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Monodisperse resorcinol formaldehyde resin (RF) microspheres are an important polymeric material because of their rich surface functional group and uniform structural characteristics and have been increasingly applied as an electrode material, catalyst support, absorbent, and carbon microsphere precursor. The polymerization conditions, such as the gelation/solidification temperature and the residence time, can largely influence the physical properties and the formation of the 3D polymeric network of the RF microspheres as well as the carbon microspheres. However, few studies have reported on the complexity of the gelation and solidification processes of resol. In this work, we developed a new RF microsphere preparation device that contains three units: a droplet generation unit, a curing unit, and a collection unit. In this system, we controlled the gelation and solidification processes of the resol and observed its curing behavior, which helped us to uncover the curing mechanism of resol. Finally, we obtained the optimized polymerization parameters, obtaining uniform RF microspheres with a variation coefficient of 4.94%. The prepared porous RF microspheres presented a high absorption ability, reaching ~90% at 10 min. Thus, our method demonstrated the practicality of on-chip monodisperse microspheres synthesis. The product was useful in drug delivery and adsorbing large poisonous molecules., Competing Interests: The authors declare no conflict of interest.

In this study, we report a colloidal synthesis of palladium sulfides (including Pd 16 S 7 , Pd 4 S, and PdS) via a facile one-pot hot-solution synthetic route and their promising application as electrocatalyst for the oxygen reduction reaction (ORR). Among the different palladium sulfides tested, monodisperse Pd 4 S nanoparticles exhibit the best electrocatalytic activity toward ORR in alkaline medium, with the half-wave potential ca. 47 mV more positive than that of the state-of-the-art Pt/C catalyst. Density functional theory calculations indicate the existence of oxygen absorption sites in Pd 4 S surface result in optimized oxygen-binding ability for the four-electron oxygen reduction.

Polyethylene glycol (PEG) and derivatives with eight and twelve ethylene glycol units were synthesized by stepwise addition of tetraethylene glycol monomers on a polystyrene solid support. The monomer contains a tosyl group at one end and a dimethoxytrityl group at the other. The Wang resin, which contains the 4-benzyloxy benzyl alcohol function, was used as the support. The synthetic cycle consists of deprotonation, Williamson ether formation (coupling), and detritylation. Cleavage of PEGs from solid support was achieved with trifluoroacetic acid. The synthesis including monomer synthesis was entirely chromatography-free. PEG products including those with different functionalities at the two termini were obtained in high yields. The products were analyzed with ESI and MALDI-TOF MS and were found close to monodispersity., (© 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Polydisperse PEGs are ubiquitously used in pharmaceutical industry and biomedical research. However, the monodispersity in PEGs may play a role in the development of safe and effective PEGylated small molecular drugs. Here, to avoid the polydispersity in polidocanol, the active ingredient in a clinically used drug, a macrocyclic sulfate-based strategy for the efficient and scalable synthesis of monodisperse polidocanols, their sulfates, and their methylated derivatives, was developed. TLC and HPLC analysis indicated a complex mixture in regular polidocanol and high purities in monodisperse polidocanols and their derivatives. Assay on HUVEC, L929, and HePG2 cells showed that monodisperse polidocanols have much higher cytotoxicity and safety than that of regular polidocanol. It was found that the monodispersity of PEGs in polidocanols is crucial for achieving the optimal therapeutic results. Therefore, based on this case study, it would be beneficial to optimize PEGylated small molecular drugs with monodisperse PEGs in pharmaceutical research and development.

