Low Temperature Synthesis of 2D p-Type α-In2Te3 with Fast and Broadband Photodetection.

2D A 2 III B 3 VI ${\mathrm{A}}_2^{{\mathrm{III}}}{\mathrm{B}}_3^{{\mathrm{VI}}}$ compounds (A = Al, Ga, In, and B = S, Se, and Te) with intrinsic structural defects offer significant opportunities for high-performance and functional devices. However, obtaining 2D atomic-thin nanoplates with non-layered structure on SiO2/Si substrate at low temperatures is rare, which hinders the study of their properties and applications at atomic-thin thickness limits. In this study, the synthesis of ultrathin, non-layered α-In2Te3 nanoplates is demonstrated using a BiOCl-assisted chemical vapor deposition method at a temperature below 350 °C on SiO2/Si substrate. Comprehensive characterization results confirm the high-quality single crystal is the low-temperature cubic phase α-In2Te3 , possessing a noncentrosymmetric defected ZnS structure with good second harmonic generation. Moreover, α-In2Te3 is revealed to be a p-type semiconductor with a direct and narrow bandgap value of 0.76 eV. The field effect transistor exhibits a high mobility of 18 cm2 V-1 s-1, and the photodetector demonstrates stable photoswitching behavior within a broadband photoresponse from 405 to 1064 nm, with a satisfactory response time of τrise = 1 ms. Notably, the α-In2Te3 nanoplates exhibit good stability against ambient environments. Together, these findings establish α-In2Te3 nanoplates as promising candidates for next-generation high-performance photonics and electronics.

Low-Temperature Fabrication of Bulk-Type All-Solid-State Lithium-Ion Battery Utilizing Nanosized Garnet Solid Electrolytes.

Garnet-type Li7 La3 Zr2 O12 (LLZ) materials are attracting attention as solid electrolytes (SEs) in oxide-based all-solid-state batteries (ASSBs) owing to their high ionic conductivity. Although the electrochemical stability of LLZ against Li metal is demonstrated with possible high energy density, high-temperature sintering above 1000 °C, which is required to achieve high Li-ion conductivity, results in the formation of insulating impurities at the electrode-electrolyte interfaces. Here, nanosized fine-particle samples of Ta-substituted Li6.5 La3 Zr1.5 Ta0.5 O12 (LLZT) are successfully prepared at a remarkably low temperature of 400 °C utilizing an amorphous precursor oxide. The dense LLZT SE sintered by hot pressing at 500 °C shows room-temperature Li-ion conductivity of 1.03 × 10-4 S cm-1 without any additives. In addition, the bulk-type NCM-graphite full battery cell fabricated with the LLZT fine particles through a hot-pressing sintering method at 550 °C exhibits a good charge-discharge performance at room temperature with the bulk-type areal discharge capacity of 0.831 mAh cm-2 . The nanosized garnet SE strategy demonstrated in this study paves the way for the formation of oxide-based ASSBs by low-temperature sintering.

Mild Microfluidic Approaches to Oxide Nanoparticles Synthesis.

Oxide nanoparticles (oxide NPs) are advanced materials with a wide variety of applications in different fields. The use of continuous flow methods is particularly appealing for their synthesis due to the high control achieved over the reaction conditions and the easy process scalability. The present review focuses on the preparation of oxide NPs using microfluidic setups at low temperature (≤80 °C), since the employment of mild reaction conditions is crucial for developing sustainable and cost-effective processes. A particular emphasis will be put on the improvement over the final product features (e. g., size, shape, and size distribution) given by flow methods with respect to conventional batch procedures. The main issues that arise by treating NPs suspensions in microfluidic systems are product deposition or channel clogging; mitigation strategies to overcome these drawbacks will also be presented and discussed.

Layer exchange synthesis of multilayer graphene.

