SEM Mapping Research Articles

Effect of cellulase-assisted cold isostatic pressure extraction on the characteristics and functional properties of polyphenol extracts from camellia sinensis seeds

In this experiment, polyphenolic substances were extracted from Camellia sinensis seeds (CSS) using a synergistic treatment of cold isostatic pressure (CIP) and cellulase. The effects of pressure, treatment time, and cellulase addition on the experiment were investigated. And the optimal extraction conditions were established by single factor experiment and Box-benhken experiments: the pressure applied by CIP was 408.649 MPa, the treatment time was 10.995 min, and the cellulase addition was 4.098 %. The polyphenols in the extract were characterized and quantified using LC-MS/MS. By comparing the different treatments, it was found that the synergistic treatment of CIP and cellulase resulted in a higher extraction yield. FTIR, XRD and SEM mapping showed that CIP synergistic pretreatment with cellulase was able to disrupt the microstructure of the plant and promote the influx of the active ingredients into solution. Finally, the activity of the extracts was detected by using in vitro antioxidant experiments and RAW264.7 cellular anti-inflammatory experiments, which indicated that CIP and cellulase synergistically treated polyphenol extracts had high antioxidant and anti-inflammatory capacity. This experiment provides a new pretreatment method for extracting active substances from CSS.

Photocatalytic activity of molybdenum-doped LOS- zeolite for efficient dye degradation and hydrogen production

This research investigates the synthesis and application of Losod-zeolite (LOS-Z), a crystalline hydrated sodium aluminosilicate (Na12Al12Si12O48.xH2O) as a potential photocatalyst for dye degradation and H2 production from dye-degraded water. The photocatalytic properties are enhanced by impregnating molybdenum (Mo) into LOS-Z (Mo@LOS-Z). XRD, FTIR, SEM, EDX, and elemental mapping were used to study the physicochemical properties of synthesized materials while UV–vis and PL were employed to explore the optoelectronic properties. The photocatalytic activities for dye degradation and H2 production were evaluated using methylene blue (MB) under visible light irradiation. An enhancement in the efficiency of dye degradation (56%–82%) and H2 production rate was demonstrated due to the competitive photocatalytic performance of 10% Mo@LOS-Z compared to the pristine LOS-Z and CFA-BFA blend. It exhibited 2.5 times higher (∼1200 μmol g−1h−1) H2 production than the LOS-Z (∼480 μmol g−1h−1) due to the synergistic effects of narrowed band gap and recombination rate. This study could pave the way forward into the synthesis of waste-derived photocatalysts for efficient dye degradation and H2 production.

Folic acid-conjugated bovine serum albumin-coated selenium-ZIF-8 core/shell nanoparticles for dual target-specific drug delivery in breast cancer.

Methotrexate (MTX), a frequently used chemotherapeutic agent, has limited water solubility, leading to rapid clearance even in local injections. In the present study, we developed folic acid-conjugated BSA-stabilized selenium-ZIF-8 core/shell nanoparticles for targeted delivery of MTX to combat breast cancer. FT-IR, XRD, SEM, TEM, and elemental mapping analysis confirmed the successful formation of FA-BSA@MTX@Se@ZIF-8. The developed nano-DDS had a mean diameter, polydispersity index, and zeta potential of 254.8nm, 0.17, and - 16.5 mV, respectively. The release behavior of MTX from the nanocarriers was pH-dependent, where the cumulative release percentage at pH 5.4 was higher than at pH 7.4. BSA significantly improved the blood compatibility of nanoparticles so that after modifying their surface with BSA, the percentage of hemolysis decreased from 12.67 to 5.12%. The loading of methotrexate in BSA@Se@ZIF-8 nanoparticles reduced its IC50 on 4T1 cells from 40.29µg/mL to 16.54µg/mL, and by conjugating folic acid on the surface, this value even decreased to 12.27µg/mL. In vivo evaluation of the inhibitory effect in tumor-bearing mice showed that FA-BSA@MTX@Se@ZIF-8 caused a 2.8-fold reduction in tumor volume compared to the free MTX, which is due to the anticancer effect of selenium nanoparticles, the pH sensitivity of ZIF-8, and the presence of folic acid on the surface as a targeting agent. More importantly, histological studies and animal body weight monitoring confirmed that developed nano-DDS does not have significant organ toxicity. Taking together, the incorporation of chemotherapeutics in folic acid-conjugated BSA-stabilized selenium-ZIF-8 nanoparticles may hold a significant impact in the field of future tumor management.

