Calcination Temperature Research Articles

Recovery of rare earth elements from sedimentary rare earth ore via sulfuric acid roasting and water leaching

Rare earth elements were extracted using a sulfuric acid roasting-water leaching process. The effect of acid roasting on a new type of low-grade sedimentary rare earth ore found in Guizhou Province, China was analyzed using X-ray diffraction and scanning electron microscopy. A systematic study was conducted on process parameters such as amount of acid, roasting temperature, roasting time, water leaching temperature, and leaching time. The results reveal that the total recovery of rare earth elements reaches 81.37%, which is 3.1 times higher than that achieved through direct acid leaching, under the optimal conditions. In addition, the leaching rate of heavy rare earth elements reaches 72.53%. Rare earth elements and some other valuable metals are transformed into soluble sulfate through the local decomposition of clay minerals under the action of the sulfuric acid attack. The dissolution rates of aluminum, iron, and titanium ions are 34.94%, 17.05%, and 62.77%, respectively. The precipitation rate of Ti reaches 99%, and the loss of rare earth ions in the solution is less than 1%. Meanwhile, the results of a leaching kinetics analysis indicate that the leaching process of rare ions is controlled by diffusion. Precious metal ions such as iron and aluminum in the leaching solution can reduce the adsorption of rare earth ions by kaolinite. This study efficiently recovered rare earth ions under conditions of low calcination temperature and direct water leaching, resulting in reduced energy consumption of the extraction process and acidity of the leaching solution. These findings provide a solid foundation for the further separation and extraction of rare earth ions.

Study on the Role of Additives in Calcination Desulfurization Process of High Sulfur Petroleum Coke

Due to the high sulfur content of high sulfur petroleum coke, sulfur-containing gas will be produced in the production process, reducing product quality and other problems, resulting in increased production costs and equipment corrosion. How to reduce the sulfur content of high sulfur petroleum coke is of great significance to improve the utilization rate of high sulfur petroleum coke and the sustainable development of related industries. In this paper, the desulfurization of high sulfur petroleum coke was carried out by using the additive-assisted high-temperature calcination method. It was found that the desulfurization effect of different kinds of desulfurization additives was different, among which MO1, MC2, MC1 desulfurization effect was better, and the desulfurization rate could reach 68%, 58%, 56%. After compounding the three desulfurizers, the desulfurization rate can be up to 75%, and then the influence of calcination temperature and time on the desulfurization rate was investigated. Finally, the physicochemical properties of petroleum coke before and after desulfurization were analyzed by X RD, FT-IR.

Effect of dopant loading and calcination conditions on structural and optical properties of ZrO2 nanopowders doped with copper and yttrium

Undoped, Cu and/or Y doped ZrO2 nanopowders were synthesized with Zr, Y, and Cu nitrates using a co-precipitation approach. Their structural and optical properties were examined regarding dopant content (0.1–8.0 mol.% of CuO and 3–15 mol.% of Y2O3) and calcination conditions (400 °C–1000 °C and, 1,2 or 5 h) through Raman scattering, XRD, TEM, EDS, AES, EPR, UV–vis and FTIR diffused reflectance methods. The results showed that both Cu and Y dopants promoted the appearance of additional oxygen vacancies in ZrO2 host, while the formation of tetragonal and cubic ZrO2 phases was primarily influenced by the Y content, regardless of Cu loading. The bandgap of most of the powders was observed within the 5.45–5.65 eV spectral range, while for those with high Y content it exceeded 5.8 eV. The (Cu,Y)-ZrO2 powders with 0.2 mol.% CuO and 3 mol.% Y2O3 calcined at 600 °C for 2 h demonstrated nanoscaled tetragonal grains (8–12 nm) and a significant surface area covered with dispersed CuxO species. For higher calcination temperatures, the formation of CuZr 2+ EPR centers, accompanied by tetragonal-to-monoclinic phase transformation, was found. For fitting of experimental FTIR reflection spectra, theoretical models with one, five, and seven oscillators were constructed for cubic, tetragonal, and monoclinic ZrO2 phases, respectively. Comparing experimental and theoretical spectra, the parameters of various phonons were determined. It was found that the distinct position of the high-frequency FTIR reflection minimum is a unique feature for each crystalline phase. It was centered at 700–720 cm−1, 790–800 cm−1, and 820–840 cm−1 for cubic, tetragonal, and monoclinic phases, respectively, showing minimal dependence on phonon damping coefficients. Based on the complementary nature of results obtained from structural and optical methods, an approach for monitoring powder properties and predicting catalytic activity can be proposed for ZrO2–based nanopowders.