Low-temperature synthesis of multilayer graphene (MLG) on arbitrary substrates is the key to incorporating MLG-based functional thin films, including transparent electrodes, low-resistance wiring, heat spreaders, and battery anodes in advanced electronic devices. This paper reviews the synthesis of MLG via the layer exchange (LE) phenomenon between carbon and metal from its mechanism to the possibility of device applications. The mechanism of LE is completely different from that of conventional MLG precipitation methods using metals, and the resulting MLG exhibits unique features. Modulation of metal species and growth conditions enables synthesis of high-quality MLG over a wide range of growth temperatures (350 °C-1000 °C) and MLG thicknesses (5-500 nm). Device applications are discussed based on the high electrical conductivity (2700 S cm-1) of MLG and anode operation in Li-ion batteries. Finally, we discuss the future challenges of LE for MLG and its application to flexible devices.

Low-Temperature Synthesis of Solution Processable Carbon Nitride Polymers.

Carbon nitride materials require high temperatures (>500 °C) for their preparation, which entails substantial energy consumption. Furthermore, the high reaction temperature limits the materials' processability and the control over their elemental composition. Therefore, alternative synthetic pathways that operate under milder conditions are still very much sought after. In this work, we prepared semiconductive carbon nitride (CN) polymers at low temperatures (300 °C) by carrying out the thermal condensation of triaminopyrimidine and acetoguanamine under a N2 atmosphere. These molecules are isomers: they display the same chemical formula but a different spatial distribution of their elements. X-ray photoelectron spectroscopy (XPS) experiments and electrochemical and photophysical characterization confirm that the initial spatial organization strongly determines the chemical composition and electronic structure of the materials, which, thanks to the preservation of functional groups in their surface, display excellent processability in liquid media.

Low-Temperature Synthesis of Honeycomb CuP2 @C in Molten ZnCl2 Salt for High-Performance Lithium Ion Batteries.

Phosphorus-rich metal phosphides have very high lithium storage capacities, but they are difficult to prepare. A low-temperature phosphorization method based on Mg reducing PCl3 in ZnCl2 molten salt at 300 °C is developed to synthesize phosphorus-rich CuP2 @C from a Cu-MOF derived Cu@C composite. Abnormal oxidation of Cu by Zn2+ in the molten salt is observed, which leads to the porous honeycomb nanostructure and homogeneously distributed ultrafine CuP2 nanocrystals. The honeycomb CuP2 @C exhibits excellent lithium storage performance with high reversible capacity (1146 mAh g-1 at 0.2 A g-1 ) and superior cycling stability (720 mAh g-1 after 600 cycles at 1.0 A g-1 ), showing the promising application of P-rich metal phosphides in lithium ion batteries.

Exploring the Phase-Selective, Green, Hydrothermal Synthesis of Upconverting Doped Sodium Yttrium Fluoride: Effects of Temperature, Time, and Precursors.

The aim of this work was i) to develop a hydrothermal, low-temperature synthesis protocol affording the upconverting hexagonal phase NaYF4 with suitable dopants while adhering to the "green chemistry" standards and ii) to explore the effect that different parameters have on the products. In optimizing the synthesis protocol, short reaction times and low temperatures (below 150 °C) were considered. Yb3+ and Er3+ ions were chosen as dopants for the NaYF4 material. Within the context of the second goal, parameters including nature of the precursors, treatment temperature, and treatment time were investigated to afford a pure hexagonal crystalline phase, both in the doped and undoped materials. To fully explore the synthesis results, the prepared materials were characterized from a structural (XRD), compositional (XPS, ICP-MS), and morphological (SEM) point of view. The upconverting properties of the compounds were confirmed by photoluminescence measurements.

Phase-Engineered PtSe2 -Layered Films by a Plasma-Assisted Selenization Process toward All PtSe2 -Based Field Effect Transistor to Highly Sensitive, Flexible, and Wide-Spectrum Photoresponse Photodetectors.

