Correction: Role of annealing temperature on the sol–gel synthesis of VO2 nanowires with in situ characterization of their metal–insulator transition

Correction for ‘Role of annealing temperature on the sol–gel synthesis of VO₂ nanowires with in situ characterization of their metal–insulator transition’ by Y.-R. Jo et al., RSC Adv., 2018, 8, 5158–5165.

The acknowledgements section in the published article omitted a funder and should instead read: This work was supported by the Samsung Research Funding Center of Samsung Electronics under Project Number SRFC-MA1402-10 and the National Research Foundation of Korea (NRF) under Grant NRF2013S1A2A2035468.The Royal Society of Chemistry apologises for these errors and any consequent inconvenience to authors and readers.     

Role of annealing temperature on the sol–gel synthesis of VO2 nanowires with in situ characterization of their metal–insulator transition

Among the techniques to create VO₂ nanostructures, the sol–gel method is the most facile and benefits from simple, manipulable synthetic parameters. Here, by utilizing various TEM techniques, we report the sequential morphological evolution of VO₂ nanostructures in a sol–gel film spin-coated on a customized TEM grid, which underwent oxygen reduction as the annealing temperature increased. In situ TEM dark-field imaging and Raman spectroscopy allowed us to confirm the sharp phase transition behavior of an individual nanowire by illustrating the effect of electrode-clamping-induced tensile stress on the nucleation of the R phase from the M1 phase. The electrical transport properties of a single-nanowire device fabricated on a customized TEM grid showed excellent control of the stoichiometry and crystallinity of the wire. These results offer critical information for preparing tailored VO₂ nanostructures with advanced transition properties by the sol–gel method to enable the fabrication of scalable flexible devices.

The single-VO₂ nanowire device synthesized via sequential morphological evolutions with oxygen reduction during annealing features a sharp metal-insulator transition.     

Effects of Ti-doping amount and annealing temperature on electrochromic performance of sol–gel derived WO3

Fine control of structural and morphological features in electrochromic materials is of paramount importance for realizing practical electrochromic devices (ECDs), which can dynamically adjust indoor light and temperature of buildings. To this end, herein we investigate impacts of two variants such as Ti-doping amount and the annealing temperature on physical and chemical properties of sol–gel derived electrochromic WO₃ films. We use a wide range of titanium coupling agents (TCAs) as Ti-dopants ranging from 0 wt% to 20 wt% and vary the annealing temperature between 200 °C and 400 °C with 50 °C interval. Both variants greatly influence the physical properties of the resulting WO₃ films, resulting in different crystallinities and morphologies. Through complementary analytical techniques, we find that the WO₃ film featuring an amorphous phase with nano-porous morphology enhances the electrochemical and electrochromic performances. The specific TCA used in this study helps stabilize the amorphous WO₃ structure and generate the nano-pores during the following thermal treatment via its thermal decomposition. As a result, the WO₃ film having an optimal 8 wt% TCA annealed at 300 °C shows a high optical density of 73.78% in visible light (400–780 nm), rapid switching speed (t_c = 5.12 s and t_b = 4.74 s), and high coloration efficiency of 52.58 cm² C⁻¹ along with a superior cyclic stability. Thus, understanding a structure–property relationship is of paramount importance in engineering the advanced electrochromic WO₃ for use in practical ECDs and other optoelectronic applications.

Fine-control of structural properties of WO₃. Faster and balanced charge transfer kinetics. Higher coloration efficiency.     

Controlled sol–gel synthesis of oxygen sensing CdO : ZnO hexagonal particles for different annealing temperatures

CdO : ZnO hexagonal particles were synthesized by a sol–gel precipitation method at different annealing temperatures. A mixed crystal phase of cubic and wurtzite structures was observed from X-ray diffraction patterns. The micrographs showed hexagonal shapes of the CdO : ZnO nanocomposites particles. The energy dispersive X-ray spectroscopy mapping images showed a uniform distribution of the Cd and Zn. The CdO : ZnO nanocomposite pallet annealed at 550 °C has an electrical resistance of 0.366 kΩ at room temperature. The nanocomposites showed an excellent sensing response against oxygen gas with a sensing response of 47% at 200 °C for the CdO : ZnO particles annealed at 550 °C. The sensor response and recovery times were found to be 43s and 45s, respectively. The sensor response was due to the sorption of oxygen ions on the surfaces of the CdO : ZnO hexagonal particles.

