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At least 307 records · Page 17

Are we modeling the properties of unconventional shales correctly?

Technological advancements have led to impressive growth in hydrocarbon (HC) production from unconventional shale reservoirs. However, major limiting factors in shale gas development are i) low recovery of gas in place (<20%), (ii) a rapid decline in well productivity, iii) release of contaminants, despite the use of advanced hydraulic fracturing fluids and multiple fracturing stages. This is mainly due to a lack of understanding of the nanoscale physicochemical properties of shales, especially that of kerogen, the macromolecule that is not only the source of the majority of the HC’s in shales but also holds most of the HC’s in adsorbed state. Over the last few years, a large number of studies have been published on simulating the physicochemical properties of shale utilizing molecular models of kerogen. However, the molecular models of kerogen input into these simulations are based on the kerogen “type” derived from a very limited number of shale samples. In this paper, we examine the variations that can exist in kerogen structure within a particular kerogen “type” across different shale basins and single shale basin at similar thermal maturity levels. We propose that using kerogen “type” based structural models for molecular simulations could lead to inaccurate estimation of HC reserves, HC recovery, HC production, frackability, and quantity and quality of produced water. Our study highlights the need for developing a better classification of kerogen based on its “molecular structure” instead of “type” for a more accurate prediction of physicochemical properties of shales.

04 OIL SHALES AND TAR SANDS↗

Surface exsolving perovskite ceramics as catalyst for microwave methane pyrolysis to co-generate hydrogen and carbon nanotube

In this study, we have successfully developed a novel surface exsolving perovskite ceramic, which demonstrates the ability to simultaneously generate CO x -free hydrogen and carbon nanotubes (CNTs) through methane pyrolysis under the influence of microwave irradiation. We conducted an extensive survey and optimization of various perovskite materials specifically tailored for microwave applications. Among the materials investigated, nickel-doped strontium titanium oxide (STON) emerged as the most promising candidate, exhibiting both a satisfactory methane conversion rate and excellent responsiveness to microwave irradiation. Refinement of STON was carried out by fine-tuning the Ni content, optimizing the reduction dwell time, and adjusting the reduction temperature. Notably, SrTiNi 0.08 O 3 (STON8), demonstrated an impressive initial methane conversion rate of up to 40%. Transmission Electron Microscopy (TEM) provided visual evidence of the correlation between Ni content and reduction temperature, with respect to the exsolved Ni metal particle size. This finding highlights the immense potential of surface exsolving perovskite ceramics as a highly effective catalyst for the simultaneous production of CNTs and COx-free hydrogen via methane pyrolysis under microwave irradiation. Furthermore, it represents a step forward in the field of catalytic materials and microwave-driven processes.

08 HYDROGEN↗

Facile synthesis of Co(OH)2 nanoneedle arrays grown on stainless steel for industrial electrochemical oxygen evolution reaction

The electrochemical oxygen evolution reaction (OER) is a critical half-reaction in a variety of energy conversion and storage applications, however, OER suffers from sluggish kinetics due to the four proton-electron transfer processes. To remedy this, interfacial engineering proves an effective strategy to design high active OER catalysts. Herein, we report a facile synthesis of Co(OH)2 nanoneedle (Co-NN) arrays grown on stainless steel (SS) via a one-step hydrothermal reaction, and the resultant impressive OER performance. Particularly, the Co-NN/SS needs 267, 307, and 576 mV overpotentials to reach 10, 100, and 1000 mA cm−2 in 1 M KOH & room temperature, and the overpotentials drop to 199, 257, and 283 mV to achieve the same current densities in 30 wt% KOH & 80 °C. Additionally, an alkaline water electrolysis (AWE) cell coupled with Co-NN/SS anode and PtRu/NiMo cathode only requires 1.65 and 1.73 V iR-free cell voltage to reach 1.0 and 2.0 A cm−2, respectively. The sterling OER performance could be attributed to four possible reasons, the Fe in SS surface tailoring the electronic properties of Co(OH)2, the mixed metal oxides on SS surface accelerating surface reconstruction of Co(OH)2 nanoneedles into CoOOH active species, a Ni-rich surface layer formation cooperatively boosting the OER activity, and a local electric field effect concentrating reactants on the tip surface and accelerating the mass transfer. This work provides a facile approach for synthesizing highly efficient OER catalysts for industrial applications by interfacial engineering.