An efficient, accurate and sensitive method for the determination of five iridoid glycosides (IGs) in Cornus officinalis fructus using molecularly imprinted solid phase extraction (MISPE) coupled with high performance liquid chromatography (HPLC) has been developed. Water-compatible molecularly imprinted beads (MIBs) were synthesized by precipitation polymerization, using alkenyl glycosides glucose as the hydrophilic functional monomer. Scanning electron microscopy showed that the MIBs had a narrow particle size distribution, with diameters in the range 7.5-9.3μm. The special molecular recognition by the MIBs of IGs in aqueous media was verified by static adsorption, kinetic adsorption, and selectivity experiments. The newly prepared MIBs were used as sorbents in solid phase extraction (SPE) for the selective recognition of five IGs (loganin, morroniside, loganic acid, 7-O-ethyl-morroniside and 7-O-methyl morroniside) in Cornus officinalis fructus. When optimized, the MISPE-HPLC method had good linearity (0.02-100mgg -1 ), with correlation coefficient (R)≥0.994. Recoveries at three spiked levels were in the range 80.0%-94.0%. Because of its excellent specificity and hydrophilicity, SPE based on monodisperse MIBs provides a promising pretreatment strategy for the analysis of active components in natural products, especially for the quality control of traditional Chinese medicines., (Copyright © 2017 Elsevier B.V. All rights reserved.)

An extended one-step Stőber method was utilized for the preparation of core@shell spheres, which was made up of a thin layer of resorcinol-formaldehyde (RF) and a silica core. After the carbonization and template-removal process, hollow porous carbon spheres (HPCSs) were synthesized. The structure of HPCSs was characterized by scanning/transmission electron microscopy and N 2 adsorption/desorption isotherms, Fourier transform infrared spectroscopy, energy dispersive X-ray spectrometer and Raman spectroscopy. The results showed that the silica cores were removed successfully and the HPCSs were in good sphere shape with uniform size, high surface areas as well as pores hollow framework structure. Compared with MWCNTs and 3D-graphene, HPCSs exhibited superior extraction ability for nine bisphenols (BPs). HPCSs showed extremely outstanding extraction efficiency for BPs as well as high adsorption capacity due to its hollow porous structure. It was applied as sorbent for the enrichment of nine BPs from environmental water samples and soft drinks prior to high performance liquid chromatographic (HPLC) analysis, obtaining recoveries ranged from 89.6% to 111.5% and the relative standard deviations (RSD) from 0.8% to 6.3%, and the limits of quantification (LOQs) were in the range of 0.183-1.763μgL -1 ., (Copyright © 2017 Elsevier B.V. All rights reserved.)

This review describes different synthetic strategies towards sequence-defined, monodisperse macromolecules, which are built up by iterative approaches and lead to linear non-natural polymer structures. The review is divided in three parts: solution phase-, solid phase-, and fluorous- and polymer-tethered approaches. Moreover, synthesis procedures leading to conjugated and non-conjugated macromolecules are considered and discussed in the respective sections. A major focus in the evaluation is the applicability of the different approaches in polymer chemistry. In this context, simple procedures for monomer and oligomer synthesis, overall yields, scalability, purity of the oligomers, and the achievable level of control (side-chains, backbone, stereochemistry) are important benchmarks., (© 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

ZnO has been demonstrated to be a promising candidate to fabricate high efficiency perovskite solar cells (PSCs) in terms of its better electron extraction and transport properties. However, the inability of synthesis of ZnO nanoparticles (NPs) with minimal surface defects and agglomeration remains a great challenge hindering the fabrication of highly efficient PSCs. In this work, highly crystalline and agglomeration-free ZnO NPs with controlled size were synthesized through a facile solvothermal method. Such ZnO NPs were applied in the fabrication of meso-structured PSCs. The solar cells with ∼40 nm ZnO NPs exhibit the highest power conversion efficiency (PCE) of 15.92%. Steady-state and time-resolved photoluminescence measurements revealed the faster injection and lower charge recombination at the interface of ∼40 nm ZnO NPs and perovskite, resulting in significantly enhanced J SC and V OC .