CdO : ZnO hexagonal particles were synthesized by a sol–gel precipitation method at different annealing temperatures.     

Green and facile sol–gel synthesis of the mesoporous SiO2–TiO2 catalyst by four different activation modes

The most environmentally friendly protocol for obtaining mesoporous SiO₂–TiO₂ catalysts has been sought. Water has been employed as a green solvent, the energy input has been minimized, and three further principles (1, 3, and 12) of Green Chemistry have been considered. Four different modes for promoting the reaction have been comparatively evaluated, namely near-infrared and microwave electromagnetic irradiations, ultrasound, and traditional mantle heating. Brunauer–Emmett–Teller (BET) analyses of the catalysts produced revealed that the non-conventional activation modes afforded both large surface areas (335–441 m² g⁻¹) and smaller crystal sizes (7.2–15.3 nm) than the mantle heating process. These modes also generated the catalysts in shorter reaction times than traditional mantle heating, 10–30 min versus 3 h, with anatase as the sole crystalline phase. The photocatalytic degradation of 4-chlorophenol has been carried out to assess the catalytic efficiencies of the hybrid materials. The catalyst synthesized with microwave assistance showed the best mineralization activity (97%), followed by those prepared with ultrasound, near-infrared, and mantle heating. The materials have been extensively characterized by FTIR, XRD, DRS-UV/Vis, SEM, ²⁹Si MAS NMR, and BET analyses. To the best of our knowledge, this is the first such comparative assessment of green energetic alternatives in developing a sol–gel process.

The most environmentally friendly protocol for obtaining mesoporous SiO₂–TiO₂ catalysts has been sought.     

Green sol–gel auto combustion synthesis and characterization of double perovskite Tb2ZnMnO6 nanoparticles and a brief study of photocatalytic activity

In this work, new double perovskite Tb₂ZnMnO₆ nanoparticles were successfully synthesized by a sol–gel auto combustion method. To synthesize these nanoparticles, three known sugars, lactose, fructose, and maltose, and liquorice powder, which contains quantities of sugar and other organic compounds, were used as fuel. Images obtained from Scanning Electron Microscopy (SEM) analysis implied that maltose-based nanoparticles are homogenous and less in particle size. Further, different maltose ratios were applied to get the best size and morphology. The optimum sample was used to continue the other analysis to check other features of the nanoparticles. Also, the optimum sample was used for the removal of dye contamination under the photocatalytic process. Photocatalytic tests were performed in neutral and alkaline pH conditions under UV-light irradiation. It has been found that the decolorization percent for methyl orange was about 35% and for methyl violet about 55% at neutral pH. Also, this value for methyl violet was about 90% at pH = 8. The results obtained from the study of photocatalytic properties introduce these nanoparticles as a desirable option for removing dye contaminants from aqueous media.

In this work, new double perovskite Tb₂ZnMnO₆ nanoparticles were successfully synthesized by a sol–gel auto combustion method.     

Synthesis of monolithic shape-stabilized phase change materials with high mechanical stability via a porogen-assisted in situ sol–gel process

The confinement of phase change materials (PCMs) in construction materials has recently solved leakage, supercooling and low thermal conductivity problems in the industrial use of PCMs as monolithic thermal energy storage materials. To produce shape-stabilized PCMs (ss-PCMs) as crack-free monoliths, less than 15–30% v/v pure or encapsulated PCMs can be used in construction materials. Therefore, the heat storage capacity of these monolithic ss-PCM boards is comparatively low. In this study, we synthesized a novel class of monolithic ss-PCM boards with high compressive strength of 0.7 MPa at 30 °C (1.2 MPa at 10 °C), high PCM loadings of 86 wt%, and latent heats in the range of 100 J g⁻¹via a porogen-assisted in situ sol–gel process. We confined butyl stearate (BS) as PCM in a core-shell-like silica matrix via stabilized silica sol as silica source, sodium dodecyl sulfate as surfactant and poly(vinyl alcohol) as co-polymer. The ss-PCMs obtained are hydrophobic, thermally stable up to 320 °C and perform 6000 state transitions from solid to liquid and vice versa, without losing melting or freezing enthalpies. We analyzed the silica structure in the ss-PCMs to understand in detail the reasons for the high mechanical stability. The silica structure in ss-PCMs consists of spherical meso- and macropores up to 10 000 nm filled with PCM, formed mostly by BS droplets in water as templates during gelation. With an increasing BS amount in the synthesis of ss-PCMs, the total nanopore volume filled with PCM in ss-PCMs increases, resulting in higher compressive strengths up to 500% and thermal conductivities up to 60%.

