Influence Of Synthesis Conditions Research Articles

Study on the Continuous Whole Process Preparation of Peptizable Pseudoboehmite by High Gravity Strengthening Reaction of CO2 and Heat Transfer.

The preparation of highly peptizable pseudoboehmite faces challenges such as slow reaction rate, prolonged aging times leading to poor peptization performance, and difficulty in achieving continuous production. In this study, a novel approach was proposed involving a high gravity reactor to enhance carbonation reaction control for pseudoboehmite nucleation, a high gravity steam heating process, and a continuous aging process in pipelines. By coupling these three processes, the continuous whole process production of highly peptizable pseudoboehmite under high gravity conditions was achieved. First, the effect of high gravity reactor enhancement on the reaction and the resulting solid phase was investigated. Second, the impact of aging temperature and time on the solid phase formed at different reaction end points was studied using high gravity and steam heating of the liquid phase. Furthermore, the influence of synthesis conditions on the peptization performance of pseudoboehmite was extensively examined. Finally, the nucleation and growth mechanisms of pseudoboehmite under high gravity conditions were analyzed. It was found that increasing high gravity factor, CO2 gas flow rate, and CO2 content accelerated carbonation reaction rate, promoting pseudoboehmite crystal nucleation. Increasing aging temperature and time facilitated the growth of pseudoboehmite nuclei and improved peptization performance. The high gravity device altered the gas-liquid phase contact state of traditional kettle-type equipment, reducing the reaction time and heating time from minutes to seconds, thus achieving the continuous whole process production of pseudoboehmite with a peptization index of 100% from sodium aluminate solution by kiln flue gas.

Size-controlled synthesis of cobalt phosphide (Co2P) nanoparticles and their application in non-enzymatic glucose sensors via a carbon fiber/Co2P composite

In this study, we synthesized Co2P nanoparticles using a solid-state phosphorization method and evaluated the electrocatalytic response to glucose oxidation reaction (GORs). The influence of synthesis conditions on the particle size, morphology of Co2P species and formation of byproducts is discussed. A lower molar ratio of the phosphorus precursor leads to a decrease in the generation of byproducts. In addition, the calcination temperature and time greatly influence the purity level of the Co2P species and its particle size. Thus, we obtained three pure Co2P nanoparticles with different sizes and morphologies. Significant differences in their electrocatalytic activity against the GOR are observed depending on the size of the particles, being the smaller ones the most efficient. Based on Tafel analysis, a higher catalytic activity was observed for the carbon fibre (CF)/Co2P composite compared to Co2P, which presented a greater onset potential and low response in current density. Tafel slopes close to 120 mV/dec were obtained for both materials, indicating that the mechanism is independent of the type of Co2P-based material used. Finally, the performance of the GCE/CF/Co2P sensor was demonstrated by amperometric measurements, with a sensitivity of 409 µAmM-1cm-2, a linear range between 39.4 µM and 150 µM, and a detection limit of 0.97 µM, analytical characteristics better than those obtained for other cobalt phosphide-based sensors reported in the literature. In addition, the GCE/CF/Co2P sensor shows excellent selectivity and demonstrated to be competitive compared to other Co-based non-enzymatic glucose sensors.

Influence of Synthesis Conditions on Catalytic Performance of Ni/CeO2 in Aqueous-Phase Hydrogenolysis of Glycerol without External Hydrogen Input.

The aqueous-phase hydrogenolysis of glycerol was studied in Ni/CeO2 catalytic systems prepared by incipient wetness impregnation. The operating conditions were 34 bar, 227 ºC, 5 wt.% of glycerol, and a W/mglycerol = 20 g catalyst min/g glycerol without a hydrogen supply. The effect of the catalyst preparation conditions on the catalytic activity and physicochemical properties of the catalysts was assessed, particularly the calcination temperature of the support, the calcination temperature of the catalyst, and the Ni content. The physicochemical properties of the catalysts were determined by N2 adsorption, H2-TPR, NH3-TPD, and XRD, among other techniques. A relevant increase in acidity was observed when increasing the nickel content up to 20 wt.%. The increase in the calcination temperatures of the supports and catalysts showed a detrimental effect on the specific surface area and acid properties of the catalysts, which were crucial to the selectivity of the reaction. These catalysts notably enhanced the yield of liquid products, achieving global glycerol conversion values ranging from 17.1 to 29.0% and carbon yield to liquids ranging from 12.6 to 24.0%. Acetol and 1,2-propanediol were the most abundant products obtained in the liquid stream.