The formation of PtSe2 -layered films is reported in a large area by the direct plasma-assisted selenization of Pt films at a low temperature, where temperatures, as low as 100 °C at the applied plasma power of 400 W can be achieved. As the thickness of the Pt film exceeds 5 nm, the PtSe2 -layered film (five monolayers) exhibits a metallic behavior. A clear p-type semiconducting behavior of the PtSe2 -layered film (≈trilayers) is observed with the average field effective mobility of 0.7 cm2 V-1 s-1 from back-gated transistor measurements as the thickness of the Pt film reaches below 2.5 nm. A full PtSe2 field effect transistor is demonstrated where the thinner PtSe2 , exhibiting a semiconducting behavior, is used as the channel material, and the thicker PtSe2 , exhibiting a metallic behavior, is used as an electrode, yielding an ohmic contact. Furthermore, photodetectors using a few PtSe2 -layered films as an adsorption layer synthesized at the low temperature on a flexible substrate exhibit a wide range of absorption and photoresponse with the highest photocurrent of 9 µA under the laser wavelength of 408 nm. In addition, the device can maintain a high photoresponse under a large bending stress and 1000 bending cycles.

A glassy carbon electrode modified with N-doped carbon dots for improved detection of hydrogen peroxide and paracetamol.

Nitrogen doped carbon dots (NCDs) were synthesized using a low temperature approach and used to modify a glassy carbon electrode (GCE) via dipping. The oxygen groups on the surface of the NCDs, and the charge delocalization of the NCDs warrant an excellent electrocatalytic activity of the GCE toward oxidation of paracetamol (PA) and reduction of H2O2. PA and H2O2 were detected at 0.34 V and -0.4 V (both vs. Ag/AgCl) using differential pulse voltammetry and amperometric I-T measurement, respectively. The modified GCE has a linear response to PA in the 0.5 to 600 µM concentration range, and to H2O2 in the 0.05 µM to 2.25 mM concentration range. The detection limits are 157 nM and 41 nM, respectively. In our perception, the modified GCE holds promise for stable, selective and sensitive determination of PA and H2O2 in pharmaceutical analysis. Graphic abstract Nitrogen doped carbon dots (NCDs) were synthesized and used to modify a glassy carbon electrode. Surface functional groups on NCDs can trigger electrocatalytic reactions toward paracetamol oxidation and H2O2 reduction with high sensitivities.

TbCu7-type Sm-Fe(-N) powder synthesized by low-temperature reduction-diffusion process using the Li-Ca reductant.

It was predicted that TbCu7-type Sm-Fe powder prepared by the low-temperature reduction-diffusion (LTRD) process using a Li-Ca reductant would contain no residual ɑ-Fe because this reductant would not produce the absorbed water that hinders the reaction between Sm and Fe by forming oxychlorides when molten salt is used as the reductant. Contrary to this expectation, a detailed microstructure analysis revealed that a residual phase of unreacted ɑ-Fe existed in some TbCu7-type Sm-Fe particles rather than as separate Fe particles. This residual ɑ-Fe phase was not located in the center of the Sm-Fe particles and was not detected in some Sm-Fe particles, suggesting that the reason for the residual ɑ-Fe phase is inhomogeneous diffusion of Sm into the Fe due to slow diffusion at low temperatures. Although this TbCu7-type Sm-Fe powder contained a small amount of unreacted ɑ-Fe phase, the magnetic properties of the nitride TbCu7-type Sm-Fe were also estimated.

Low-Temperature Synthesis of Mesoporous Half-Metallic High-Entropy Spinel Oxide Nanofibers for Photocatalytic CO2 Reduction.

High-entropy oxides (HEOs) exhibit great prospects owing to their varied composition, chemical adaptability, adjustable light-absorption ability, and strong stability. In this study, we report a strategy to synthesize a series of porous high-entropy spinel oxide (HESO) nanofibers (NFs) at a low temperature of 400 °C by a sol-gel electrospinning technique. The key lies in selecting six acetylacetonate salt precursors with similar coordination abilities, maintaining a high-entropy disordered state during the transformation from stable sols to gel NFs. The as-synthesized HESO NFs of (NiCuMnCoZnFe)3O4 show a high specific surface area of 66.48 m2/g, a diverse elemental composition, a dual bandgap, half-metallicity property, and abundant defects. The diverse elements provide various synergistic catalytic sites, and oxygen vacancies act as active sites for electron-hole separation, while the half-metallicity and dual-bandgap structure offer excellent light absorption ability, thus expanding its applicability to a wide range of photocatalytic processes. As a result, the HESO NFs can efficiently convert CO2 into CH4 and CO with high yields of 8.03 and 15.89 µmol g-1 h-1, respectively, without using photosensitizers or sacrificial agents.

