AbstractTo achieve a desired microstructure and minimize the thickness variation in rolled foils, researchers must understand the effects of foil fabrication process variables on microstructure evolution. We developed an integrated simulation of deformation and recrystallization that employs the finite element method (FEM) and the kinetic Monte Carlo (KMC) Potts model, respectively, to investigate microstructure evolution during multiple-pass hot rolling and heat treatment in polycrystalline U-10Mo fuel. Scanning electron microscopy and electron backscatter diffraction images of microstructures were directly used as input in FEM calculation of deformation, and the calculated strains were used to determine the driving force of nucleation and growth of recrystallized grains in the Potts model. Grain structures predicted by the Potts model were used to update the grain structure and material properties for FEM. Simulation alternated between FEM and the Potts model to simulate grain structure evolution during multiple rolling and heat treatments. The initial model parameters were determined by benchmarking the recrystallization kinetics against experimental data. Then, the model was applied to predict the grain structure evolution. Results showed that our model can capture the coupling between deformation and recrystallization and can quantitatively reproduce the observed U-10Mo recrystallization and grain growth kinetics. The simulation results demonstrated that the developed model can predict U-10Mo grain structures as a function of initial microstructure and foil fabrication parameters.

Characterization of Grid Lines Formed by Laser-Induced Forward Transfer and Effect of Laser Fluence on the Silver Paste Transformation

The investigation of novel approaches for forming solar cell grid lines has gained importance with the rapid development of the photovoltaic industry. Laser-induced forward transfer (LIFT) is a very promising approach for microstructure fabrication. In this work, the morphology of grid lines deposited by LIFT was investigated. A characterization scheme for solar cell grid lines was proposed. The shape of grid lines was described, combined with confocal imaging. The evolution process of grid lines from no forming to single-peak and double-peak with a variation of laser fluence was observed. According to experimental conditions, different types of grid line morphology were obtained and transfer mechanisms of silver paste were proposed based on fluid dynamics. The influence of laser fluence on the morphology of formed grid lines was explained through phenomenology and analysis. This can provide a guide for morphology control in forming the process of grid lines.

NV-doped microstructures with preferential orientation by growth on heteroepitaxial diamond

For the wafer-scale fabrication of diamond devices, the growth of diamond substrates by heteroepitaxial chemical vapor deposition is the most promising option currently available. However, the transfer of growth and also structuring processes from small homoepitaxial to larger heteroepitaxial samples is not straightforward and requires adaptation. In this study, we present an approach for the fabrication of functional microstructures including pyramids and mesas as well as more complex structures with hollow centers. The associated methods were previously demonstrated by homoepitaxial growth and are now evaluated on heteroepitaxially grown diamond films. After optimizing the growth procedures to ensure a sufficient quality of the bare diamond substrates, precursor structures for overgrowth were fabricated by e-beam lithography and plasma etching. In the overgrowth of nanopillars, a truncated pyramidal shape was achieved. The characterization with scanning electron microscopy revealed the growth of higher-index facets. Nevertheless, photoluminescence spectroscopy reveals localized doping on the sides of the microstructures. In addition, optically detected magnetic resonance reaches a contrast of 6% of one preferred nitrogen vacancy orientation per facet and a transverse relaxation time T2∗ of 96 ns.

Fabrication of GRIN microstructures by two-photon lithography

The method of two-photon lithography is used to fabricate GRIN microstructures. Test rectangular structures with sizes 25 × 25 × 3 micrometers were used with varying laser intensity by linear or gaussian distribution in one dimension. The resulting refractive index has been tuned in the range of 0.03. The suggested method can be applied to produce arbitrarily shaped 3D GRIN micro-optical elements.

Fabrication of Optical Microstructures with Gradient Refractive Index by Two-Photon Laser Lithography

Fabrication of Optical Microstructures with Gradient Refractive Index by Two-Photon Laser Lithography

Porous metal micro-pillars by thermomechanical molding of two-phase alloys

Creep-based thermomechanical molding of crystalline metals has emerged as a low-cost manufacturing technique for metal nanostructures. Here, we demonstrate the potential of such molding approach in fabrication of porous metal microstructures by using binary alloys such as Au-Si and Al-Cu. Two-phase alloys were isothermally molded against microscale templates followed by selective etching of one of the phases resulting in porous micro-pillars. The porosity of micro-pillars was varied by changing the phase fractions through alloy composition. Scanning electron microscopy is used to understand the different stages of molding and etching processes for two-phase metal alloys. While the nanoscale thermomechanical molding of similar alloys has been attributed to diffusional creep, the microscale forming presented here is dominated by the dislocation and grain boundary mediated deformation mechanisms. The molding and selective etching methodology can be potentially used to tailor the size and the distribution of pores by optimizing the microstructure of feedstock alloy.

Regulation of bimodal structure and mechanical properties of powder-thixoformed GO/ZK60 magnesium matrix composite through adjusting GO content

Although remarkable strength enhancements can be achieved in graphene oxide (GO)/ graphene nanoplatelets (GNPs) reinforced Mg matrix composites by using the available techniques, their ductility is always quite poor due to the difficultly avoided strength-ductility trade-off. To conquer this dilemma, GO/ZK60 composites with bimodal-grain structure were fabricated using powder thixoforming in this work. The results indicate that the grain size and volume fraction of coarse grains (CGs) first decrease as the GO content increases to 0.2 wt.% and then increase again as the content increases to 0.3 wt.%, while the grain size in the fine grains (FGs) almost does not change. Consequently, the strength of the composites is improved with increasing GO content and reaches the peak values at the content of 0.2 wt.%. The composite with 0.1 wt.% GO content exhibits significantly increased tensile yield strength up to 177 ± 2 MPa while maintaining a high elongation of 23.1% ± 2.5%, being equivalent to that of the ZK60 matrix alloy. The increased FGs volume fraction, together with the promoted dislocation accumulation and storage via GO and grain refinement of large-sized CGs lead to the improvement of strain hardening ability, thus rendering the composite an excellent ductility. Furthermore, the deformation of the GO/ZK60 composites occurs progressively from the FGs to the CGs, which is opposite to the status of the milled ZK60 matrix alloy. In view of the microstructure characteristics of the composites, a new complex calculation model was proposed and it could well predict the strength of the bimodal GO/ZK60 composites. This study provides a new insight into the microstructure design and fabrication technology of GO/GNPs reinforced metal-based composites with high strength and ductility.