Molybdenum tailings calcination for phase composition of Si-Ca-K-Mg fertilizers: Modification of phase transformation and its effects on plant growth

The high value and comprehensive utilization of molybdenum tailings for the production of fertilizer of calcium silicon magnesium potassium (Si-Ca-K-Mg fertilizer) was investigated, considering the abundant potassium feldspar (K-feldspar) content in the tailings. The effects of calcination temperatures, times, and additives (CaCO3 and CaSO4) on reaction degree, final product type, and phase transition process were studied. The results indicated that at 1200 °C, calcination time of 120 min and m(molybdenum tailings):m(CaCO3):m(CaSO4) = 1:0.7:0.2, the final product met Type I product requirements according to Chinese national standards GB/T36207-2018 as well as extremely low heavy metal contents. In the calcination process, CaO resulted from CaCO3 absorbs the liquid phase produced during K-feldspar decomposition to form CaSiO3, facilitating the K-feldspar decomposes into KAlSiO4. Simultaneously, the Ca2+ in CaSO4 replaces undecomposed K-feldspar’s K+. Additionally, CaO reacts with Al2O3, MgO, and SiO2 to produce gehlenite (Ca2Al2SiO7) and akermanite (Ca2MgSi2O7), providing plants with Ca, Mg, and Si elements. The nutrients of the fertilizer were readily assimilated by plants, improving acidic soil without causing any harm to the soil or vegetation. This work offers new ideas for large-scale and high-value utilization of molybdenum tailings as well as addressing the shortage of soluble potassium resource in China.

The Effect of Calcination Temperature on the Characteristics of CeO2 Synthesized Using the Precipitation Method

Cerium oxide (CeO2) was synthesized using the precipitation method at various calcination temperatures ranging from 500 to 700°C. Cerium(III) nitrate hexahydrate (Ce(NO)3.6H2O) was used as the precursor for cerium, while Cetyltrimethylammonium bromide (CTAB) acted as the morphology-directing agent. Characterization results indicated that pure CeO2 was obtained at all calcination temperature variations. Calcination temperature influences crystallinity, crystal size, and CeO2 crystal parameters. The crystallinity and crystal size of CeO2 increased with the rising calcination temperature, reaching values of 81.1–84.5% and 15.58–23.12 nm, respectively, along with larger crystal parameters as the temperature increased (a = 5.406–5.410 Å). Surface morphology showed irregular shapes of CeO2 particles, with decreasing sizes as the calcination temperature increased, ranging from 0.2-5.6 μm at 600°C to 0.12-2.9 μm at 700°C. The Ce/O ratio on the surface increased with the rising calcination temperature, reaching a range of 0.48–0.57. CeO2 obtained from calcination at 600°C exhibited the highest fluorescence emission intensity (λ= 496 nm), indicating the least oxygen vacancies presence. Therefore, for antioxidant and catalyst applications, it is preferable to calcinate CeO2 at 700°C.

Asymmetric Supercapacitors Based on ZnCo2O4 Nanohexagons and Orange Peel Derived Activated Carbon Electrodes.