Hofmeister Effect Promoted the Introduction of Tunable Large Mesopores in MOFs at Low Temperature for Femtomolar ALP Detection.

In addressing the demand for hierarchically mesoporous metal-organic frameworks (HMMOFs) with adjustable large mesopores, a method based on the synergistic effects of low-temperature microemulsions and Hofmeister ions is developed. Low temperature dramatically enhanced the solubility of hydrophobic solvent in the microemulsion core, enlarging the mesopores in HMMOFs replica. Meanwhile, Hofmeister salt-in ions continuously controlled mesopore expansion by modulating the permeability of swelling agent into the microemulsion core. The large mesopores up to 33 nm provided sufficient space for the alkaline phosphatase (ALP) enrichment, and retained the remaining channel to facilitate the free mass diffusion. Leveraging these advantages, a colorimetric sensor is successfully developed using large-mesopore HMMOFs for femtomolar ALP detection based on the enrichment and cycling amplification principles. The sensor exhibited a linear detection range of 100 to 7500 fm and a limit of detection of 42 fm, presenting over 4000 times higher sensitivity than classic para-nitrophenyl phosphate colorimetric methods. Such high sensitivity highlights the importance of adjustable mesoporous structures of HMMOFs in advanced sensing applications, and prefigures their potential for detecting large biomolecules in diagnostics and biomedical research.

Facile Low-Temperature synthesis of novel carbon nitrides for efficient conversion of carbon dioxide into Value-Added chemicals.

The interest in using carbon nitrides (CN) for CO2 conversion has stimulated extensive research on CN synthesis. Herein, we report the synthesis of two novel CN materials using low-cost commercially available precursors at low temperatures in a short duration of time. Two CN materials, one derived from 5-amino tetrazole (named 4NZ-CN) and the other derived from 3, 5-diamino-1, 2, 4-triazole (named 3NZ-CN) precursors, are prepared by refluxing these precursors for 2 h at 100 °C. 4NZ-CN and 3NZ-CN catalysts show higher surface areas (55.80 and 52.00 m2 g-1) and more basic sites (10.05 and 5.65 mmol g-1) than the conventional graphitic carbon nitride (g-C3N4) derived from melamine, for which the corresponding values are 9.20 m2 g-1 and 0.62 mmol g-1, respectively. In addition, both CN exhibit a 3-fold higher catalytic activity for CO2 cycloaddition to epoxides than g-C3N4. The structure-activity relationship was ascertained using a combination of experimental and computational studies, and a catalytic mechanism was proposed. This work provides a facile strategy for the synthesis of novel CN materials at relatively low temperatures, and the developed catalysts show remarkable performance in the conversion of CO2 to value-added chemicals.

Low-Temperature Synthesis of Cu-Doped Anatase TiO2 Nanostructures via Liquid Phase Deposition Method for Enhanced Photocatalysis.

Titanium dioxide (TiO2) photocatalysis can harness the energy from sunlight, providing a solution to many green- and energy-related problems. In this study, we aimed to produce Cu doped TiO2 (Cu-TiO2) structures at a low temperature (~70 °C) under atmospheric pressure based on liquid phase deposition. The products prepared with Cu nitrate exhibited anatase-phase TiO2 with the presence of Cu, and the particles showed a waxberry-like structure. Changing the Cu nitrate concentration allowed control of the atomic concentration; we confirmed ~1.3 atm.% of Cu ions in the product when we applied 10 mM in the precursor solution. By doping Cu, the light absorption edge shifted to 440 nm (~2.9 eV), and we proved the photocatalytic reaction through action spectral measurement. We observed the decomposition of acetaldehyde into CO2 on Cu-TiO2 photocatalysts, which produced optimized improvements in photocatalytic activity at Cu dopant levels between 0.2 and 0.4 atm.%. This study demonstrates that the liquid phase deposition technique can be used for doping metallic ions into TiO2, which shows promise for preparing novel and unique nanomaterials as visible light photocatalysts.