Palladium (Pd) nanoparticle (NP)-decorated carbon nanotube (CNT) ropes (or CNT@PdNP) are used as the sensing element for hydrogen gas (H 2 ) chemiresistors. In spite of the fact that Pd NPs have a mean diameter below 6 nm and are highly dispersed on the CNT surfaces, CNT@PdNP ropes produce a relative resistance change 20-30 times larger than is observed at single, pure Pd nanowires. Thus, CNT@PdNP rope sensors improve upon all H 2 sensing metrics (speed, dynamic range, and limit-of-detection), relative to single Pd nanowires which heretofore have defined the state-of-the-art in H 2 sensing performance. Specifically, response and recovery times in air at [H 2 ] ≈ 50 ppm are one-sixth of those produced by single Pd nanowires with cross-sectional dimensions of 40 × 100 nm Pd. The LOD H2 is <10 ppm versus 300 ppm, and the dynamic range (10 ppm -4%) is nearly twice that afforded by the Pd nanowire. CNT@PdNP rope sensors are prepared by the dielectrophoretic deposition of a single semiconducting CNT rope followed by the electrodeposition of Pd nanoparticles with mean diameters ranging from 4.5 (±1) nm to 5.8 (±3) nm. The diminutive mean diameter and the high degree of diameter monodispersity for the deposited Pd nanoparticles are distinguishing features of the CNT@PdNP rope sensors described here, relative to prior work on similar systems.

Molecularly imprinted polymers (MIPs) gained an expansively growing interest in the past few decades. After an initial, explorative period of preparing MIPs exclusively with bulk polymerization, new polymer synthesis routes have been adapted to overcome the drawbacks of the traditional method. Among these the most appealing is precipitation polymerization that results in nano- and microspheres with narrow size distribution and makes the production of MIPs more straightforward. Here, we describe a precipitation polymerization protocol for a common small molecule template, propranolol that is carried out in the conventional way, in dilute monomer solution. Moreover, a modified precipitation polymerization protocol from concentrated monomer solution is presented for a diclofenac imprinted polymer which makes the synthesis even more versatile and circumvents the disadvantages of the dilute solution conditions.

An in-depth review on a new ultrasonic micro-droplet generator which utilizes megahertz (MHz) Faraday waves excited by silicon-based multiple Fourier horn ultrasonic nozzles (MFHUNs) and its potential applications is presented. The new droplet generator has demonstrated capability for producing micro droplets of controllable size and size distribution and desirable throughput at very low electrical drive power. For comparison, the serious deficiencies of current commercial droplet generators (nebulizers) and the other ultrasonic droplet generators explored in recent years are first discussed. The architecture, working principle, simulation, and design of the multiple Fourier horns (MFH) in resonance aimed at the amplified longitudinal vibration amplitude on the end face of nozzle tip, and the fabrication and characterization of the nozzles are then described in detail. Subsequently, a linear theory on the temporal instability of Faraday waves on a liquid layer resting on the planar end face of the MFHUN and the detailed experimental verifications are presented. The linear theory serves to elucidate the dynamics of droplet ejection from the free liquid surface and predict the vibration amplitude onset threshold for droplet ejection and the droplet diameters. A battery-run pocket-size clogging-free integrated micro droplet generator realized using the MFHUN is then described. The subsequent report on the successful nebulization of a variety of commercial pulmonary medicines against common diseases and on the experimental antidote solutions to cyanide poisoning using the new droplet generator serves to support its imminent application to inhalation drug delivery., Competing Interests: Conflicts of Interest: The authors declare no conflict of interest.