Herein, the performance of asymmetric supercapacitors (ASC) fabricated using ZnCo2O4 (ZCO) nano-hexagons and orange peel-derived activated carbon (OPAC) as electrodes was studied. ZCO was prepared by a double hydroxide method and OPAC was prepared from orange peel followed by KOH activation. For ZCO, the calcination temperature was determined using TGA analysis. The XRD showed the presence of a cubic spinel structure. The chemical structure was analyzed using XPS, FTIR, and Raman spectroscopy respectively. For OPAC, the presence of an amorphous nature was inferred; FTIR and Raman studies indicate the presence of functional groups and defect structure in the material. The presence of ZCO nano-hexagons was observed from SEM and TEM respectively. For OPAC, an interconnected pore structure was observed from the SEM image. The specific capacitance for ZCO and OPAC was found to be 194 F.g-1 and 159 F.g-1 at a current density of 0.25 A.g-1. Further, an ASC was fabricated using ZCO as a positive and OPAC as a negative electrode in 2M KOH-soaked separator. A cell voltage of 1.2 V was achieved and the specific capacitance was calculated to be 64 F.g-1 at 0.25 A.g-1. Further, the cyclic stability and the changes at the electrode/electrolyte interface were studied.

Soft-templating synthesis of mesoporous MnSiOx composites as catalytic supports for Pd nanoparticles towards solvent-free oxidation of benzyl alcohol under atmospheric pressure O2

Solvent-free and liquid-phase selective oxidation of aromatic alcohols using O2 as an oxidant is a green strategy for the synthesis of aromatic aldehydes and other carbonyl compounds. Wherein, the design and preparation of heterogeneous catalysts with high activity and selectivity is a hot topic in this process. Herein, a series of manganese oxide-silica (MnSiOx) composites were synthesized using cetyltrimethylammonium bromide as a soft template. During the preparation process, the amounts of tetraethyl orthosilicate and ammonia and the calcination temperature significantly affected the textural properties and Mn cation distributions of MnSiOx. The MnSiOx composites were then employed as catalysts for Pd nanoparticles. In the solvent-free and atmospheric conditions, Pd/MnSiOx materials showed high catalytic conversions of benzyl alcohol (BZA), and the catalytic activity thereof is related to the fractions of Pd0 and Mn3+. As the reaction time and temperature are 4 h and 90 °C, the conversion of BZA (feeding dosage: 4 mL) and the selectivity of benzaldehyde are 64.8 % and 94.9 %, respectively. The catalyst can be reused at least five times without any significant loss of activity. Furthermore, the correlation between physiochemical properties and catalytic activity of Pd/MnSiOx was analyzed.

Transforming crystal structures of cobalt molybdate to generate electron-rich sites for electrochemical detection of Pb(II)

BackgroundMost of the investigations on distinct crystal structures of catalysts are individually focused on the difference of surface functional groups or adsorption properties, but rarely explore the changes of active sites to affect the electrocatalytic performance. Catalysts with diverse crystal structures had been applied to modified electrodes in different electrocatalytic reactions. However, there is currently a lack of an essential understanding for the role of real active sites in catalysts with crystalline structures in electroanalysis, which is crucial for designing highly sensitive sensing interfaces. ResultsHerein, cobalt molybdate with divergent crystal structures (α-CoMoO4 and β-CoMoO4) were synthesized by adjusting the calcination temperature, indicating that α-CoMoO4 (800 °C) (60.00 μA μM−1) had the highest catalytic ability than β-CoMoO4 (700 °C) (38.68 μA μM−1) and α-CoMoO4 (900 °C) (29.55 μA μM−1) for the catalysis of Pb(II). It was proved that the proportion of Co(II) and Mo(IV) as electron-rich sites in α-CoMoO4 (800 °C) were higher than β-CoMoO4 (700 °C) and α-CoMoO4 (900 °C), possessing more electrons to participate in the valence cycles of Co(II)/Co(III) and Mo(IV)/Mo(VI) to boost the catalytic reduction of Pb(II). Specifically, Co(II) transferred a part of electrons to Mo(VI), promoting the formation of Mo(IV). Co(II) and Mo(IV), as the electron-rich sites, providing electrons to Pb(II), further accelerating the conversion of Pb(II) into Pb(0). SignificanceIn the process of detecting Pb(II), the CoMoO4 structures under different temperatures have distinct content of electron-rich sites Co(II) and Mo(IV). α-CoMoO4 (800 °C), with the highest content are benefited to detect Pb(II). This work is conducive to understanding the effect of the changes of active sites resulting from crystal transformation on the electrocatalytic performance, and provides a way to construct sensitive electrochemical interfaces of distinct active sites.