Modification of Silica with Sucrose and Ammonium Fluoride Agents: A Facile Route to Prepare Supports of Iridium Catalysts for Hydrogenation Reaction.

Mesoporous silica materials were synthesized using inexpensive and environmentally friendly sucrose as a porogeneous agent. It was found that the presence of sucrose and the products of its chemical transformation during synthesis (e.g., furfural polymer) significantly affected the structure of the obtained porous silica. The influence of synthesis conditions (pH, temperature, time) on the textural properties of the final materials was determined. Samples obtained in an acidic medium, at pH = 1, and treated at room temperature, yielded products with a large surface area and a narrow pore size distribution in the range of 2-5 nm, while the synthesis at pH = 8 allowed for the formation of mesoporous systems with pores in the range of 14-20 nm. To generate acidity, the silicas were modified with an ammonium fluoride solution and then used as supports for iridium catalysts in a hydrogenation reaction, with toluene as a model hydrocarbon. The influence of parameters such as specific surface area, support acidity, and iridium dispersion on catalytic activity was determined. It was shown that modification with sucrose improved the porous structure, and NH4F modification generated acidity. These parameters favored better reducibility and dispersion of the active phase, resulting in higher activity of the catalysts in the studied hydrogenation reaction.

Pure TeO2 glass: Influence of synthesis conditions on linear and non-linear optical, magneto-optical and structural properties

The first systematic study of linear and non-linear optical, magneto-optical and structural properties of pure TeO2 glass is presented with regard to different synthesis and material processing conditions. Prepared glasses were synthesized by the intermittent quenching from 900 ∘C in platinum or alumina crucibles and characterized prior to and after optical polishing. The position of the long-wavelength/phonon absorption edge was investigated using various optical models and experimentally obtained data of refractive index and Verdet constants were used for the estimation of magneto-optical anomaly parameter. During synthesis in alumina crucible, up to about 11 wt.% of Al2O3 incorporates into the glass (verified by EDS/XRF and Raman/FTIR spectroscopy) partially transforming the original pure TeO2 glass backbone structure composed of [TeO4] trigonal bipyramids to [TeO3+1] and [TeO3] structural units with the expected integration of Al into Te−O−Al bridges. The presence of Al2O3 results in lowered density ρ (5.60 → 4.72 g cm−3), refractive index n1550 (2.086 → 1.927) and Verdet constant V632 (36.3 → 21.9 rad T−1 m−1) and in increased optical-band-gap energy Eg (3.69 → 3.72 eV) and Abbe number νD (19.9 → 26.9) compared to pure TeO2 glass prepared in platinum crucible. A dataset of the obtained complex optical parameters (refractive index and extinction coefficient) in the wide spectral range of 193 − 11000 nm is included in the supplementary part.

Absorption edge shift and broadening in nanostructured Al doped ZnO thin films

Samples of ZnO were prepared by sol-gel and deposited by dip-coating. The influence of synthesis conditions on the optical properties were studied in different sets of ZnO films, synthesized by alternately varying the following parameters: addition of additives to the precursor solution, Al doping percentage and number of layers. The optical properties of the obtained films were studied by transmittance, being typically >90 % at 600 nm. The absorption edge for undoped samples showed a structure due to exciton formation at room temperature. The bandgap energy Eg, was between (3.227 ± 0.010) eV and (3.275 ± 0.010) eV for undoped samples, increasing to (3.352 ± 0.010) eV for Al doped ones (10 % Al/Zn in solution with additives). For intermediate 5 % doping the mean bandgap energy was (3.315 ± 0.015) eV. A similar value (3.320 eV ± 0.010) eV was obtained for 10 % Al/Zn when no additives were included. Doped samples showed a smoother absorption edge. This edge shape evolution was studied by Urbach band tail analysis. The Urbach band tail parameter EU increased with doping, varying from 30 meV to 90 meV and increasing as Eg increases. This correlation describes the influence of impurity states in the structure and optical properties of the material.

Influence of Synthesis Conditions on the Structural, Optical, and Electrophysical Properties of TiO2/CuxO Nanocomposites

Influence of Synthesis Conditions on the Structural, Optical, and Electrophysical Properties of TiO2/CuxO Nanocomposites

Influence of Synthesis Conditions on Chabazite Zeolite Crystallization in LiOH Solution

Influence of Synthesis Conditions on Chabazite Zeolite Crystallization in LiOH Solution

Synthesis of L-Lactide from Lactic Acid and Production of PLA Pellets: Full-Cycle Laboratory-Scale Technology.