Artificial solids and thin films assembled from colloidal nanomaterials give rise to versatile properties that can be exploited in a range of technologies. In particular, solution-based processes allow for the large-scale and low-cost production of nanoelectronics on rigid or mechanically flexible substrates. To achieve this goal, several processing steps require careful consideration, including nanomaterial synthesis or exfoliation, purification, separation, assembly, hybrid integration, and device testing. Using a ubiquitous electronic device - the field-effect transistor - as a platform, colloidal nanomaterials in three electronic material categories are reviewed systematically: semiconductors, conductors, and dielectrics. The resulting comparative analysis reveals promising opportunities and remaining challenges for colloidal nanomaterials in electronic applications, thereby providing a roadmap for future research and development., (© 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Copper sulfides (Cu 2-x S), are a novel kind of photothermal material exhibiting significant photothermal conversion efficiency, making them very attractive in various energy conversion related devices. Preparing high quality uniform Cu 2-x S nanocrystals (NCs) is a top priority for further energy-and sustainability relevant nanodevices. Here, a shape-controlled high quality Cu 7 S 4 NCs synthesis strategy is reported using sulfur in 1-octadecene as precursor by varying the heating temperature, as well as its forming mechanism. The performance of the Cu 7 S 4 NCs is further explored for light-driven water evaporation without the need of heating the bulk liquid to the boiling point, and the results suggest that as-synthesized highly monodisperse NCs perform higher evaporation rate than polydisperse NCs under the identical morphology. Furthermore, disk-like NCs exhibit higher water evaporation rate than spherical NCs. The water evaporation rate can be further enhanced by assembling the organic phase Cu 7 S 4 NCs into a dense film on the aqueous solution surface. The maximum photothermal conversion efficiency is as high as 77.1%., (© 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Polysaccharide-based nanoparticles are promising carriers for drug delivery applications. The particle size influences the biodistribution of the nanoparticles; hence size distributions and polydispersity index (PDI) are critical characteristics. However, the preparation of stable particles with a low PDI is a challenging task and is usually based on empirical trials. In this study, we report the use of multivariate evaluation to optimize the formulation factors for the preparation of alginate-zinc nanoparticles by ionotropic gelation. The PDI was selected as the response variable. Particle size, size distributions, zeta potential and pH of the samples were also recorded. Two full factorial (mixed-level) designs were analyzed by partial least squares regression (PLS). In the first design, the influence of the polysaccharide and the crosslinker concentrations were studied. The results revealed that size distributions with a low PDI were obtained by using a low polysaccharide concentrations (0.03-0.05%) and a zinc concentration of 0.03% (w/w). However, a high polysaccharide concentration can be advantageous for drug delivery systems. Therefore, in the second design, a high alginate concentration was used (0.09%) and a reduction in the PDI was obtained by simultaneously increasing the ionic strength of the solvent and the zinc concentration. The multivariate analysis also revealed the interaction between the factors in terms of their effects on the PDI; hence, compared to traditional univariate analyses, the multivariate analysis allowed us to obtain a more complete understanding of the effects of the factors scrutinized. In addition, the results are considered useful in order to avoid extensive empirical tests for future formulation studies., (Copyright © 2016 Elsevier B.V. All rights reserved.)

The technique of stray field diffusion NMR is adapted to study the diffusion properties of water in monodisperse wet foams. We show for the first time, that the technique is capable of observing q-space diffusion diffraction peaks in monodisperse aqueous foams with initial bubble sizes in the range of 50-85μm. The position of the peak maximum can be correlated simply to the bubble size in the foam leading to a technique that can investigate the stability of the foam over time. The diffusion technique, together with supplementary spin-spin relaxation analysis of the diffusion data is used to follow the stability and coarsening behaviour of monodisperse foams with a water fraction range between 0.24 and 0.33. The monodisperse foams remain stable for a period of hours in terms of the initial bubble size. The duration of this stable period correlates to the initial size of the bubbles. Eventually the bubbles begin to coarsen and this is observed in changes in the position of the diffusion diffraction maxima., (Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.)

Uniform silver nanoparticles ranging in size from 12 to 80nm were prepared by reducing silver ammonia complex with resorcinol in presence of Arabic gum. Despite the high ionic strength of the system, the precipitation process yields stable dispersions at metal concentrations as high as 4.0wt% (0.38moldm(-3)). Stable dispersions with higher solids concentration up to 20wt% silver (1.9moldm(-3)) were obtained by subjecting the 'as precipitated' dispersions to ultrafiltration. The effects of reaction parameters (pH, concentration of reactants, metal/stabilizer ratio, and temperature) on particle size and dispersion stability are discussed and a mechanism for the reduction of silver is proposed., (Copyright © 2016 Elsevier Inc. All rights reserved.)