Improvement of Hydrogen Peroxide and Glucose Detection in Serum using Persistent Luminescent Nanoparticles: Impact of Synthesis Parameters and Particle Size

AbstractPersistent Luminescent Nanoparticles (PLNPs) emit prolonged light after excitation, allowing getting images with high signal‐to‐noise ratio, making them particularly beneficial for in vitro biodetection. In this study, we report the preparation of a library of gallium and zinc‐based Persistent Luminescent Nanoparticles doped with chromium (ZnGa2O4:Cr3+) through two distinct syntheses conducted at 120 °C for 12 hours or 24 hours, followed by a calcination at 500 °C or 750 °C. Using centrifugation, and starting from polydisperse samples, we demonstrated the ability to achieve different sizes in a monodisperse manner. Furthermore, our research revealed that ZnGa2O4:Cr3+ (ZGO) nanoparticles react differently with hydrogen peroxide (H2O2) based on their size, synthesis duration, and calcination temperature. We observed the most significant amplification of persistent luminescence for ZGO particles prepared at 120 °C for 12 hours and calcinated at 500 °C, with a size of approximately 100 nm, in the presence of 100 mM H2O2 (later named ZGO‐2). This study enabled the detection of H2O2 in serum without autofluorescence using the developed PLNPs, with a detection limit of up to 2.1 μM and a recovery rate of around 99 %. Additionally, we designed a glucose test for based on the responsiveness of ZGO PLNPs to H2O2. Using glucose oxidase, the glucose detection limit in serum was established around 0.13 μM, with a detection range between 0–5 μM. These findings could open new avenues to further control the size, synthesis, calcination temperature, and persistent luminescence of PLNPs, thus enhancing their utility in the development of new in vitro biosensors.

Carbon-decorated diatomite stabilized lauric acid-stearic acid as composite phase change materials for photo-to-thermal conversion and storage

Diatomite is a promising supporting matrix in the preparation of composite phase change material for latent thermal energy storage. Raw diatomite has the advantages of porous space but with a shortage of thermal conductivity than carbon materials. In this work, the carbon-decorated diatomite (DC) matrix was synthesized by a novel template-carbonization method at different calcination temperatures of 600 °C, 800 °C, and 1000 °C. Then, the matrix was used to stabilize binary lauric-stearic acid of LA-SA for the preparation of diatomite-based composite phase change material which is used to explore the application of composite in photo-to-thermal conversion/storage. Results show that the carbon-decorated process on diatomite causes an increment of specific surface area and pore space. Thus, more phase change material being loaded in the matrix leads to a larger heat storage capacity of the composite. The designed composite with a matrix carbonization temperature of 1000 °C, LA-SA/DC-1000, has a loadage of 49.92 %, melting temperature of 31.48 °C, and latent heat of 70.07 J g-1 which is improved by 23 %. Compared with the raw diatomite-based composite, the enhancements of thermal conductivity were 90 % for that of LA-SA/DC-1000. Moreover, the corresponding composite exhibits better photo-to-thermal conversion performance and transient temperature response.

Multienzyme Mimicking Cascade Mn3O4 Catalyst to Augment Reactive Oxygen Species Elimination and Colorimetric Detection: A Study of Phase Variation upon Calcination Temperature.