Влияние технологических параметров на микроструктуру и свойства сплава AlSiMg, полученного методом селективного лазерного плавления

Introduction. The development of additive technologies is aimed at the synthesis of new powder compositions for selective laser melting plants, the study of the effect of mode parameters on the stable quality of products. The purpose of this work is to study the effect of the scanning strategy on the microstructure, elemental composition, porosity and density of specimens obtained by selective laser melting from non-spherical powders (Al — 91 wt. %, Si — 8 wt. %, Mg — 1 wt. %), subjected to special preparation to determine the optimal conditions for selective laser melting. The research methods are methods of X-ray diffraction and X-ray phase analysis, transmission electron microscopy. The paper examines specimens formed using four different scanning strategies. Results and discussions. A promising aluminum alloy AlSi8Mg is developed for selective laser melting. The material has good manufacturability and low powder cost. The technological parameters of melting make it possible to form a thin structure with a low level of porosity. The mechanism of influence of the scanning strategy on porosity, surface morphology, relative density and microstructure is investigated. A specimen from the AlSi8Mg powder composition with a high relative density of 99.97 % is produced by selective laser melting with an energy density of 200 J/mm3, a specimen scanning circuit when the direction of laser movement changes by an angle of 90° each odd layer. It is proved that the density of the AlSiMg alloy depends on the scanning strategy used. The calculated density of the specimen was 2.5 g/cm3, which corresponds to the density of silumin. Analysis of SEM images and maps of the distribution of elements (Al, Mg, Si) of the specimens showed that different specimen formation strategies do not affect the nature of silicon distribution. A unique grain structure is observed in the resulting AlSi8Mg alloy. The melt pool consists of small grains along the border and large grains in the center. The formation of fine grains is explained by the addition of Si and the high cooling rate during selective laser melting.

Fabrication of graphene field effect transistors on complex non-planar surfaces

Graphene field effect transistors (GFETs) are promising devices for biochemical sensing. Integrating GFETs onto complex non-planar surfaces could uncap their potential in emerging areas of wearable electronics, such as smart contact lenses and microneedle sensing. However, the fabrication of GFETs on non-planar surfaces is challenging using conventional lithography approaches. Here, we develop a combined spray-coating and photolithography setup for the scalable fabrication of GFETs on non-planar surfaces and demonstrate their application as integrated GFETs on microneedles. We optimize the setup to pattern ∼ 67 μm long GFET channels across the microneedle tips. Graphene is deposited between photo-patterned electrodes by spray-coating a liquid-phase exfoliated graphene ink while monitoring the channel resistance to achieve the required conductivity. The formation of the GFET channels is confirmed by SEM and EDX mapping, and the GFETs are shown to modulate in solution. This demonstrates an approach for manufacturing graphene electronic devices on complex non-planar surfaces like microneedles and opens possibilities for wearable GFET microneedle sensors for real-time monitoring of biomarkers.

Electrodeposited Pt nanoparticles loaded on support composites of metal-organic frameworks and carbon quantum dots for the enhancement of alcohol electrooxidation