Lyu, Xiang [ORNL] (ORCID:0000000208673248)↗

Change in Pattern of Relapse After Antiangiogenic Therapy in High-Grade Glioma

Purpose: Local recurrence is the dominant pattern of relapse in high-grade glioma (HGG) after conventional therapy. The recent use of antiangiogenic therapy has shown impressive radiologic and clinical responses in adult HGG. The preclinical data suggesting increased invasiveness after angiogenic blockade have necessitated a detailed analysis of the pattern of recurrence after therapy. Methods and Materials: A total of 162 consecutive patients with HGG, either newly diagnosed (n = 58) or with recurrent disease (n = 104) underwent therapy with bevacizumab at 10 mg/kg every 2 weeks and conventional chemotherapy with or without involved field radiotherapy until disease progression. The pattern of recurrence and interval to progression were the primary aims of the present study. Diffuse invasive recurrence (DIR) was defined as the involvement of multiple lobes with or without crossing the midline. Results: At a median follow-up of 7 months (range, 1-37), 105 patients had recurrence, and 79 patients ultimately developed DIR. The interval to progression was similar in the DIR and local recurrence groups (6.5 and 6.3 months, p = .296). The hazard risk of DIR increased exponentially with time and was similar in those with newly diagnosed and recurrent HGG (R{sup 2} = 0.957). The duration of bevacizumab therapy increased the interval to recurrence (p < .0001) and improved overall survival (p < .0001). However, the pattern of relapse did not affect overall survival (p = .253). Conclusion: Along with an increase in median progression-free survival, bevacizumab therapy increased the risk of DIR in HGG patients. The risk of increased invasion with prolonged angiogenic blockade should be addressed in future clinical trials.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Anatomic Distribution of Fluorodeoxyglucose-Avid Para-aortic Lymph Nodes in Patients With Cervical Cancer

Purpose: Conformal treatment of para-aortic lymph nodes (PAN) in cervical cancer allows dose escalation and reduces normal tissue toxicity. Currently, data documenting the precise location of involved PAN are lacking. We define the spatial distribution of this high-risk nodal volume by analyzing fluorodeoxyglucose (FDG)-avid lymph nodes (LNs) on positron emission tomography/computed tomography (PET/CT) scans in patients with cervical cancer. Methods and Materials: We identified 72 PANs on pretreatment PET/CT of 30 patients with newly diagnosed stage IB-IVA cervical cancer treated with definitive chemoradiation. LNs were classified as left-lateral para-aortic (LPA), aortocaval (AC), or right paracaval (RPC). Distances from the LN center to the closest vessel and adjacent vertebral body were calculated. Using deformable image registration, nodes were mapped to a template computed tomogram to provide a visual impression of nodal frequencies and anatomic distribution. Results: We identified 72 PET-positive para-aortic lymph nodes (37 LPA, 32 AC, 3 RPC). All RPC lymph nodes were in the inferior third of the para-aortic region. The mean distance from aorta for all lymph nodes was 8.3 mm (range, 3-17 mm), and from the inferior vena cava was 5.6 mm (range, 2-10 mm). Of the 72 lymph nodes, 60% were in the inferior third, 36% were in the middle third, and 4% were in the upper third of the para-aortic region. In all, 29 of 30 patients also had FDG-avid pelvic lymph nodes. Conclusions: A total of 96% of PET positive nodes were adjacent to the aorta; PET positive nodes to the right of the IVC were rare and were all located distally, within 3 cm of the aortic bifurcation. Our findings suggest that circumferential margins around the vessels do not accurately define the nodal region at risk. Instead, the anatomical extent of the nodal basin should be contoured on each axial image to provide optimal coverage of the para-aortic nodal compartment.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

The Tumor Radiobiology of SRS and SBRT: Are More Than the 5 Rs Involved?