Nanoconfinement of PCMs in core-shell-like silica structures via an inexpensive porogen-assisted sol–gel process to produce shape-stabilized PCMs as monoliths with high mechanical stability and high loading capacity.     

Synthesis of Ni2+ ion doped ZnO–MWCNTs nanocomposites using an in situ sol–gel method: an ultra sensitive non-enzymatic uric acid sensing electrode material

Nickel (Ni²⁺) ion doped zinc oxide-multi-wall carbon nanotubes (NZC) with different composition ratios of MWCNTs (from 0.01 to 0.1 wt%) are synthesized through an in situ sol–gel method. The synthesized NZC nanocomposites (NCs) are used as electrode materials with glassy carbon electrodes (GCEs) for electrochemical detection of uric acid (UA). The cyclic voltammogram of the representative NZC 0.1 modified GCE (NZC 0.1/GCE) revealed the highest electrochemical sensing activity towards the oxidation of UA at 0.37 V in 0.2 M phosphate buffer solution (PBS) having pH 7.4 ± 0.02. The limit of detection (LOD) and limit of quantification (LOQ) for the NZC 0.1/GCE are determined to be 5.72 nM and 19.00 nM (S/N = 3) respectively, which is the lowest compared to the literature values reported for enzymatic and non-enzymatic detection techniques. The synergistic effect of NZC 0.1 NCs is proposed as one of the factors for the enhanced electrochemical oxidation of UA complemented by the phase, lattice parameters, functional groups, morphology, elemental compositions, types of bonding and specific surface area with pore size ascertained using various techniques. The synthesized NZC 0.1 NCs are further proposed as selective electrode materials for the electrochemical detection of UA as authenticated further by performing interference tests with other metabolites such as ascorbic acid (AA), dopamine (DA) and d-glucose. The optimized electrochemical studies are further adopted for sensing of UA from human excretion samples using NZC 0.1 NCs.

Nickel (Ni²⁺) ion doped zinc oxide-multi-wall carbon nanotubes (NZC) with different composition ratios of MWCNTs (from 0.01 to 0.1 wt%) are synthesized through an in situ sol–gel method.     

Preparation and anti-coking application of sol–gel SiO2 coating in a delayed coking furnace

To isolate iron sulphide and reduce coke adhesion reactions that occur on the surface of a delayed coking furnace, a SiO₂ coating was developed on Cr9Mo alloy by employing the sol–gel method. The coating was characterised through Fourier transformation infrared spectroscopy, X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, potentiodynamic scanning, InfiniteFocus optical 3D surface metrology, thermal shock and coking experiments. After heat treatment at 550 °C, the silicon methyl groups were oxidised and the coating exhibited a Si–O–Si connected crosslinked network structure. The coating surface was uniformly dense with a roughness and thickness of 0.2 and approximately 4 μm, respectively. The coating still adhered to the substrate tightly after 20 cycles of thermal shock treatment. Compared with an uncoated sample, the coating effectively improved the corrosion resistance of the substrate, suppressed the iron sulphide reaction, and reduced coke adhesion onto the sample. The coating had a better inhibition effect on coke fouling in a delayed coking furnace.

To isolate iron sulphide and reduce coke adhesion reactions that occur on the surface of a delayed coking furnace, a SiO₂ coating was developed on Cr9Mo alloy by employing the sol–gel method.     