Metal-organic frameworks comprising divalent metal (M)-linked 4,4′-bipyridine (bpy), {[CuII4(bpy)3(OH)2(mal)3]·4H2O}n(Cubpy) and Ni2(bpy)3(NO3)4(H2O)4(Nibpy) were modified with carbon quantum dots (Mbpy/CQD; M = Cu, Ni) to prepare a composite support. Then, platinum (Pt) nanoparticles were electrodeposited onto the modified Mbpy/CQD support for the preparation of Pt-based catalysts (Pt/Mbpy/CQD) for the electrocatalytic improvement of alcohol oxidation. The influence of Mbpy with electrodeposited Pt nanostructures on CQD support electrodes is particularly discussed in detail through numerous physical characterizations, e.g., SEM, TEM, EDX, XPS, XRD, and elemental mapping. Dispersed Pt nanoparticles with diameters of 3-10 nm can be obtained on the modified Mbpy/CQD supports with suitable chemical and structural conditions for electrocatalytic oxidation improvement. The various prepared Pt/Mbpy/CQD catalysts with different compositions also enhance the kinetics of alcohol oxidation; they have a greater electrochemically active surface area (ECSA) and more development activity for alcohol oxidation than do the Pt/CQD catalysts. For the oxidation of all the selected small alcohol molecules, e.g., methanol, ethanol and isopropanol, the Pt/Cubpy/CQD catalyst composites also mostly exhibited improved catalytic activity, outstanding stability, and lower onset potential (Eonset) and CO tolerance. The favorable performance of the prepared composite catalysts is attributed to their superior ECSA owing to the suitable mixed surface of metal and functional groups of electrodeposited Pt, Mbpy, and CQD on the catalytic composites. Consequently, these as-prepared Pt/Mbpy/CQD composites, which are promising oxidative heterogeneous catalysts, can be used as active and stable catalysts for alcohol oxidation in alkaline solutions.

Sodium-doped LiFe0.5Mn0.5PO4 using sodium gluconate as both reducing agent and a doping source in Lithium-ion batteries

LiFexMn1-xPO4 (LFMP) cathode materials faces developmental challenges because Fe2+ and Mn2+ ions are prone to oxidation during the synthesis process and exhibit low electronic and ionic conductivities. We propose employing a multifunctional sodium gluconate that simultaneously acts as a reducing agent and dopant. XPS analysis shows an increased ratio of Fe2+ and Mn2+ ions within LFMP following the introduction of the reducing agent. Rietveld refinement indicates an expanded b-axis lattice space at an appropriate amount of Na-doped LFMP/C, which results in enhancement the Li+ diffusivity. SEM and TEM-EDS mapping confirm the morphology and elemental distribution of the LFMP materials. Electrochemical properties show the introduction of sodium gluconate enhanced the electrochemical properties of LFMP materials. This result demonstrates that the reducing agent prevents oxidation of transition metals during synthesis and Na doping significantly increases the Li+ diffusion coefficient. The Li0.97Na0.03Fe0.5Mn0.5PO4/C sample, when combined with a reducing agent, exhibits an outstanding rate performance of 122.6 mAh/g at 1C, 113.4 mAh/g at 5C, and 85.1 mAh/g at 20C. The enhancements in both electronic and ionic conductivities of LFMP cathodes are mainly ascribed to the incorporation of a reducing agent and Na doping.

Mechanical and absorption properties of carbon-basalt and glass fiber reinforced composites: A comprehensive study with implications for advanced manufacturing technology

In this research, a combination of hybrid and non-hybrid composite materials were tested for their mechanical properties and water absorption rates. The study focused on composites produced through hand-layup techniques, examining their void percentage, morphology, and elemental composition. Specifically, three different stacking sequences of hybrid composites were compared with three non-hybrid composites of equal thickness. Combining carbon and glass allows the composites to balance flexural (367 MPa, 23 GPa) and tensile (440 MPa, 5.7 GPa) strength and modulus, all while remaining cost-effective and easily accessible. The glass fiber-based composites exhibited exceptional impact (27 J/cm2) strength due to their interfacial solid bonding. Additionally, the study found that basalt and carbon-basalt composites had varying degrees of water absorption when exposed to seawater and river water. SEM and EDS Mapping analyses were conducted to understand better fibrous and granular composites' mechanical properties and water absorption behaviors. These analyses provided valuable insights and a comprehensive knowledge of composite properties. Ultimately, the study recommends using hybrid composite materials for specific applications based on desired flexural tensile strength, impact strength, or water absorption characteristics.