Stereotactic radiosurgery (SRS) and stereotactic body radiation therapy (SBRT), also known as stereotactic ablative radiation therapy (SABR), are rapidly becoming accepted practice for the radiation therapy of certain tumors. Typically, SRS and SBRT involve the delivery of 1 or a few large-dose fractions of 8 to 30 Gy per fraction: a major paradigm shift from radiation therapy practice over the past 90 years, when, with relatively large amounts of normal tissues receiving high doses, the goal was to maximize tumor response for an acceptable level of normal tissue injury. The development of SRS and SBRT have come about because of technologic advances in image guidance and treatment delivery techniques that enable the delivery of large doses to tumors with reduced margins and high gradients outside the target, thereby minimizing doses to surrounding normal tissues. Because the results obtained with SRS and SBRT have been impressive, they have raised the question whether classic radiobiological modeling, and the linear-quadratic (LQ) model, are appropriate for large doses per fraction. In addition to objections to the LQ model, the possibility of additional biological effects resulting from endothelial cell damage, enhanced tumor immunity, or both have been raised to account for the success of SRS and SBRT. In this review, we conclude that the available preclinical and clinical data do not support a need to change the LQ model or to invoke phenomena over and above the classic 5 Rs of radiobiology and radiation therapy, with the likely exception that for some tumors high doses of irradiation may produce enhanced antitumor immunity. Thus, we suggest that for most tumors, the standard radiobiology concepts of the 5 Rs are sufficient to explain the clinical data, and the excellent results obtained from clinical studies are the result of the much larger biologically effective doses that are delivered with SRS and SBRT.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Medical Student–Reported Outcomes of a Radiation Oncologist–Led Preclinical Course in Oncology: A Five-Year Analysis

Purpose: There is a recognized need for more robust training in oncology for medical students. At our institution, we have offered a core dedicated oncology block, led by a radiation oncologist course director, during the second year of the medical school curriculum since the 2008-2009 academic year. Herein, we report the outcomes of the oncology block over the past 5 years through an analysis of student perceptions of the course, both immediately after completion of the block and in the third year. Methods and Materials: We analyzed 2 separate surveys. The first assessed student impressions of how well the course met each of the course's learning objectives through a survey that was administered to students immediately after the oncology block in 2012. The second was administered after students completed the oncology block during the required radiology clerkship in the third year. All questions used a 5-level Likert scale and were analyzed by use of a Wilcoxon signed-rank test. Results: Of the 169 students who took the oncology course in 2012, 127 (75.1%) completed the course feedback survey. Over 73% of students agreed or strongly agreed that the course met its 3 learning objectives. Of the 699 medical students who took the required radiology clerkship between 2010 and 2013, 538 participated in the second survey, for a total response rate of 77%. Of these students, 368 (68.4%) agreed or strongly agreed that the course was effective in contributing to their overall medical education. Conclusion: Student perceptions of the oncology block are favorable and have improved across multiple categories since the inception of the course. Students self-reported that a dedicated preclinical oncology block was effective in helping identify the basics of cancer therapy and laying the foundation for clinical electives in oncology, including radiation oncology.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Coexistence of positive and negative exchange bias effect in Pr-doped NdCrO 3 samples

Positive and negative exchange bias effects are observed in Nd 1-x Pr x CrO 3 (0.00 ≤ x ≤ 1.00) polycrystalline samples. The shift of hysteresis loops, either opposing or following the direction of the field cooling, depends on the concentration of praseodymium. The temperature dependence of magnetization reveals a magnetic transition at T ≈ 220 K likely ascribed to the N é el temperature of Cr 3+ magnetic moments. The non-Kramer Pr 3+ ion seems to play an important role in the magnetic properties of this compound. In the range 0.00 ≤ x ≤ 0.60, all samples presented a decrease in the magnetization below TN and a clear compensation point. Pr-rich samples (x ≥ 0.70) show a paramagnetic-like behavior down to low temperatures. We report the most impressive result is the relation between reversal magnetization and the signal of exchange bias effect which seems be tuned by the Pr-doping.

36 MATERIALS SCIENCE↗

Defect engineering of mesoporous nickel ferrite and its application for highly enhanced water oxidation catalysis

Spinel nickel ferrite (NiFe 2 O 4 ) emerges as a promising low-cost catalyst for water splitting but it usually shows low catalytic activity because of its limited number of active sites and poor conductivity. For the first time, herein we have successfully overcome its weaknesses using defect engineering approach by creating oxygen vacancies in NiFe 2 O 4 . The existence of oxygen vacancy not only shifts up the d-band center, strengthens the adsorption of H 2 O, and thus provides more active catalytic sites, but also tunes the electron configuration and creates massive number of defective donor states in the band gap to facilitate charge transfer processes. The optimal defective catalyst showed significantly enhanced catalytic OER performance with an OER overpotential as low as 0.35 V at 10 mA cm -2 and a Tafel slope of only ~40 mV dec -1 . Moreover, the impressive specific mass and area current density of 17.5 A g -1 and 0.106 A m -2 at 1.58 V vs. Finally, RHE have been achieved, which are ~23 and ~36 times higher than that of defect-free counterpart, respectively.