Auxiliary-directed etherification of sp2 C–H bonds under heterogeneous metal–organic framework catalysis: synthesis of ethenzamide

An efficient protocol for 8-aminoquinoline assisted alkoxylation and phenoxylation of sp² C–H bonds under heterogeneous catalysis was developed. The optimal conditions employed Cu-MOF-74 (20%), K₂CO₃ base, pyridine ligand or dimethyl formamide solvent, and O₂ oxidant at 80 °C or 100 °C for 24 hours. Cu-MOF-74 revealed remarkably higher activity when compared with other previously commonly used Cu-MOFs in cross coupling reactions, supported copper catalysts, and homogeneous copper salts. The reaction scope with respect to coupling partners included a wide range of various substrates. Interestingly, the developed conditions are applicable for the synthesis of high-profile relevant biological agents from easily accessible starting materials. Furthermore, a leaching test confirmed the reaction heterogeneity and the catalyst was reused and recycled at least 8 times with trivial degradation in activity.

An efficient protocol for 8-aminoquinoline assisted alkoxylation and phenoxylation of sp² C–H bonds under heterogeneous catalysis was developed.     

A molecular dynamics study on the mechanical properties of Fe–Ni alloy nanowires and their temperature dependence

Fe–Ni alloy nanowires are widely used in high-density magnetic memories and catalysts due to their unique magnetic and electrochemical properties. Understanding the deformation mechanism and mechanical property of Fe–Ni alloy nanowires is of great importance for the development of devices. However, the detailed deformation mechanism of the alloy nanowires at different temperatures is unclear. Herein, the deformation mechanism of Fe–Ni alloy nanowires and their mechanical properties were investigated via the molecular dynamics simulation method. It was found that the local atomic pressure fluctuation of the Fe–Ni alloy nanowire surface became more prominent with an increase in the Ni content. At low temperature conditions (<50 K), the plastic deformation mechanism of the Fe–Ni alloy nanowires switched from the twinning mechanism to the dislocation slip mechanism with the increase in the Ni content from 0.5 at% to 8.0 at%. In the temperature range of 50–800 K, the dislocation slip mechanism dominated the deformation. Simulation results indicated that there was a significant linear relationship between the Ni content, temperature, and ultimate stress in the temperature range of 50–800 K. Our research revealed the association between the deformation mechanism and temperature in Fe–Ni alloy nanowires, which may facilitate new alloy nanowire designs.

Deformation mechanism and mechanical property of Fe–Ni alloy nanowires are investigated through molecular dynamics simulation method.     

Correction: Tantalum(v) 1,3-propanediolate β-diketonate solution as a precursor to sol–gel derived,metal oxide thin films

Correction for ‘Tantalum(v) 1,3-propanediolate β-diketonate solution as a precursor to sol–gel derived, metal oxide thin films’ by Christopher Beale et al., RSC Adv., 2020, 10, 13737–13748, DOI: 10.1039/D0RA02558E.

The authors regret that the plasma treatment and printing parameters were reported incorrectly in the subsection “Deposition on a-SiO₂ for UV/Vis spectrophotometry” in the Experimental section of the original article.Before printing, the substrate for both samples was subjected to an argon plasma treatment for 5 minutes (150 W, 0.6 mbar). The plasma power is now corrected to be the same as stated in the “Deposition on a-SiO₂ for Raman/XRD” subsection, where originally it was incorrectly stated that “the power was set slightly higher” for the Raman/XRD samples. For both the acetylacetone and benzoylacetone inks, the inks were printed on their respective substrates with a 75 μm drop pitch having dimensions of 400 × 220 drops to create a uniform layer.The correct section is as follows:     

Synthesis of simple,low cost and benign sol–gel Cu2InxZn1−xSnS4 alloy thin films: influence of different rapid thermal annealing conditions and their photovoltaic solar cells