Over decades, nanozyme has served as a better replacement of bioenzymes and fulfills most of the shortcomings and intrinsic disadvantages of bioenzymes. Recently, manganese-based nanomaterials have been highly noticed for redox-modulated multienzyme mimicking activity and wide applications in biosensing and biomedical science. The redox-modulated multienzyme mimicking activity was highly in tune with their size, surface functionalization, and charge on the surface and phases. On the subject of calcination temperature to Mn3O4 nanoparticles (NPs), its phase has been transformed to Mn2O3 NPs and Mn5O8 NPs upon different calcination temperatures. Assigning precise structure-property connections is made easier by preparing the various manganese oxides in a single step. The present study has focused on the variation of multienzyme mimicking activity with different phases of Mn3O4 NPs, so that they can be equipped for multifunctional activity with greater potential. Herein, spherical Mn3O4 NPs have been synthesized via a one-step coprecipitation method, and other phases are obtained by direct calcination. The calcination temperature varies to 100, 200, 400, and 600 °C and the corresponding manganese oxide NPs are named M-100, M-200, M-400, and M-600, respectively. The phase transformation and crystalline structure are evaluated by powder X-ray diffraction and selected-area electron diffraction analysis. The different surface morphologies are easily navigated by Fourier transform infrared, field-emission scanning electron microscopy, and high-resolution transmission electron microscopy analysis. Fortunately, for the mixed valence state of Mn3O4 NPs, all phases of manganese oxide NPs showed multienzyme mimicking activity including superoxide dismutase (SOD), catalase, oxidase (OD), and peroxidase; therefore, it offers a synergistic antioxidant ability to overexpose reactive oxygen species. Mn3O4 NPs exhibited good SOD-like enzyme activity, which allowed it to effectively remove the active oxygen (O2•-) from cigarette smoke. A sensitive colorimetric sensor with a low detection limit and a promising linear range has been designed to detect two isomeric phenolic pollutants, hydroquinone (H2Q) and catechol (CA), by utilizing optimized OD activity. The current probe has outstanding sensitivity and selectivity as well as the ability to visually detect two isomers with the unaided eye.

Enhancing photocatalytic tetracycline degradation through the fabrication of high surface area CeO2 from a cerium-organic framework.

Water pollution is a global environmental issue, and the presence of pharmaceutical compounds, such as tetracyclines (TCs), in aquatic ecosystems has raised growing concerns due to the potential risks to both the environment and human health. A high surface area CeO2 was prepared via atmospheric thermal treatment of a metal-organic framework of cerium and benzene-1,3,5-tricarboxylate. The effects of calcination temperature on the morphology, structure, light absorption properties and tetracycline removal efficiency were studied. The best activity of the photocatalysts could be achieved when the heat treatment temperature is 300 °C, which enhances the photocatalytic degradation performance towards tetracycline under visible light. The resulting CeO2 particles have high capacity for adsorbing TCs from aqueous solution: 90 mg g-1 for 60 mg L-1 TCs. As a result, 98% of the initial TC can be removed under simulated sunlight irradiation. The cooperation of moderate defect concentration and disordered structure showed tetracycline removal activity about 10 times higher than the initial Ce-MOF. An embryotoxicity assessment on zebrafish revealed that treatment with CeO2 particles significantly decreased the toxicity of TC solutions.

(1 1 1) Facet-dominant peracetic acid activation by octahedral CoO anchored hollow carbon microspheres for tetracycline degradation

Peracetic acid (PAA), an environmental friendly disinfectant, has attracted increasing interest in applications on advanced oxidation processes for treating emerging pollutants. Herein, octahedral cobalt oxide anchored on cation exchange resin (CER)-derived hollow carbon microspheres were fabricated via a facile strategy and employed as the heterogeneous catalyst for PAA activation to degrade tetracycline (TC) antibiotic. Calcination temperature was demonstrated to play a significant role in resulted structure and composition, physicochemical properties and catalytic activities of the cobalt-based compounds/carbon composites. With the optimal catalyst which was calcined at 600 °C, namely the Co@CER-600, complete elimination of TC was achieved within 10 min in Co@CER-600/PAA system. The determination of reactive oxygen species (ROS) indicated that both non-radical (singlet oxygen) and radical (superoxide radical) mechanisms were evidenced in Co@CER-600/PAA system. Particularly, it is notable that the extensively exposed (111) facet in octahedral CoO was confirmed to show remarkable PAA activation activity, therefore promoted the ROS generation process. Considering that facet engineering is a novel whilst important strategy for catalyst regulation, the proposed (111) facet-dominant octahedral CoO anchored hollow carbon microspheres might suggest new inspirations for catalyst design in PAA-based AOPs toward antibiotic contamination remediation.

