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Facet-selective morphology-controlled remote epitaxy of ZnO microcrystals via wet chemical synthesis
We report on morphology-controlled remote epitaxy via hydrothermal growth of ZnO micro- and nanostructure crystals on graphene-coated GaN substrate. The morphology control is achieved to grow diverse morphologies of ZnO from nanowire to microdisk by changing additives of wet chemical solution at a fixed nutrient concentration. Although the growth of ZnO is carried out on poly-domain graphene-coated GaN substrate, the direction of hexagonal sidewall facet of ZnO is homogeneous over the whole ZnO-grown area on graphene/GaN because of strong remote epitaxial relation between ZnO and GaN across graphene. Atomic-resolution transmission electron microscopy corroborates the remote epitaxial relation. The non-covalent interface is applied to mechanically lift off the overlayer of ZnO crystals via a thermal release tape. The mechanism of facet-selective morphology control of ZnO is discussed in terms of electrostatic interaction between nutrient solution and facet surface passivated with functional groups derived from the chemical additives.
Synthesis Methods for Nanoparticle Morphology Control in Energy Applications
Lightweight nano-composite materials, nano-coatings, nanocatalysts, nano-structured materials have demonstrated an ability to reduce emissions and maximize clean energy production. Nanoparticles play an important role in engineering and decarbonization for energy applications, and a wide range of nanoparticle synthesis methods have been developed to include those that enable control over particle morphology. The ability to control nanoparticle morphology allows the tailoring and improvement of material properties that will accelerate efforts towards lowering carbon emissions by developing advanced catalysts for carbon sequestration and will enhance energy efficient processes and technologies. Synthesis methods aimed towards shape control of nanoparticles have demonstrated an ability to form spheres, rods, flower-like shapes, cubes, plates, shells, and chiral geometries. Processing methods used to form these morphologies include microwave assisted synthesis, solvothermal, hydrothermal, and a wide range of capping agents. A discussion of a few of these methods is given along with results and applications.
Metal‐Organic Framework (MOF) Morphology Control by Design
Abstract Exerting morphological control over metal‐organic frameworks (MOFs) is critical for determining their catalytic performance and to optimize their packing behavior in areas from separations to fuel gas storage. A mechanism‐based approach to tailor the morphology of MOFs is introduced and experimentally demonstrated for five cubic Zn 4 O‐based MOFs. This methodology provides three key features: 1) computational screening for selection of appropriate additives to change crystal morphology based on knowledge of the crystal structure alone; 2) use of additive to metal cluster geometric relationships to achieve morphologies expressing desired crystallographic facets; 3) potential for suppression of interpenetration for certain phases.
Solvation directed morphological control in metal oxide nanostructures
The development of structural hierarchy on various length scales during the crystallization process is ubiquitous in biological systems and minerals and is common in synthetic nanomaterials. The driving forces for the formation of complex architectures range from local interfacial interactions, that modify interfacial speciation, local supersaturation, and nucleation barriers, to macroscopic interparticle forces. Although it is enticing to interpret the formation of hierarchical architectures as the assembly of independently nucleated building blocks, crystallization pathways often follow monomer-by-monomer addition with structural complexity arising from interfacial chemical coupling and strongly correlated fluctuation dynamics in the electric double layers. Here, we show that the development of structural hierarchy through heterogeneous nucleation is driven by dipolar and solvation forces. Specifically, coupled simulations and experimental studies revealed that dipole build-up along the slow growth direction can trigger twinning and the development of branched architectures. Enthalpic solvation interactions were shown to either enhance or reduce the dipole moment of the nanoparticles and, thereby, control crystal morphology and architecture. The systematic studies of chemical coupling between different solvents and undercoordinated surface atoms of the growing nanocrystals revealed the mechanism of dimensionality control and the development of structural hierarchy without ligands or structure-directing agents.
Freeze-drying for morphological control of high performance semi-interpenetrating polymer networks. III
The feasibility of using a freeze-drying (solvent removal by sublimation) approach for controlling the morphology of a high-performance semi-IPN is assessed. A high-performance thermoplastic polyimide and commercially available 4,4'-bismaleimide diphenylenemethane were dissolved in a solvent, 1,3,5-trioxane. The solvent was removed from the constituents by freeze-drying. For purposes of comparison, the constituents were dissolved in a high-boiling-point solvent, N,N-dimethylformamide. The solvent was removed from the solution by evaporation. The physical and mechanical properties and phase morphology of the neat resins and composites prepared by freeze-drying and traditional solution methods are presented and compared. It is concluded that the TG is higher and that the magnitude of minor constituent separation is less in the freeze-dry processed materials than for the processed solution.