Ratiometric visualization of lysosomal pH fluctuations during autophagy by two-photon carbonized polymer dots-based probe.

Monitoring the pH variation in lysosomes is very conducive to studying the autophagy process, and fluorescent ratiometric pH nanoprobes with inherent lysosome targeting ability are highly desirable. Here, a carbonized polymer dots-based pH probe (oAB-CPDs) was developed by self-condensation of o-aminobenzaldehyde and further carbonization at low temperature. The obtained oAB-CPDs display improved performance in pH sensing, including robust photostability, intrinsic lysosome-targeting ability, self-referenced ratiometric response, desirable two-photon-sensitized fluorescence property, and high selectivity. With the suitable pKa value of 5.89, the as-prepared nanoprobe was successfully applied to monitor the variation of lysosomal pH in HeLa cells. Moreover, the occurrence that lysosomal pH decreased during both starvation-induced and rapamycin-induced autophagy was observed by using oAB-CPDs as fluorescence probe. We believe that nanoprobe oAB-CPDs can work as a useful tool for visualizing autophagy in living cells.

Influence of Additives and Growth Inhibitors in Improving the Physicochemical Properties of Silicoaluminophosphate Molecular Sieve, SAPO-11.

Silicoalumiophosphates (SAPOs) are microporous crystalline materials extensively utilized as adsorbents and catalysts. The present work utilized two strategies to synthesize nanocrystalline SAPO-11. The first strategy involves a surfactant as a mesoporogen to reduce the crystallite size and increase the surface area for the materials synthesized at 200 °C in 2 days. In the second strategy, the synthesis temperature and time were significantly reduced to 160 °C and 3 h using propylene oxide as a pH accelerator. The reduction in the particle size and the improvement in the surface area were achieved using propyltriethoxysilane, which inhibited the growth of SAPO-11 particles. The materials were thoroughly characterized using XRD, N2 -sorption, FTIR, pyridine-adsorbed FTIR, electron microscopy, XPS, and NMR. The surfactant-assisted synthesis formed a nanorod morphology with a large external and BET surface area. The low-temperature synthesis involving silane as a growth inhibitor and propylene oxide as a pH modulator demonstrated a rectangular nanoplatelet morphology with a large surface area. The synthesis was scaled up to 10 g with no change in the experimental parameters. A synthesis strategy facilitating nuclei formation and retarding the growth of particle size will attract academia and industrial researchers to utilize these strategies for the manufacturing of zeolites of different frameworks on a large scale.

Low-Temperature Sintering of a Garnet-Type Li6.5La3Zr1.5Ta0.5O12 Solid Electrolyte and an All-Solid-State Lithium-Ion Battery.

Garnet-type Ta-substituted Li7La3Zr2O12 materials attract considerable attention as solid electrolytes for use in future oxide-based all-solid-state lithium-ion batteries owing to their superior ionic conductivity and chemical and electrochemical stabilities. However, high-temperature sintering above 1000 °C, which is needed to realize high lithium-ion conductivity, results in the formation of insulating interface impurities at the electrode-electrolyte interface. Herein, the low-temperature sintering of the Li6.5La3Zr1.5Ta0.5O12 (LLZT) solid electrolyte at a remarkably low temperature of 400 °C was demonstrated using the submicrometer-sized garnet-type LLZT fine powder sample prepared at 600 °C through a reaction of Li2O and La2.4Zr1.2Ta0.4O7. The lithium-ion conductivity at 25 °C was 4.54 × 10-5 S cm-1 without any additives through low-temperature sintering at 400 °C. In addition, the preliminary battery performance of the oxide-based all-solid-state LiNi1/3Co1/3Mn1/3O2-Li4Ti5O12 full-battery cell fabricated at 400 °C using the present LLZT fine powder sample as the solid electrolyte was demonstrated.