Tune and turn the pyrolysis of metal organic frameworks towards stable supported nickel catalysts for the dry reforming of methane

Dry reforming of methane (DRM) is an inimitable approach for eliminating both greenhouse gases, methane and CO2, while producing synthesis gas which further can be converted to added-value fuels. However, the industrialization of DRM has been limited due to sintering and coking to the catalysts under the harsh reaction conditions. Here, we propose a new methodology for producing tunable supported nickel-based catalysts for DRM using metal organic frameworks (MOFs) as precursors of the catalyst components. In particular, Ni- and La-MOFs were coalesced using sonication and then calcined at different temperatures to produce catalysts with tailored Ni metal size (5–20 nm) and tuned strong metal-support interactions (SMSI). Here, the synthesis of nickel and nickel oxide nanoparticles embedded on lanthanum-based supports by controlled calcination of the MOF structures is demonstrated; the Ni supported catalysts were then used for DRM reaction. Among the developed catalysts, the catalyst produced following calcination at 500 °C (Ni-La-500) has shown stable and high CH4 conversion rates under DRM conditions at 800 °C with negligible carbon formation at elevated gas hourly space velocities. Further, the catalytic performance of Ni-La-500 catalyst (sonicated) was compared to the physically mixed MOFs derived catalyst (Ni-La-500-PM), conventional wetness impregnated catalyst (Ni-La-500 WI), Ni-MOF derived unsupported catalyst (Ni-500), and lower Ni concentration catalyst (sonicated, 10Ni-La-500). The observed CH4 conversion rates at 50,000 mL·gcat–1·h−1 GHSV are 81.8, 67.9, 85.4, 34.7, and 57.9 % for Ni-La-500, Ni-La-500 PM, Ni-La-500 WI, Ni-500, and 10Ni-La-500 catalysts, respectively after 24 h of DRM reaction. With isotopic studies, it was found that the 18O exchange rate was higher in case of Ni-La-500-PM catalyst (8.1 mmol·g−1) as compared to Ni-La-500 catalyst (5.5 mmol·g−1). Prior interaction between MOFs, calcination temperatures, reaction conditions, and the carbon pathways during catalytic activity dictates the conversion rates and selectivity of the products. Overall, with the herein proposed approach of MOF-derived supported catalysts exceptional conversion rates and stability during the DRM reaction with nominal coking and sintering were demonstrated, solving the two major challenges faced by conventional and unsupported catalysts.

Temperature-Induced Conversion of 2D Vanadium-Doped MoSe2 Nanosheets to 1D V2MoO8 Rods: Enhanced Performance in Electrochemical Antibiotic Detection in Biological and Environmental Samples.

In this work, new strategies were developed to prepare 1D-V2MoO8 (VMO) rods from 2D V-doped MoSe2 nanosheets (VMoSe2) with good control over morphology and crystallinity by a facile hydrothermal and calcination process. The morphological changes from 2D to 1D rods were controlled by changing the calcination temperature from 300 to 600 °C. The elimination of Se and the incorporation of O into the V-Mo structure were evaluated by TGA, p-XRD, Raman, FE-SEM, EDAX, FE-TEM, and XPS analyses. These results prove that the optimization of the physical parameters leads to changes in the crystal phase and textural properties of the prepared material. The VMoSe2 and its calcined products were investigated as electrochemical sensors for the detection of the antibacterial drug nitrofurantoin (NFT). At a calcination temperature of 500 °C, the modified screen-printed carbon electrodes (SPCE) proved to be an excellent electrochemical sensor for the detection of NFT in neutral media. Under the optimized conditions, VMO-500 °C/SPCE exhibits low detection limit (LOD) (0.015 μM), wide linear ranges (0.1-31, 47-1802 μM), good sensitivity, and selectivity. The proposed sensor was successfully used for the analysis of NFT in real samples with good recovery results. Moreover, the reduction potential of NFT agreed well with the theoretical analysis using quantum chemical calculations, with the B3LYP with 6-31G(d,p) basis set predicting an E0 value of -0.45 V. The interaction between the electrode surface and NFT via the LUMO diagram and the electrostatic potential surface is also discussed.