Equally high efficiencies of organic solar cells processed from different solvents reveal key factors for morphology control
The power conversion efficiency of organic solar cells (OSCs) is exceeding 20%, an advance in which morphology optimization has played a significant role. It is generally accepted that the processing solvent (or solvent mixture) can help optimize morphology, impacting the OSC efficiency. Here we develop OSCs that show strong tolerance to a range of processing solvents, with all devices delivering high power conversion efficiencies around 19%. By investigating the solution states, the film formation dynamics and the characteristics of the processed films both experimentally and computationally, we identify the key factors that control morphology, that is, the interactions between the side chains of the acceptor materials and the solvent as well as the interactions between the donor and acceptor materials. Our work provides new understanding on the long-standing question of morphology control and effective guides to design OSC materials towards practical applications, where green solvents are required for large-scale processing.
Morphology Control of Growth by Hydride Vapor Phase Epitaxy on Faceted GaAs Substrates Produced by Controlled Spalling for Low Cost III-V Devices
In this work, we apply the morphology control of hydride vapor phase epitaxial (HVPE) growth to planarize faceted, non-planar substrates. Controlled spalling is a promising high-throughput substrate reuse technology that could reduce substrate costs for III-V devices; however, the spalling fracture for (100)-oriented GaAs substrates produces a regularly corrugated surface of facets that are 5-20 um in height. We discuss how to planarize these surfaces using only a few minutes of HVPE growth and how to minimize the impact on throughput when integrating faceted wafers into a potential manufacturing process at scale.
Synthesis of energetic material particles with controlled morphology
A surfactant-assisted self-assembly method can be used to crystallize energetic materials with controlled morphology. Microparticles of hexanitrohexaazaisowurtzitane (CL-20) formed by this method may have enhanced functional reproducibility due to their monodisperse nature, and decreased shock sensitivity due to their sub-2 μm particle size.
Morphology‐controlled synthesis of multi‐metal‐based spinel oxide nanocatalysts and their performance for oxygen reduction
Abstract We present a one‐pot colloidal synthesis method for producing monodisperse multi‐metal (Co, Mn, and Fe) spinel nanocrystals (NCs), including nanocubes, nano‐octahedra, and concave nanocubes. This study explores the mechanism of morphology control, showcasing the pivotal roles of metal precursors and capping ligands in determining the exposed crystal planes on the NC surface. The cubic spinel NCs, terminated with exclusive {100}‐facets, demonstrate superior electrocatalytic activity for the oxygen reduction reaction (ORR) in alkaline media compared to their octahedral and concave cubic counterparts. Specifically, at 0.85 V, (CoMn)Fe 2 O 4 spinel oxide nanocubes achieve a high mass activity of 23.9 A/g and exhibit excellent stability, highlighting the promising ORR performance associated with {100}‐facets of multi‐metal spinel oxides over other low‐index and high‐index facets. Motivated by exploring the correlation between ORR performance and surface atom arrangement (active sites), surface element composition, as well as other factors, this study introduces a prospective approach for shape‐controlled synthesis of advanced spinel oxide NCs. It underscores the significance of catalyst shape control and suggests potential applications as nonprecious metal ORR electrocatalysts.
Reaction‐induced morphology control in block copolymers
Abstract Controlling the self‐assembly behaviors of block copolymers (BCPs) is a focal point of many research thrusts due to their broad use in various applications. While BCP molecular weight, volume fraction, and chemical identities are key thermodynamic parameters to determine their morphology, an emergent method in this area is through reaction‐induced changes to the characteristics of a BCP in situ , which provides access to multiple morphologies and domain sizes from a single parent polymer, as well as enabling the formation of metastable morphologies which may be difficult to attain otherwise. This work provides a focused review about the current state of reaction‐induced morphology control in BCPs in both solution and solid states. Furthermore, we provide a forward‐looking perspective on the future opportunities of understanding and employing reaction engineering to manipulate and advance BCP self‐assembly. © 2023 Society of Industrial Chemistry.
Freeze drying for morphological control of inter-penetrating polymer networks
The intrinsic brittleness of BMI resins can be reduced through the creation of an interpenetrating network (IPN) of BMI with a reactive-encapped thermoplastic, such as the presently considered polyimidesulfone, PISO2. The PISO2 and BMI were dissolved in a common solvent, which was then removed from the constituents by freeze drying; in an alternative method, an IPN was formed through dissolution of the constituent in a common solvent with either high or low melting point, followed by evaporative removal of the solvent. The effectiveness of the freeze-drying approach for morphological control is evaluated.