Preparation and Characterization of Novel 5Mg(OH)2·MgSO4·7H2O Whiskers.

Herein, novel monodisperse basic magnesium sulfate whiskers (5Mg(OH)2·MgSO4·7H2O) were prepared under low-temperature and atmospheric-pressure conditions, using the admixture sodium citrate. X-ray diffraction, Raman spectroscopy, scanning electron microscopy, energy-dispersive spectroscopy, transmission electron microscopy, selected area electron diffraction, thermogravimetric analysis, Fourier-transform infrared spectroscopy, and X-ray photoelectron spectroscopy were used to characterize the structure and morphology of the whisker products. The analysis results showed that the product was composed of high-purity basic magnesium sulfate whiskers. The lengths and diameters of the whiskers were 10-20 µm and 0.1-0.2 µm, respectively, and their aspect ratios were higher than 30. The formation mechanism of 5Mg(OH)2·MgSO4·7H2O involved direct assembly from the precursors without the formation of magnesium hydroxide for redissolution. High-purity MgO whiskers with smooth surfaces were prepared using the as-prepared whisker products via thermal decomposition. Thus, the findings of this study can provide technical support for the cost-effective industrial-scale preparation of basic magnesium-sulfate whiskers and associated whisker products.

Flexible Thermoelectric Generator Based on Polycrystalline SiGe Thin Films.

Flexible and reliable thermoelectric generators (TEGs) will be essential for future energy harvesting sensors. In this study, we synthesized p- and n-type SiGe layers on a high heat-resistant polyimide film using metal-induced layer exchange (LE) and demonstrated TEG operation. Despite the low process temperature (<500 °C), the polycrystalline SiGe layers showed high power factors of 560 µW m-1 K-2 for p-type Si0.4Ge0.6 and 390 µW m-1 K-2 for n-type Si0.85Ge0.15, owing to self-organized doping in LE. Furthermore, the power factors indicated stable behavior with changing measurement temperature, an advantage of SiGe as an inorganic material. An in-plane π-type TEG based on these SiGe layers showed an output power of 0.45 µW cm-2 at near room temperature for a 30 K temperature gradient. This achievement will enable the development of environmentally friendly and highly reliable flexible TEGs for operating micro-energy devices in the future Internet of Things.

Low temperature energy- efficient synthesis methods for bismuth-based nanostructured photocatalysts for environmental remediation application: A review.

Bismuth-based composite materials have unique structural, chemical, optical, and electrical properties that are highly beneficial in Photocatalysis. The layered structure and tunable bandgap properties of the Bismuth-based composites are advantageous for the absorption of solar light efficiently. Also, these properties help the separation and recombination of photogenerated charge carriers, leading to enhancement in the photocatalytic activity. Synthesis of the catalyst at a lower temperature to produce catalyst reduces the production cost and electrical energy consumption. This review provides an overview of the recent development in Bismuth-based composite nanostructured photocatalytic materials, mainly using low-temperature driven synthesis methods. Herein, we have mainly summarized the primarily used low temperature-based synthetic routes, particularly in the temperature range of 50-300 °C for synthesizing Bismuth-based composite materials. In addition to this, the photocatalytic mechanism, the textural, structural, electronic, and photocatalytic properties of the synthesized photocatalysts are discussed. The literature shows that the surface area of the composite Bismuth-based photocatalytic materials synthesized using the low-temperature synthetic route is in the range of 1.5-81 m2/g and can be activated by solar, ultraviolet, and Light Emitting Diode (LEDs) light irradiation based on the synthetic route. Their photocatalytic performance and structural stability are excellent and utilized for several runs. The comprehensive understanding of the low-temperature synthesis of Bismuth-based composite materials for visible light-activated photocatalytic applications provided will be useful for developing photocatalytic materials on an industrial scale due to energy-efficient synthetic routes. Furthermore, the prospects of low temperature-driven Bismuth-based composite synthesis routes are discussed.