Lactide is one of the most popular and promising monomers for the synthesis of biocompatible and biodegradable polylactide and its copolymers. The goal of this work was to carry out a full cycle of polylactide production from lactic acid. Process conditions and ratios of reagents were optimized, and the key properties of the synthesized polymers were investigated. The influence of synthesis conditions and the molecular weight of lactic acid oligomers on the yield of lactide was studied. Lactide polymerization was first carried out in a 500 mL flask and then scaled up and carried out in a 2000 mL laboratory reactor setup with a combined extruder. Initially, the lactic acid solution was concentrated to remove free water; then, the oligomerization and synthesis of lactide were carried out in one flask in the presence of various concentrations of tin octoate catalyst at temperatures from 150 to 210 °C. The yield of lactide was 67-69%. The resulting raw lactide was purified by recrystallization in solvents. The yield of lactide after recrystallization in butyl acetate (selected as the optimal solvent for laboratory purification) was 41.4%. Further, the polymerization of lactide was carried out in a reactor unit at a tin octoate catalyst concentration of 500 ppm. Conversion was 95%; Mw = 228 kDa; and PDI = 1.94. The resulting products were studied by differential scanning calorimetry, NMR spectroscopy and gel permeation chromatography. The resulting polylactide in the form of pellets was obtained using an extruder and a pelletizer.

Influence of Synthesis Conditions on the Physical Characteristics and Antibacterial activities of Cerium Oxide Nanoparticles in Biomedical Applications

Influence of Synthesis Conditions on the Physical Characteristics and Antibacterial activities of Cerium Oxide Nanoparticles in Biomedical Applications

Influence of Synthesis Conditions on the Performance of Palladium–Copper Ethanol-to-Butanol Conversion Catalysts

The influence of the synthesis conditions on the performance of Pd–Cu ethanol-to-butanol conversion catalysts was studied. The optimum conditions for forming the most active system 0.2%Cu/0.3%Pd/Al2O3 are as follows: sample synthesis by Al2O3 impregnation from aqueous solutions of Pd and Cu nitrates; deposition of the metal precursors in succession; total content of Pd and Cu in the sample 0.5 wt %; Pd : Сu molar ratio 1 : 1; catalyst reduction temperature 200○С. As shown by TEM, XPS, TPD-NH3, TPR-H2, XRD, and N2 adsorption, the surface of the most active catalyst contains Pd0Cu0 particles with the mean size of 4 ± 2 nm. The bimetallic particles are an alloy with the fcc structure and Pd : Cu ratio of 40 : 60. At 275○C, the performance of 0.2%Cu/0.3%Pd/Al2O3 is 182 × 10–4 mol h–1 g–1. The value obtained is higher by several orders of magnitude than the performance of the reference catalysts M1/Al2O3 (M1 = Fe, Ni, Co) and by an order of magnitude than that of the reference catalysts M2/Al2O3 (M2 = Ru, Rh, Pt, Pd, Pt–Re, Ni–Mo).

Magnetic Chitosan Bionanocomposite Films as a Versatile Platform for Biomedical Hyperthermia.

Responsive magnetic nanomaterials offer significant advantages for innovative therapies, for instance, in cancer treatments that exploit on-demand delivery on alternating magnetic field (AMF) stimulus. In this work, biocompatible magnetic bionanocomposite films are fabricated from chitosan by film casting with incorporation of magnetite nanoparticles (MNPs) produced by facile one pot synthesis. The influence of synthesis conditions and MNP concentration on the films' heating efficiency and heat dissipation are evaluated through spatio-temporal mapping of the surface temperature changes by video-thermography. The cast films have a thickness below 100µm, and upon exposure to AMF (663kHz, 12.8 kA m-1), induce exceptionally strong heating, reaching a maximum temperature increase of 82 °C within 270 s irradiation. Further, it is demonstrated that the films can serve as substrates that supply heat for multiple hyperthermia scenarios, including: i) non-contact automated heating of cell culture medium, ii) heating of gelatine-based hydrogels of different shapes, and iii) killing of cancerous melanoma cells. The films are versatile components for non-contact stimulus with translational potential in multiple biomedical applications.