Resource utilisation of hazardous aluminium dross and coal gangue for fibre-reinforced cemented foam backfill

The resource utilisation of hazardous aluminium dross and coal gangue for fibre-reinforced cemented foam backfill can enhance the stability of filling stopes and address environmental issues. Herein, aluminium dross was first co-calcined with quicklime at 800°C, 950°C and 1100°C to prepare modified foaming agents, and their phase transformations during calcination were analysed. Next, the calcined mixes, cement, coal gangue and fibres were employed to prepare the samples. The expansion ratio and hydration evolution—as well as the strength, deformation and heavy metal–leaching behaviours—of the fibre-reinforced cemented foam backfill were comprehensively investigated. Experimental results reveal that partial elemental Al in raw aluminium dross becomes active in the C12A7 and CA2 forms, which enhances the hydration reactivity of the calcined mixes. The efficient denitrification achieved at 1100°C is because of the coupled effects of quicklime dispersion and high-temperature calcination. The grindability of the calcined mixes initially improves and subsequently worsens with increasing calcination temperature, which is related to the Al2O3 crystallinity. Active Al in the calcined mixes is conducive to hydration at an early age, leading to the generation of larger quantities of Hc/Mc and the AH3 gel and a smaller amount of portlandite. Owing to the coupled effects of the porous structure and fibre reinforcement, the fibre-reinforced cemented foam backfill exhibits good mechanical performance and large plastic deformation. Furthermore, the M1-10, M2-10 and M2-30 samples possessing an expansion ratio of 4%–10 %, a compressive strength of >3 MPa and a good ability to stabilise heavy metals are excellent choices for the practical application of foam backfill technology in mining engineering.

Investigation of the thermal decomposition of Pu(IV) oxalate: a transmission electron microscopy study

The degradation of the internal structure of plutonium (IV) oxalate during calcination was investigated with Transmission Electron Microscopy (TEM), electron diffraction, Electron Energy-Loss Spectroscopy (EELS), and 4D Scanning TEM (STEM). TEM lift-outs were prepared from samples that had been calcined at 300°C, 450°C, 650°C and 950°C. The resulting phase at all calcination temperatures was identified as PuO2 with electron diffraction. The grain size range was obtained with high-resolution TEM. In addition, 4D STEM images were analyzed to provide grain size distributions. In the 300°C calcined sample, the grains were <10 nm in diameter, at 650°C, the grains ranged from 10 to 20 nm, and by 950°C, the grains were 95–175 nm across. Using the Kolmogorov-Smirnov (K-S) two sample test, it was shown that morphological measurements obtained from 4D-STEM provided statistically significant distributions to distinguish samples at the different calcination conditions. Using STEM-EELS, carbon was shown to be present in the low temperature calcined samples associated with oxalate but had formed carbon (possibly graphite) deposits in the 950°C calcined sample. This work highlights the new methods of STEM-EELS and 4D-STEM for studying the internal structure of special nuclear materials (SNM).

Synthesis of Cu0.5Zn0.5-xNixFe2O4 nanoparticles as heating agents for possible cancer treatment