Cu₂In_xZn_1−xSnS₄ (x = 0.4) alloy thin films were synthesized on soda lime glass (SLG) substrate by a simple low-cost sol–gel method followed by a rapid annealing technique. The influence of sulfurization temperature and sulfurization time on the structure, morphology, optical and electrical properties of Cu₂In_xZn_1−xSnS₄ thin films was investigated in detail. The XRD and Raman results indicated that the crystalline quality of the Cu₂In_xZn_1−xSnS₄ alloy thin films was improved, accompanied by metal deficiency, particularly tin loss with increasing the sulfurization temperature and sulfurization time. From absorption spectra it is found that the band gaps of all Cu₂In_xZn_1−xSnS₄ films are smaller than that (1.5 eV) of the pure CZTS film due to In doping, and the band gap of the Cu₂In_xZn_1−xSnS₄ films can be tuned in the range of 1.38 to 1.19 eV by adjusting the sulfurization temperature and sulfurization time. Hall measurement results showed that all Cu₂In_xZn_1−xSnS₄ alloy thin films showed p-type conductivity characteristics, the hole concentration decreased and the mobility increased with the increase of sulfurization temperature and sulfurization time, which is attributed to the improvement of the crystalline quality and the reduction of grain boundaries. Finally, the Cu₂In_xZn_1−xSnS₄ film possessing the best p-type conductivity with a hole concentration of 9.06 × 10¹⁶ cm⁻³ and a mobility of 3.35 cm² V⁻¹ s⁻¹ was obtained at optimized sulfurization condition of 580 °C for 60 min. The solar cell using Cu₂In_xZn_1−xSnS₄ as the absorber obtained at the optimized sulfurization conditions of 580 °C for 60 min demonstrates a power conversion efficiency of 2.89%. We observed an increment in open circuit voltage by 90 mV. This work shows the promising role of In in overcoming the low V_oc issue in Cu-kesterite thin film solar cells.

Cu₂In_xZn_1−xSnS₄ (x = 0.4) alloy thin films were synthesized on soda lime glass (SLG) substrate by a simple low-cost sol–gel method followed by a rapid annealing technique.     

Photocatalytic activity of Ag/Al2O3–Gd2O3 photocatalysts prepared by the sol–gel method in the degradation of 4-chlorophenol

The photocatalytic activity in the degradation of 4-chlorophenol (4-ClPh) in aqueous medium (80 ppm) using 2.0 wt% Ag/Al₂O₃–Gd₂O₃ (Ag/Al–Gd-x; where x = 2.0, 5.0, 15.0, 25.0 and 50.0 wt% of Gd₂O₃) photocatalysts prepared by the sol–gel method was studied under UV light irradiation. The photocatalysts were characterized by N₂ physisorption, X-ray diffraction, SEM, HRTEM, UV-Vis, XPS, FTIR and fluorescence spectroscopy. About 67.0% of 4-ClPh was photoconverted after 4 h of UV light irradiation using Ag/γ-–Al₂O₃. When Ag/Al–Gd-x photocatalysts were tested, the 4-ClPh photoconversion was improved and more than 90.0% of 4-ClPh was photoconverted after 3 h of UV light irradiation in the materials containing 15.0 and 25.0 wt% of Gd₂O₃. Ag/Al–Gd-25 was the material with the highest efficacy to mineralize dissolved organic carbon, mineralizing more than 85.0% after 4 h of UV light irradiation. Silver nanoparticles and micro-particles of irregular pentagonal shape intersected by plane nanobelts of Al₂O₃–Gd₂O₃ composite oxide were detected in the Ag/Al–Gd-25 photocatalyst. This material is characterized by a lowest recombination rate of electron–hole pairs. The low recombination rate of photo-induced electron–hole pairs in the Ag/Al–Gd-x photocatalysts with high Gd₂O₃ contents (≥15.0 wt%) confirmes that the presence of silver nanoparticles and microparticles interacting with Al₂O₃–Gd₂O₃ composite oxide entities favors the separation of photo-induced charges (e⁻ and h⁺). These materials could be appropriate to be used as highly efficient photocatalysts to eliminate high concentrations of 4-ClPh in aqueous medium.

Ag/Al₂O₃–Gd₂O₃ showed high efficacy to photodegradate 4-chlorophenol, the strong interaction between silver nano-particles and micro-particles and Al₂O₃–Gd₂O₃ entities favors the decrease in the recombination rate.     

Fabrication of hydroxyapatite coatings on AZ31 Mg alloy by micro-arc oxidation coupled with sol–gel treatment

Magnesium (Mg) alloys, can potentially be used as biodegradable orthopedic implants because of their biodegradability and good mechanical properties. However, a quick degradation rate and low bioactivity have prevented their clinical application. In order to enhance the corrosion resistance and the in vitro bioactivity of Mg alloys, protective composite coatings were prepared on AZ31 magnesium alloy followed by sol–gel sealing treatment under low-pressure conditions. The morphologies, crystalline structure and the composition of the samples were characterized by SEM, XRD, and XPS. Electrochemical corrosion test and the in vitro bioactivity were also studied. The results indicated that the composite coatings not only improved the corrosion resistance, but also enhanced the in vitro bioactivity of AZ31 Mg alloy. Therefore, Mg alloy treated with micro-arc oxidation and sol–gel offers a promising approach for biodegradable bone implants.