A threshold method of evaluating the critical trimming stage of FAP surface based on interface friction

Trimming technology is crucial for fixed abrasive pads (FAP) to maintain peak performance and prolonging their lifespan. However, there is a lack of effective evaluation methods for trimming FAP, which leads to under-trimming and over-trimming of FAP. As a result, it is very important to recognize and evaluate the critical trimming stage of the FAP. Therefore, the discriminative method for trimming FAP based on interfacial friction is proposed to determine the optimal trimming stage of FAP. Firstly, according to lapping experiments and tribological experiments of the FAP, the mapping relationship between the characteristics of interfacial friction and the parameters related to the FAP surface has been established. Secondly, the specific indices were identified to evaluate the surface state of FAP by the SEM analysis and mapping relationship of the FAP. Finally, the trimming thresholds of FAP were determined by combining the receiver operating characteristic (ROC) curves and Youden index, and the threshold achieved an average accuracy of over 92 % in recognizing the trimming requirements of the FAP. This research provides the theoretical basis for the online trimming technology and intelligent processing of FAP.

Mechanistic insights into molybdenum immobilization within geopolymer waste form

Molybdenum (Mo) tends to form highly mobile, non-sorbing complex redox species, which complicates its immobilization and encapsulation in cement and glass matrices. This study explores the potential of incorporating Mo into an alternative green cementitious material known as geopolymer (GP). By employing X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), morphological analysis, and nitrogen adsorption-desorption techniques, we obtained comprehensive insights into the chemical behavior of Mo and its impact on the morphology and structure of the GP matrix. XRD and TGA analysis demonstrated that increasing Mo content significantly enhances the crystallinity and thermal stability of the GP matrix, attributed to Mo field effects. High-resolution SEM, TEM, and EDS mapping revealed the structural encapsulation of Mo-rich cavities within the GP waste form. A decrease in leaching rates with higher Mo content, alongside reduced pore volume and pore size, underscores the material's chemical durability. Post-leaching characterizations confirmed that the GP retains excellent structural strength with minimal changes in mesoporosity and surface area. This resilience highlights the effectiveness of GPs in immobilizing non-sorbing species like MoO32−, making them ideal for long-term waste management.

Up-conversion luminescence and temperature sensing properties of Ho3+-, Tm3+-, and Yb3+-codoped Bi2WO6 materials in a water environment

A series of x%Ho3+, 5 %Tm3+, y%Yb3+:Bi2WO6 (x = 0, 0.5, 1, 3, 5; y = 0.5, 1, 3) luminescent materials was prepared using a high-temperature solid-phase method. The microstructure, up-conversion luminescence, and temperature sensing properties of the synthesized powders were analyzed. X-ray diffraction patterns revealed that doping with Ho3+, Tm3+, and Yb3+ ions at certain concentrations did not affect the orthorhombic crystal structure of the Bi2WO6 host. Scanning electron microscopy revealed that the morphology of the sample consisted of lumpy particles with a particle size range of 1–5 µm and agglomeration. SEM mapping and energy-dispersive X-ray spectroscopy analyses revealed that each element was relatively uniformly distributed on the particle surface. Under 980 nm excitation (380 mW), the strongest luminescence of the sample was obtained when both Ho3+ and Yb3+ doping concentrations were 1 %. Compared with the luminescence of the 5 %Tm3+ and 1 %Yb3+:Bi2WO6 sample, with increasing Ho3+ concentrations, the luminescence intensity of Tm3+ was first enhanced and subsequently weakened, whereas the luminescence of Ho3+ was significantly weakened, which indicates the positive energy transfer from Ho3+ → Tm3+. At 980 nm (80–380 mW), for the 1 %Ho3+, 5 %Tm3+, and 1 %Yb3+:Bi2WO6 sample, the 538 nm, 545 nm, 660 nm, and 804 nm emission peaks originated from the two-photon absorption. FIR660 nm/804 nm, FIR545 nm/804 nm, and FIR538 nm/804 nm were used to characterize the temperature and corresponded to temperature sensitivities Sr of 0.0046 K−1, 0.022 K−1 and 0.024 K−1 at 573 K, respectively. At 498 K, the minimum temperature resolution δT values were 0.03384 K, 0.03203 K and 0.04373 K. When the temperature increased from 298 K to 573 K, the powder sample luminescence gradually shifted from the yellow-green region to the red region. The results of environmental discoloration and thermochromic performance tests indicate that this sample has potential application in optical anti-counterfeiting. FIR804 nm /660 nm and FIR804 nm /538 nm were obtained for the 40 NTU turbidity suspension under identical excitation conditions. At 298 K, for the 40 NTU turbidity sample, the maximum Sr values were 0.0197 K−1 and 0.0405 K−1; at 340 K, the minimum temperature resolutions δT values were 0.54037 K and 0.66237 K. When the temperature decreased from 340 K to 298 K, the luminescence of the 40 NTU suspension samples gradually shifted from the yellow region to the green region.