Ultra-high-pressure homogenization (UHPH) was used to generate monodisperse stable peanut oil nanoemulsions within a desired nanosize range (<100 nm) (DNR) stabilized using combinations of whey protein concentrate (WPC), sodium dodecyl sulfate, Triton X-100 (X100), and zwitterionic sulfobetaine-based surfactants differing in hydrophobicity. For WPC [2.0% (w/v)], the dispersed-phase fractions (φ) of 0.05 and 210 MPa significantly reduced the mean globule size (dvs) but the grouped frequency distribution was bimodal and larger than that of DNR. Addition of co-emulsifier sulfobetaine 3-10 (SB3-10) [7.5% (w/w) WPC] gave particles within DNR (dvs of 73 nm) though still in a bimodal distribution. Circular dichroism prior to UHPH showed little disruption of the secondary structure of proteins in WPC by SB3-10, whereas X100 obliterated it. A WPC/SB3-10 mixture retained some periodic structure even when mixed with X100 [10% (w/w) WPC] and remarkably gave a narrow monomodal distribution within DNR with the highest stability reflected by a lack of creaming after storage for 30 days (22 °C).

Structural forces play an important role in the rheology, processing and stability of colloidal systems and complex fluids, with polyelectrolytes representing a key class of structuring colloids. Here, we explore the interactions between soft colloids, in the form of air bubbles, in solutions of monodisperse sodium poly(styrene sulfonate) as a model polyelectrolyte. It is found that by self-consistently modelling the force oscillations due to structuring of the polymer chains along with deformation of the bubbles, it is possible to precisely predict the interaction potential between approaching bubbles. In line with polyelectrolyte scaling theory, two distinct regimes of behaviour are seen, corresponding to dilute and semi-dilute polymer solutions. It is also seen that by blending monodisperse systems to give a bidisperse sample, the interaction forces between soft colloids can be controlled with a high degree of precision. At increasing bubble collision velocity, it is revealed that hydrodynamic flow overwhelms oscillatory structural interactions, showing the important disparity between equilibrium behaviour and dynamic interactions., (Copyright © 2015 Elsevier Inc. All rights reserved.)

The success of the oral delivery of insulin (INS) as a therapeutic protein drug would significantly improve the quality of life of diabetic patients who would otherwise receive multiple daily INS injections. The oral delivery of INS, however, is still limited in its delivery efficiency, which could be due to the chemical, enzymatic, and adsorption barriers. In this work, in an attempt to improve the delivery efficiency, the INS-loaded polymer-lipid hybrid nanoparticles (INS-PLGA-lipid-PEG NPs) were designed and constructed through a double-emulsion solvent evaporation technique, followed by formulation of the spherical micro-particles using a spray freeze dryer (SFD). This kind of dryers has a uniquely designed microfluidic aerosol nozzle (MFAN), ensuring the formation of uniform particles. The resulted particles of ∼212 μm could easily be reverted to discrete INS-PLGA-lipid-PEG NPs in an aqueous solution. The INS-PLGA-lipid-PEG NPs created in this work showed a highly negative surface charge, excellent entrapment efficiency (92.3%) and a sustained drug release (∼24 h). Confocal laser scanning microscopy and flow cytometer were used to show that the cellular uptake efficiency for the INS-PLGA-lipid-PEG NPs was more effective than the INS in Caco-2 cells. More importantly, the in vivo pharmacodynamics demonstrated that the orally delivered system induced a prolonged decrease in blood glucose levels among diabetic rats. The relative bioavailability of INS compared with subcutaneous injection in diabetic rats was found to be approximately 12%. These results suggested that the encapsulated INS-PLGA-lipid-PEG NPs are promising and should be investigated further in the near future as an effective INS oral delivery system., (Copyright © 2015. Published by Elsevier B.V.)