Magnesium (Mg) alloys, can potentially be used as biodegradable orthopedic implants because of their biodegradability and good mechanical properties.     

Characteristics of Ag-incorporated bioactive glasses prepared by a modified sol–gel method with a shortened synthesis time and without the use of catalysts

This work presents the preparation of bioactive glasses 70SiO₂–(26 − x)CaO–4P₂O₅–xAg₂O (with x = 0, 1, 3, 10 mol%) by a modified sol–gel method with reduced synthesis time based on hydrothermal reaction in a medium without acid or base catalysts. The synthetic materials were characterized by several physical–chemical techniques such as TG-DSC, XRD, SEM, TEM, and N₂ adsorption/desorption measurement. The analysis data confirmed that the glass sample not containing Ag has a completely amorphous structure, while glass samples containing Ag exhibited a pure phase of metallic nano-silver in the glass amorphous phase. All the synthetic glasses have mesoporous structures with particle sizes of less than 30 nm. The addition of silver to the bioactive glass structure in general did not drastically reduce the specific surface areas and pore volumes of glasses as in previous studies. The bioactivity of the silver-incorporated glasses did not reduce, and even increased in the cases of bioactive glass containing 3, and 10 mol% of Ag₂O. The biocompatibility of synthetic glasses with fibroblast cells (L-929) was confirmed, even with glass containing high amounts of Ag. Representatively, Ag-incorporated glass samples (sample x = 3, and x = 10) were selected to check the antibacterial ability using bacterial strain Pseudomonas aeruginosa ATCC 27853 (Pa). The obtained results indicated that these glasses exhibited good antibacterial ability to Pseudomonas aeruginosa. Thus, the synthetic method in this study proved to be a fast, environmentally friendly technique for synthesizing Ag-incorporated glass systems. The synthesized glasses show good bioactive, biocompatible, and antibacterial properties.

This work presents the preparation of bioactive glasses 70SiO₂–(26 − x)CaO–4P₂O₅–xAg₂O (with x = 0, 1, 3, 10 mol%) by a modified sol–gel method with reduced synthesis time based on hydrothermal reaction in a medium without acid or base catalysts.     

Enhanced CO2 methanation at mild temperature on Ni/zeolite from kaolin: effect of metal–support interface

Catalytic CO₂ hydrogenation to CH₄ offers a viable route for CO₂ conversion into carbon feedstock. The research aimed to enhance CO₂ conversion at low temperature and to increase the stability of Ni catalysts using zeolite as a support. NaZSM-5 (MFI), NaA (LTA), NaY (FAU), and NaBEA (BEA) synthesized from kaolin were impregnated with 15% Ni nanoparticles in order to elucidate the effect of surface area, porosity and basicity of the zeolite in increasing Ni activity at mild temperature of ∼200 °C. A highly dispersed Ni catalyst was produced on high surface area NaY meanwhile the mesoporosity of ZSM-5 has no significant effect in improving Ni dispersion. However, the important role of zeolite mesoporosity was observed on the stability of the catalyst. Premature deactivation of Ni/NaA within 10 h was due to the relatively small micropore size that restricted the CO₂ diffusion, meanwhile Ni/NaZSM-5 with a large mesopore size exhibited catalytic stability for 40 h of reaction. Zeolite NaY enhanced Ni activity at 200 °C to give 21% conversion with 100% CH₄ selectivity. In situ FTIR analysis showed the formation of hydrogen carbonate species and formate intermediates at low temperatures on Ni/NaY, which implied the efficiency of electron transfer from the basic sites of NaY during CO₂ reduction. The combination of Ni/NaY interfacial interaction and NaY surface basicity promoted CO₂ methanation reaction at low temperature.

Different Na-zeolites as supports of Ni metal were successfully synthesized from kaolin-based material. Combination of interfacial interaction Ni-support and surface basicity promoted CO₂ methanation reaction at a low temperature of ∼200 °C.     