Graphene Oxide Surface Modification of Reverse Osmosis (RO) Membrane via Langmuir-Blodgett Technique: Balancing Performance and Antifouling Properties.

The reverse osmosis water treatment process is prone to fouling issues, prompting the exploration of various membrane modification techniques to address this challenge. The primary objective of this study was to develop a precise method for modifying the surface of reverse osmosis membranes to enhance their antifouling properties. The Langmuir-Blodgett technique was employed to transfer aminated graphene oxide films assembled at the air-liquid interface, under specific surface pressure conditions, to the polyamide surface with pre-activated carboxylic groups. The microstructure and distribution of graphene oxide along the modified membrane were characterized using SEM, AFM, and Raman mapping techniques. Modification carried out at the optimal surface pressure value improved the membrane hydrophilicity and reduced the surface roughness, thereby enhancing the antifouling properties against colloidal fouling. The flux recovery ratio after modification increased from 65% to 87%, maintaining high permeability. The modified membranes exhibited superior performance compared to the unmodified membranes during long-term fouling tests. This membrane modification technique can be easily scaled using the roll-to-roll approach and requires minimal consumption of the modifier used.

Label free and ultrasensitive electrochemical detection of carcinoembryonic antigen using a disposable aptasensor based on Pd and graphene

We prepared an electrochemical aptasensor for label-free analysis of carcinoembryonic antigen (CEA). Herein, PdNPs were synthesized on the surface of graphene-modified screen-printed carbon electrodes (Pd-GN/SPCE) via electrochemical method for immobilisation of CEA aptamer as a bio-recognition element. The morphological characterizations of the fabricated Pd-GN/SPCE were performed using SEM, EDX, and elemental mapping that confirmed the successful electrochemical deposition of PdNPs. A disposable aptasensor for ultrasensitive electrochemical measurement of CEA was proposed by immobilising CEA aptamer on Pd-GN/SPCE. The electrochemical measurements were performed using 5 mM [Fe(CN)6]3-/4- as a redox probe. The electrochemical deposition of PdNPs improved the electrical conductivity resulting in enhanced current response for the redox probe. When CEA antigen interacts with CEA aptamer, it reduces the oxidation and reduction current of [Fe(CN)6]3-/4- due to the attachment of biomolecules to the electrode surfaces that hinders the electron transfer. The current changes of the redox species before and after CEA binding were measured using DPV. The developed aptasensor possessed a wide calibration range of 0.002–200 ng/mL and detection limit of 1.0 pg/mL. The aptamer-immobilised electrode provides an exceptional selectivity, reproducibility, and sensitive measurement of CEA. Moreover, the effective sensing of CEA in human serum samples with great recoveries (99.4––106 %) demonstrated its capability for clinical analysis.