Catalytic Oxidation of CO over LaNi1/3Sb5/3O6 Synthesized by Different Methods

Methods for the synthesis of LaNi1/3Sb5/3O6 with a rosiaite structure have been developed using citrate method and coprecipitation followed by annealing. The influence of synthesis conditions on the morphology of the samples has been demonstrated. A comparative analysis of the catalytic properties of LaNi1/3Sb5/3O6 synthesized by various methods, in the reaction of CO oxidation has been carried out. The catalyst synthesized by the citrate method demonstrated the greatest efficiency and stability (the temperature of 90% CO conversion was T90 = 336°C). The LaNi1/3Sb5/3O6 surface was studied before and after catalysis by in situ diffuse reflectance IR spectroscopy, X-ray photoelectron spectroscopy, and temperature-programmed O2 desorption. It has been shown that the catalytic oxidation of CO on the LaNi1/3Sb5/3O6 surface proceeds according to the Mars–van Krevelen mechanism and is accompanied by redox Sb3+ ↔ Sb5+ processes. It has been established that no contamination of the sample surface occurs during the catalysis process.

Hierarchically Organized MoS2 Films as Promising Electrodes for Flexible Supercapacitors

The formation of hierarchically organized MoS2 films on various substrates by a hydrothermal method was studied. The influence of synthesis conditions and the substrate (a glass or a flexible carbon paper substrate) on the crystal structure of sulfide films was determined using X-ray powder diffraction (XRD). Scanning electron microscopy (SEM) showed that the films on glass substrates comprised structurally different elements, namely a continuous dense layer of spherical nanoparticles on the surface of which hierarchically organized globular agglomerates of two types are arranged. A molybdenum disulfide shell about 1.5 μm thick, consisting of hierarchically organized nanosheets less than 10 nm thick, was formed on the surface of carbon fibers that make up the carbon paper. Elemental mapping was used to evaluate the homogeneity of the MoS2 film formed on the carbon paper. Atomic force microscopy (AFM) showed that an individual carbon fiber modified with a sulfide film had a mean square roughness of about 13 nm (over an area of about 100 μm2). According to Kelvin-probe force microscopy (KPFM) data, the electron work function of the material was 4.53 eV. The electrochemical characteristics of the manufactured flexible electrode based on a hierarchically organized molybdenum disulfide film were investigated. The specific capacitance and the stability of functional and microstructural properties of the manufactured supercapacitor electrode in 2000 charge–discharge cycles were evaluated. Thus, the proposed strategy is promising for the fabrication of efficient hierarchically organized MoS2 electrodes for flexible supercapacitors.

Sludge-derived biochar: A review on the influence of synthesis conditions on environmental risk reduction and removal mechanism of wastewater pollutants

Sludge-derived biochar: A review on the influence of synthesis conditions on environmental risk reduction and removal mechanism of wastewater pollutants

Effects of synthesis conditions on the crystal and local structures of high-entropy oxides Ln[formula omitted]O[formula omitted] (Ln = La-Yb, Y; M = Ti, Zr, Ce)

The synthesis and detailed study of six series of high-entropy complex oxides containing lanthanides (Ln) and transition metals with the general formula Ln2M2O7 (Ln = La-Yb, and Y; M = Ti, Zr, and Ce) with the number of different Ln cations not less than six in each case are reported. The influence of synthesis conditions (types of the Ln3+ and M4+ cations, calcination temperature) used in the synthesis via either coprecipitation or sol–gel method on the crystal and local structures of target materials is comprehensively surveyed. The studies were carried out using a combination of long- (s-XRD), medium- (Raman, FT-IR, SEM-EDS) and short-range (XAFS) sensitive techniques, as well as AES-ICP and STA. It was established that the ratio of the cation radii γ = r̄Ln3+/r̄M4+ is the main factor that determines the type of initially formed crystal structure. In the boundary region (γ∼ 1.42–1.47), the average radius of lanthanide cation (r̄Ln3+), along with the r̄Ln3+/r̄M4+ ratio, also plays a significant role in the type of the resulting crystal structure of the high-entropy lanthanide complex oxides. The presence of inhomogeneity in the distribution of elements in precursors significantly affects the phase composition of the resulting high-entropy oxides. An increase in the calcination temperature promotes not only the occurrence of subsequent phase transitions, but also an increase in the single-phase nature of the resulting high-entropy complex rare-earth oxides. At the same time, the cations included in the composition retain some independence, despite the fact that they occupy one crystallographic position in the resulting crystal structure.