Random Polymerization Strategy Leads to a Family of Donor Polymers Enabling Well‐Controlled Morphology and Multiple Cases of High‐Performance Organic Solar Cells
Abstract Developing high‐performance donor polymers is important for nonfullerene organic solar cells (NF‐OSCs), as state‐of‐the‐art nonfullerene acceptors can only perform well if they are coupled with a matching donor with suitable energy levels. However, there are very limited choices of donor polymers for NF‐OSCs, and the most commonly used ones are polymers named PM6 and PM7, which suffer from several problems. First, the performance of these polymers (particularly PM7) relies on precise control of their molecular weights. Also, their optimal morphology is extremely sensitive to any structural modification. In this work, a family of donor polymers is developed based on a random polymerization strategy. These polymers can achieve well‐controlled morphology and high‐performance with a variety of chemical structures and molecular weights. The polymer donors are D–A1–D–A2‐type random copolymers in which the D and A1 units are monomers originating from PM6 or PM7, while the A2 unit comprises an electron‐deficient core flanked by two thiophene rings with branched alkyl chains. Consequently, multiple cases of highly efficient NF‐OSCs are achieved with efficiencies between 16.0% and 17.1%. As the electron‐deficient cores can be changed to many other structural units, the strategy can easily expand the choices of high‐performance donor polymers for NF‐OSCs.
Process for controlling morphology and improving thermal mechanical performance of high performance interpenetrating and semiinterpenetrating polymer networks
In the process of the present invention, a non-polar, aprotic solvent is removed from an oligomer/polymer solution by freeze-drying in order to produce IPNs and semi-IPNs. By thermally quenching the solution to a solid in a short length of time, the size of the minor constituent-rich regions is greatly reduced as they are excluded along with the major constituent from the regions of crystallizing solvent. The use of this process sequence of controlling phase morphology provides IPNs and semi-IPNs with improved fracture toughness, microcracking resistance, and other physical-mechanical properties as compared to IPNs and semi-IPNs formed when the solvent is evaporated rather than sublimed.
Process for controlling morphology and improving thermal-mechanical performance of high performance interpenetrating and semi-interpenetrating polymer networks
In the process of the present invention, a non-polar, aprotic solvent is removed from an oligomer/polymer solution by freeze-drying in order to produce IPNs and semi-IPNs. By thermally quenching the solution to a solid in a short length of time, the size of the minor constituent-rich regions is greatly reduced as they are excluded along with the major constituent from the regions of crystallizing solvent. The use of this process sequence of controlling phase morphology provides IPNs and semi-IPNs with improved fracture toughness, microcracking resistance, and other physical-mechanical properties as compared to IPNs and semi-IPNs formed when the solvent is evaporated rather than sublimed.
Lowering oxygen evolution overpotential via morphology control of NiO x nanocatalysts
NiO x nanocatalysts with two distinct morphologies, nano-spindles and nano-plates, were synthesized and evaluated for oxygen evolution reaction (OER) performance. Spindle-like NiO x was prepared via a hydrothermal reaction of nickel nitrate and urea with cetyltrimethylammonium bromide as a surfactant at 120 °C for 24 h, forming Ni(OH) 2 -based intermediates that were subsequently calcined at 300 °C for 3 h. In contrast, platelet-like Ni(OH) 2 nanocrystals were obtained using nickel(II) acetate and KOH at 180 °C for 24 h, followed by calcination at 400 °C or 500 °C for 4 h to yield NiO x nano-plates. The NiO x nano-spindles exhibited an OER overpotential of 395 mV at 10 mA/cm 2 , whereas the NiO x nano-plates annealed at 400 °C and 500 °C showed overpotentials of 565 mV and 474 mV at 10 mA/cm 2 , respectively. Structural characterization and X-ray photoemission spectroscopy indicate these differences arise from morphology-dependent surface structures that govern catalytic activity.
Morphological controls on flow conductivity and viscosity of bentonite–polymer composites
In this study, the authors investigate the morphological organisation of polymers in bentonite–polymer composites (BPCs) used in geosynthetic clay liners and controls on hydraulic conductivity and viscosity. A limited understanding of the relationship between the microstructure of BPCs and their macroscopic engineering behaviour motivates this study. The polymer resides in the inter-granular pores of bentonite based on synchrotron-based small-angle X-ray scattering measurements, scanning electron microscopy imaging and pore size analyses. On wetting, the polymer swells to produce a swollen hydrogel residing in the inter-granular pores. Enhanced tortuosity arising from hydrogel formation reduces the hydraulic conductivity of BPCs. The higher viscosity of the BPC slurry is attributed to the higher shear resistance emerging from swelling of the polymer fraction on wetting. These findings link the morphological features of BPCs to the observed hydraulic conductivity and viscosity of these materials.
Surface-Tailoring and Morphology Control as Strategies for Sustainable Development in Transport Sector
Surface wetting plays an important role in the corrosion protection processes of aerospace applications. Here, we demonstrate the use of ultrafast femtosecond (fs) laser processing techniques to tailor the wetting properties of aluminum (Al) substrates by creating diverse surface morphologies. Specifically, two distinct laser scanning methods—dot-hatching and cross-hatching—were employed to fabricate microstructures on the substrates. By varying the incident laser parameters, we confirmed that the resulting surface morphologies exhibit different wetting behaviors, spanning from hydrophilicity to hydrophobicity. Furthermore, time-resolved spreading tests validate that dynamic wetting behaviors can also be modified. This fs laser processing approach provides a straightforward, one-step fabrication method for effectively modifying the wetting properties of Al alloys.