Enhanced mechanical properties of hBN–ZrO2 composites and their biological activities on Drosophila melanogaster: synthesis and characterization

In this study, six compositions in the system [x(h-BN)–(100 − x)ZrO₂] (10 ≤ x ≤ 90) were synthesized by a bottom up approach, i.e., the solid-state reaction technique. XRD results showed the formation of a novel and main phase of zirconium oxynitrate ZrO(NO₃)₂ and SEM exhibited mixed morphology of layered and stacked h-BN nanosheets with ZrO₂ grains. The composite sample 10 wt% h-BN + 90 wt% ZrO₂ (10B90Z) showed outstanding mechanical properties for different parameters, i.e., density (3.12 g cm⁻³), Young''s modulus (10.10 GPa), toughness (2.56 MJ m⁻³), and maximum mechanical strength (227.33 MPa). The current study further checked the in vivo toxicity of composite 10B90Z and composite 90B10Z using Drosophila melanogaster. The composite 10B90Z showed less cytotoxicity in this model, while the composite 90B10Z showed higher toxicity in terms of organ development as well as internal damage of the gut mostly at the lower concentrations of 1, 10, and 25 μg mL⁻¹. Altogether, the current study proposes the composite 10B90Z as an ideal compound for applications in biomedical research. This composite 10B90Z displays remarkable mechanical and biological performances, due to which we recommend this composition for various biomedical applications.

In this study, six compositions in the system [x(h-BN)–(100 − x)ZrO₂], (10 ≤ x ≤ 90) were synthesized by a bottom up approach, i.e., the solid-state reaction technique.     

Multiblock copolymers of PPC with oligomeric PBS: with low brittle–toughness transition temperature

In order to decrease the brittle–toughness transition temperature and increase the mechanical strength of poly(propylene carbonate) (PPC), a series of multiblock copolymers of poly(propylene carbonate)-multiblock-poly(butylene succinate) (PPC-mb-PBS) are designed and synthesized. ¹H-NMR, DOSY and GPC results demonstrate the successful synthesis of PPC-mb-PBSs with designed multiblock sequence. The thermal, crystalline and mechanical properties of these PPC-mb-PBSs are evaluated by DSC, TGA, POM, tensile and tearing testing. Experiment results demonstrate that crystallinity, thermal and mechanical properties of PPC-mb-PBSs can be readily modulated by changing the composition and block length of PPC and PBS moieties. It is found that all the prepared PPC-mb-PBSs are semi-crystalline polymers with a melting temperature at 93–109 °C and a T_g at around −40 °C. Both crystallization rate and crystallinity of the multiblock copolymers increase with increasing both PBS content and PBS block length. As a consequent, the tensile strength increases with increasing PBS/PPC block ratios at room and lower temperatures. In conclusion, the amorphous PBS phase in the block copolymers acts as soft segment, endowing PPC-mb-PBS copolymers with much better flexibility than PPC at low temperature of 273 K when PPC segments are frozen.

In present work, biodegradable multiblock copolymers from oligomeric PPC and PBS with low brittle–toughness transition temperature and superior mechanical properties was synthesized, making it more potential candidate as packaging materials.     

Copper-catalyzed one-pot domino reactions via C–H bond activation: synthesis of 3-aroylquinolines from 2-aminobenzylalcohols and propiophenones under metal–organic framework catalysis

A Cu₂(OBA)₂(BPY) metal–organic framework was utilized as a productive heterogeneous catalyst for the synthesis of 3-aroylquinolines via one-pot domino reactions of 2-aminobenzylalcohols with propiophenones. This Cu-MOF was considerably more active towards the one-pot domino reaction than a series of transition metal salts, as well as nano oxide and MOF-based catalysts. The MOF-based catalyst was reusable without a significant decline in catalytic efficiency. To the best of our knowledge, the transformation of 2-aminobenzylalcohols to 3-aroylquinolines was not previously reported in the literature, and this protocol would be complementary to previous strategies for the synthesis of these valuable heterocycles.

Cu₂(OBA)₂(BPY) metal–organic framework was utilized as a productive heterogeneous catalyst for the synthesis of 3-aroylquinolines via one-pot domino reactions of 2-aminobenzylalcohols with propiophenones.