Influence of Synthesis Conditions on the Crystal, Local Atomic, Electronic Structure, and Catalytic Properties of (Pr1−xYbx)2Zr2O7 (0 ≤ x ≤ 1) Powders

The influence of Yb3+ cations substitution for Pr3+ on the structure and catalytic activity of (Pr1−xYbx)2Zr2O7 powders synthesized via coprecipitation followed by calcination is studied using a combination of long- (s-XRD), medium- (Raman, FT-IR, and SEM-EDS) and short-range (XAFS) sensitive methods, as well as adsorption and catalytic techniques. It is established that chemical composition and calcination temperature are the two major factors that govern the phase composition, crystallographic, and local-structure parameters of these polycrystalline materials. The crystallographic and local-structure parameters of (Pr1−xYbx)2Zr2O7 samples prepared at 1400 °C/3 h demonstrate a tight correlation with their catalytic activity towards propane cracking. The progressive replacement of Pr3+ with Yb3+ cations gives rise to an increase in the catalytic activity. A mechanism of the catalytic cracking of propane is proposed, which considers the geometrical match between the metal–oxygen (Pr–O, Yb–O, and Zr–O) bond lengths within the active sites and the size of adsorbed propane molecule to be the decisive factor governing the reaction route.

Influence of Synthesis Conditions on the Performance of Palladium–Copper Ethanol-to-Butanol Conversion Catalysts

Influence of Synthesis Conditions on the Performance of Palladium–Copper Ethanol-to-Butanol Conversion Catalysts

Effects of Processing Conditions on the Properties of Monoammonium Phosphate Microcapsules with Melamine-Formaldehyde Resin Shell.

To develop monoammonium phosphate (MAP) as a novel acid source for durable intumescent fire retardants (IFR), MAP microcapsules (MCMAPs) containing MAP as the internal core and melamine-formaldehyde (MF) as the external shell were prepared by in situ polymerization in this study. The influences of synthesis conditions (including reaction temperature, polymerization time, and reaction pH value) on the properties of obtained MCMAPs (MAP content, yield, morphologies, and thermal properties) were then investigated systematically. The morphologies, chemical structures, and thermal properties were characterized by optical microscopy, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Fourier transform infrared (FTIR) spectroscopy, and thermogravimetry analyzer (TGA). The results show that MAP was well encapsulated by MF resin. No microcapsules are obtained at <55 °C or with polymerization times <1 h. Optimal preparation conditions of reaction temperature, polymerization time, and reaction pH value are 75 °C, 3 h, and 5.5, respectively. Those results provide process reference and theoretical basis for preparing MCMAPs and could promote the application of MAP microcapsules in wood flame-retardant materials.

FORMATION OF CRYSTALLINE SiC IN NEAR-SURFACE SILICON LAYERS BY METHOD OF COORDINATED SUBSTITUTION OF ATOMS

In this work, monocrystalline films of silicon carbide were synthesized on the surface of a Si(100) silicon wafer using the method of coordinated substitution of atoms. The films were synthesized at temperatures of 1200 °C and 1300 °C for 20 minutes in a CO gas flow at a pressure of 0.8 Pa. The effect of 1200–1300 °C temperatures on the formation of single- and polycrystalline layers, as well as nanostructured SiC phases in the near-surface region of silicon by the method of atom substitution, is analyzed. The formation of a high-quality crystalline silicon carbide film and the influence of synthesis conditions on the total volume of SiC structural phases, microstructure and nanostructure of the surface are shown. It was found that an increase in temperature from 1200 °C to 1300 °C led to a more intensive formation of silicon carbide and an increase in the number of Si–C bonds by 1.9 times due to an increase in the thickness of the synthesized silicon carbide layer. There is an increase in the proportion of the crystalline phase due to a more intense transformation of the nuclei of nanocrystals into micro- and nanocrystals. Intense processes of penetration of carbon atoms deep into silicon at a temperature of 1300 °C with amorphization of its structure and the formation of Si-C, which can transform into crystalline phases at temperatures above 1300 °C, are assumed. The proportion of the SiC crystalline phase increases to 50.2% of the film volume due to the intensive transformation of nanocrystal nuclei into micro- and nanocrystals. It has been experimentally shown that the formation of various SiC structures on Si (100) occurs in full accordance with the main principles of the method of coordinated substitution of atoms.