Magnetic mixed ferrites with high heating efficacy have attracted lots of attention as a complementary method for cancer treatment via magnetic hyperthermia therapy. In the present study, magnetic Cu0.5Zn0.5-xNixFe2O4 nanoparticles were synthesized via a sol–gel combustion method. The effects of nickel substitution (x = 0.1, 0.2, 0.3, 0.4 and 0.5) on the magnetic and structural properties of the produced nanoparticles were investigated. The produced magnetic nanopowders were studied via X-ray diffraction (XRD), scanning electron microscopy (SEM), simultaneous thermal analysis (STA), Fourier-transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), and vibrating-sample magnetometry (VSM) techniques. The results showed that the saturation magnetization and coercivity of ZnCuFe2O4 nanoparticles were strongly affected by nickel substitution in the structure so that saturation magnetization decreased from 55.4 emu/g to 36.0 emu/g, whereas coercivity increased from 87.9 Oe to 156.4 Oe. In addition, saturation magnetization for the Cu0.5Zn0.4Ni0.1Fe2O4 sample increases from 55 to 58.1 emu/g with a rise in calcination temperature from 400 to 700 °C, respectively. The heating efficiency of the samples was investigated under different magnetic fields for magnetic hyperthermia therapy. The Cu0.5Zn0.4Ni0.1Fe2O4 sample exhibits a temperature increase from 37 °C to 49.5 °C during 10 min in the exposure of a magnetic field of 400 Oe and frequency of 200 kHz. The specific absorption rate value calculated for the Cu0.5Zn0.5-xNixFe2O4 nanoparticles was 53.1 W/g. With the increase in the viscosity of the environment, the heating efficiency of nanoparticles is reduced. Despite this decrease, the magnetic characteristics of nanoparticles remained strong enough to envision their usage as heating agents in magnetic hyperthermia.

Noble metal (Pt, Pd and Rh) promoted Ni-Co/Mg(Al)O catalysts for steam reforming of tar impurities from biomass gasification

Steam reforming is a promising approach to remove biomass gasification tar impurities. Noble metal promotion (Pt/Pd/Rh), Ni+Co loading (20–40 wt%) and calcination temperature (600–800 °C) effects were investigated with hydrotalcite-derived Ni-Co/Mg(Al)O catalysts for bio-syngas tar steam reforming. Fresh catalysts were characterized by XRD, ICP-MS, XRF, N2-physisorption, H2-chemisorption and TPR. Small-diameter metal particles were achieved (5.1–5.8 nm) below a Ni+Co loading threshold (above 30 wt%). Model bio-syngas activity tests were performed (CH4/H2/CO/CO2 molar ratio = 10/35/25/25, 700 °C, steam-to-carbon = 3.0) with and without tar addition (toluene/1-methylenaphthalene, 10 g/Nm3). Tar elimination was achieved with all samples. Enhanced reforming activity accompanied by strong tar active site inhibition effects were found for the Rh promoted catalyst. Noble metal promoted samples were effectively reduced in the bio-syngas environment (H2/CO/CH4) without any pre-reduction (in situ activation by the action of the syngas) with Rh > Pt > Pd. Coke characterization was conducted with TPO-MS and Raman spectroscopy. High-dispersion 20NiCo/30NiCo samples were strongly deactivated through active site inhibition and coke formation. High-temperature calcination (800 °C) reduced the deactivation effects of the coke deposition, attributed to enhanced Mg(Al)O-assisted coke gasification.

Bismuth-rich BiOBr/Bi24O31Br10/Ti3C2 polyheterojunction for visible photocatalytic degradation of dyes and Cr(VI) reduction and hydrogen production applications

The construction of bismuth-rich heterostructures is an important strategy to improve the performance of bismuth-based visible photocatalytic materials. In this study, the binary heterojunction BiOBr/Bi24O31Br10 (BOB) with efficient visible photocatalytic activity was constructed by in situ induced growth of BixOyBrz on the surface of BiOBr, and the multivariate heterojunction composite BiOBr/Bi24O31Br10/Ti3C2 (BOBT) was synthesized by using Ti3C2 as an electron acceptor. It was shown that the solvothermal pH, Bi/Br and calcination temperature had a strong influence on the composition and crystalline structure of BOBT. The optimized synthesis conditions were pH=8, Bi/Br=1/1 (molar ratio), and calcination temperature of 400℃. The introduction of Mxene significantly enhanced the visible-light responsiveness and photoelectric efficiency of BOBT. The visible light-catalyzed degradation of complex conjugated systems containing aromatic and azo structures by BOBT was synchronously accompanied by benzene ring opening, demonstrating an efficient visible light degradation capability. BOBT has a reduced reduction current peak compared to BOB, can rapidly reduce Cr (VI), and improves the photocatalytic hydrogen production efficiency by nearly three times compared to BiOBr without the addition of Pt additives. This study provides fundamental data for the construction of efficient bismuth-based visible photocatalytic materials and their applications.