A new strategy for immobilization of copper on the Fe3O4@EDTA nanocomposite and its efficient catalytic applications in reduction and one-pot reductive acetylation of nitroarenes and also N-acetylation of arylamines

A new and efficient Cu(II)-containing mesoporous nanocatalytic system was synthesized by direct immobilization of copper metal powder on the Fe3O4@EDTA nanocomposite. The as-prepared Fe3O4@EDTA@Cu(II) nanocomposite was then characterized by FT-IR, XRD, SEM, TEM, SEM-based EDX and elemental mapping, XPS, TGA, VSM, and also BET and BJH analyses. The resulting Fe3O4@EDTA@Cu(II) mesoporous nanocomposite exhibited satisfactory catalytic activity towards the reduction and one-pot reductive acetylation of nitroarenes and also N-acetylation of arylamines in water at 60 °C. Notably, the applied Cu(II)-containing nanocatalyst was efficiently recovered from the reaction mixture using an external magnetic field and could be reused successfully for five cycles. The protocol developed in this study offers several advantages in terms of mild reaction conditions, simple workflows, using water as a green solvent, and easy recovery and catalyst reuse, making it more ecologically and economically attractive.

Bioactive material‑sodium alginate-polyvinyl alcohol composite film scaffold for bone tissue engineering application

Road accidents and infection-causing diseases during bone surgery are serious problems in orthopedics, and thus, addressing these pressing challenges is crucial. In the present study, the 70S30C calcium silicate bioactive material (BM) is synthesized by a sustainable approach employing a precipitation method using recycled rice husk and eggshells as a precursor of silica and calcium. Further, 70S30C BM is composited with sodium alginate (SA) and polyvinyl alcohol (PVA), and the films were prepared by solvent casting method. The composite films were prepared without the addition of acid, binder, and crosslinking agents. Further, the films were characterized by BET, XRD, ATR-FTIR, SEM, and EDS mapping. The in vitro bioactivity and biodegradation study is performed in the simulated body fluid (SBF). The in vitro haemolysis study is executed using human blood and the results demonstrate haemocompatibility of the composite films. The ex ovo CAM assay also exhibits good neovascularization. The in vitro and in vivo biocompatibility assay proves its non-toxic nature. Further, the in vivo study reveals that the engineered composite film demonstrates accelerated osteogenesis. This work broadens the orthopedic potential of the composite film and offers bioactivity, haemocompatibility, angiogenesis, non-toxicity, and in vivo osteogenesis which would serve as a potential candidate for bone tissue engineering application.

Design and synthesis of C3-symmetric polymers with triazine-core and acetamide-linkers eliminating mobile genetic elements

A new class of C3-symmetric polymers with a s-triazine core hybrid and three acetamide linkers was successfully prepared from the etherification of acetamide derivatives Ace-1–4 with 1,3,5-tris-(4-hydroxyphenyl)triazine (THT), resulting in C3-symmetric polymers PTriAce-1–4. The precursor THT was synthesized through cyclotrimerization in the present superacid, while Ace-1–4 was synthesized through the condensation of chloroactyl chloride and different diamine derivatives. The synthesized C3-symmetric polymers were characterized by investigating their FT-IR, PXRD, SEM, and EDX mapping. These characterization techniques showed semi-crystalline structures, homogeneous distribution of microparticles, and good thermal stability as displayed by TGA. The preliminary results suggest that PTriAce-1 demonstrates substantial antibacterial efficacy against a diverse array of pathogenic strains and eliminates the mobilization of mobile genetic elements. The results indicate that this polymer interferes with S. aureus temperate bacteriophage 80α and affects their replication. This indicates the potential of these polymers as important agents in eliminating pathogens, bacteriophage replication, and the growth of antibiotic-resistant bacteria.

Scatalysis: Exploring the mechanism of photocatalytic algal removal

Photocatalytic algal removal is an environmentally friendly and low-cost algal bloom control technology. In this work, carbon nitride nanosheets based on morphology control were synthesized, and a ternary Z-scheme photocatalyst was designed through heterojunction engineering for photocatalytic removal of harmful algae and their organic matter, and the removal rate of chlorophyll a was close to 100 % in 300 min. Three-dimensional fluorescence spectrograms and cellular SEM maps revealed the removal of algae and their organic matter, and the mechanism of Ag/AgCl/ZIF-8/SCN photocatalytic algal removal was explored in conjunction with the changes in membrane permeability and various physiological functions. Mechanistic studies showed that excess O2·− played a crucial role in cell inactivation and organic matter degradation. Oxidative stress caused by O2·− promoted the accumulation of H2O2 in cells and accelerates cell death. This study provides new ideas and support for the application of harmful algal bloom control and the mechanism of algal cell inactivation in real water bodies.