Ultrafine monodisperse bimetallic NiPt nanoparticles with different compositions have been successfully synthesized by coreduction of nickel acetylacetonate and platinum acetylacetonate with borane-tert-butylamine in oleylamine. Among all the catalysts tested, Ni84Pt16/graphene exhibited 100% hydrogen selectivity, and marked high catalytic activity, with TOF values of 415 h(-1) at 50 °C, and 133 h(-1) at 25 °C for hydrogen generation from alkaline solution of hydrazine.

Porous monodisperse chitosan microspheres were synthesized for enzyme immobilization. The microspheres were prepared using microchannels and modified with glutaraldehyde. The microspheres had a mean diameter of 495 µm; the polydispersity indices were less than 0.08, and the specific surface area was between 121 and 173 m(2) /g. Candida sp. 1619 lipase was selected as a model lipase. Immobilization conditions such as enzyme loading, glutaraldehyde concentration, and immobilization time were optimized. The temperature, pH, and storage stability of the free and immobilized enzymes were also investigated. The immobilized enzyme had broad-ranging pH and temperature optima as compared with free enzyme. The storage stability of the immobilized enzyme was higher than that of the free enzyme., (© 2014 International Union of Biochemistry and Molecular Biology, Inc.)

The increasing realisation of the impact of size and surface properties on the bio-distribution of drug loaded colloidal particles has driven the application of micro fabrication technologies for the precise engineering of drug loaded microparticles. This paper demonstrates an alternative approach for producing size controlled drug loaded PLGA based microparticles using silicon Microfluidic Flow Focusing Devices (MFFDs). Based on the precise geometry and dimensions of the flow focusing channel, microparticle size was successfully optimised by modifying the polymer type, disperse phase (Qd) flow rate, and continuous phase (Qc) flow rate. The microparticles produced ranged in sizes from 5 to 50 μm and were highly monodisperse (coefficient of variation <5%). A comparison of Ciclosporin (CsA) loaded PLGA microparticles produced by MFFDs vs conventional production techniques was also performed. MFFDs produced microparticles with a narrower size distribution profile, relative to the conventional approaches. In-vitro release kinetics of CsA was found to be influenced by the production technique, with the MFFD approach demonstrating the slowest rate of release over 7 days (4.99 ± 0.26%). Finally, MFFDs were utilised to produce pegylated microparticles using the block co-polymer, PEG-PLGA. In contrast to the smooth microparticles produced using PLGA, PEG-PLGA microparticles displayed a highly porous surface morphology and rapid CsA release, with 85 ± 6.68% CsA released after 24h. The findings from this study demonstrate the utility of silicon MFFDs for the precise control of size and surface morphology of PLGA based microparticles with potential drug delivery applications., (Copyright © 2014 Elsevier B.V. All rights reserved.)

Simple hexagonal (sh) AB 2 binary superlattices (BSLs) of organic ligand-capped silicon (A; 5.40(±9.8%) nm diameter) and gold (B; 1.88(±10.1%) nm diameter) nanocrystals were assembled by evaporation of colloidal dispersions and characterized using transmission electron microscopy (TEM) and grazing incidence small-angle X-ray scattering (GISAXS). When deposited on tilted substrates by slow evaporation, the sh-AB 2 superlattice contracts slightly towards the substrate with centered orthorhombic structure. Heating the BSL to 200°C in air led to gold coalescence and segregation to the surface of the assembly without disrupting the Si nanocrystal sublattice, thus creating a simple hexagonal superlattice of Si nanocrystals.

This report is a review of the procedures and equipment used in the preparation of polymers of predictable molecular weights and narrow molecular weight distributions. The monomers considered in detail are styrene, α-methylstyrene, isoprene, and butadiene.