Full colour luminescence tuning including white light from a mixed lanthanide activated metal-organic complex

In an attempt, metal–organic compounds of rare earth ions with 2,6-pyridinedicarboxylic acid (H2pydc) were synthesized and characterized. This paper summarizes the synthesis, characterization, and multicolour luminescence behaviour of a europium and terbium co-doped metal–organic compound (MOC) of formula [Y1.972Eu0.013Tb0.014(pydcH)6]·3H2O, 1 {H2pydc = 2,6-pyridinedicarboxylic acid}. The synthesis was performed by simple solvent evaporation method. We have also synthesized a pure yttrium based compound [Y2(pydcH)6]·3H2O, 1a following a similar procedure. The powder XRD patterns indicated that 1 and 1a were new materials; the patterns being entirely consistent with the simulated XRD pattern generated based on the structure of pure Eu compound determined using the single-crystal XRD. Compound 1 was well characterized by SEM, IR, TGA, EDX, and EDX elemental mapping analysis. Compound 1 showed different colour upon the variation of the excitation wavelength from 260 nm to 385 nm.

A low-temperature molten salt synthesis strategy of Eu2Ti2O7 ceramic enabling ultra-durable glass-ceramic waste forms

The conventional solid-phase sintering method for the preparation of Ln2Ti2O7 ceramics using oxides as reactants generally requires higher temperature, larger pressure, and greater energy consumption. In this paper, we synthesize a Eu2Ti2O7 ceramic powder in relatively low-temperature molten salt (KCl–NaCl) using Eu2O3 powder and TiO2 powder as reactants at 1000 °C. The results of XRD, SEM, and element mapping indicate that the product have high phase purity, good crystal morphology and uniform chemical composition. Moreover, Eu2Ti2O7-based glass-ceramics are obtained by sintering with different contents of borosilicate glass. The SEM images of glass-ceramic show that almost no obvious defects or voids are found on the surface of the samples. The values of water absorption for all glass-ceramic waste forms are less than 0.5 %. With the increase of ceramic embedding rate, the hardness of the glass-ceramics first increases and then decreases, while the density gradually increases. When the embedding rate increased to 30 wt%, the hardness of glass-ceramic reaches a maximum of 19.53 GPa. The glass-ceramic waste form embedded with 30 wt% Eu2Ti2O7 exhibits very stable chemical durability with a low leaching rate of 1.42 × 10−8 g m−2 d−1 at 90 °C even after 28 days.

Unveiling high resistivity mechanism in (0.8-x)BaTiO3-0.2BiScO3-x(Bi0.5Li0.5)TiO3 ceramics with good dielectric temperature-stability

Focusing on the high resistivity together with low intrinsic conduction in BaTiO3–BiMeO3 materials, it can contribute to the development of reliable high-temperature capacitor materials. In this work, x(Bi0·5Li0.5)TiO3-(0.8-x)BaTiO3-0.2BiScO3 (where x ranges from 0 to 0.2) ceramics were fabricated by a solid reaction method. The temperature stability of dielectric permittivity and resistance are improved significantly by the introduce of (Bi0·5Li0.5)TiO3 (referred to as BL) compared to BaTiO3–BiMeO3. The composition discrepancy due to chemical inhomogeneity can be determined by SEM and EDS mapping although XRD exhibit a single perovskite phase. The characteristics of distinct conductivity behaviors in micro-regions was measured by kelvin probe force microscopy (KPFM). The non-stoichiometry gives rise to two kinds of defects for charge compensation: an ionic compensation and oxygen-vacancy compensation in different grains. The increase of the hopping activation energy of charged carries enhances the high-temperature resistance of the system. The sample of x = 0.15 shows very good temperature stability of dielectric permittivity in the temperature range from 200 °C to 400 °C, and that of x = 0.1 exhibits the highest resistivity of 3.6 MΩ cm at 570 °C. The proposed method gives an efficient strategy for improving the dielectric temperature stability and insulation by the special defect compensation in the perovskite oxides.