36 MATERIALS SCIENCE↗

Synergistic double-atom catalysts of metal-boron anchored on g-C 2 N for electrochemical nitrogen reduction: Mechanistic insight and catalyst screening

The rational design of a novel catalytic center with a sound basis remains both challenging and rewarding for the electrochemical reduction of N 2 (eNRR), which has provided a feasible route for achieving clean and sustainable NH 3 production under ambient conditions. Herein, using density functional theory calculations, we demonstrate that hybrid metal (M)-boron (B) double-atom catalysts (DACs) embedded in g-C 2 N substrate (M-B@C 2 N, M = 3d, 4d and 5d transition metals) can achieve both high catalytic activity and high selectivity in eNRR. The proposed M-B@C 2 N DACs have exhibited impressive feasibility and stability thanks to the resilient and robust C 2 N substrate with abundant pyridinic N atoms distributed among right-sized pore structures. Our results reveal that like the metal center, the embedded B atom can actively involve in Ntriple bondN bond activation via π*-backdonation mechanism concomitant with the substantial charge transfer to adsorbed *N 2 , leading to sizable Nsingle bondN bond elongation. Accordingly, both adsorption energy and Nsingle bondN bond length of *N 2 can be employed as catalytic descriptors for predicting eNRR activity in terms of the limiting potentials (UL). Using high-throughput screening method, we found that six M-B@C 2 N candidates have stood out as the outstanding electrocatalysts for driving eNRR, namely, M = Ti (U L = 0 V), Mo (U L = 0 V), Nb (U L = -0.04 V), W (U L = -0.23 V), Zr (U L = -0.26 V), V (U L = -0.28 V). The underlying origin is attributed to the balanced and constrained N-affinity of M-B dual site working in synergy, which can thus be used as one important guide of catalyst design.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Additive manufacturing of AISI M2 tool steel by binder jetting (BJ): Investigation of microstructural and mechanical properties

The presented research demonstrates for the first time the successful processing of AISI M2 tool steel by binder jetting, a promising additive manufacturing technique capable of producing complex shapes with minimal residual stresses and isotropic properties. The optimal printing parameters were explored by varying processing parameters such as the binder saturation (45 %–105 %), binder set time (0 to 10 s), targeted bed temperature (50–60 °C), oscillator (2600–2750 rpm), recoater (20–28 mm/s), and roller speeds (200–300 rpm). Microstructural characterization and evaluation of mechanical properties of binder jetted parts were performed using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) to study their chemical composition, powder morphology, microstructure, carbide morphologies, relative density, hardness, compressive strength, and ductility. Two powder sizes (5 and 10 μm) were used, and sintering was performed at varying temperatures (1270, 1280, and 1300 °C) and durations (60 and 120 min), followed by a furnace, air, and water cooling. An optimum hardness of ~970 HV was obtained when parts were sintered at 1270 °C for 60 min, followed by water quenching. Impressive compressive strength of ~ 3580 MPa was observed in the sample sintered at 1280 °C for 60 min duration, followed by air cooling. Furnace-cooled parts showed the highest density of ~95 %, whereas the relative density of air- and water-cooled parts varied between ~91 to 93.50 %, respectively. The microstructure of sintered samples revealed the formation of M 6 C stable carbide, M 2 C metastable carbide, MC as a secondary carbide, and a-Fe matrix, which contributed to the observed increase in mechanical properties.

36 MATERIALS SCIENCE↗

An overview of the first principles studies of doped RE-TM5 systems for the development of hard magnetic properties

In this study, we compiled all the first principles calculations performed on RE-TM 5 (RE: rare earth, TM: transition metal) system to address the following question: Has everything been tried to improve the hard magnetic properties of this special intermetallic compound, and are there any venues that are worth pursuing? As it is the case with the first principles studies in any field, they are driven mainly by experimental work: (i) to validate their results, and (ii) to extend our understanding of the underlying physical phenomena so that the theory in hand can be used as a predictive tool to shed light on certain what-if scenarios. Our analysis indicates that three major compounds are investigated more than others: (1) YCo 5 , because it can potentially be an intermediate-performance hard magnet, and the presence of yttrium with no localized 4f electrons simplifies calculations significantly, (2) SmCo 5 , because it has the largest magnetic anisotropy energy among all RE hard magnets as well as very impressive high temperature performance, (3) CeCo 5 , because Ce is the most abundant rare earth element with a curious 4f electron behavior that gives rise to pronounced deviations in its structural and magnetic properties across the lanthanides series. This is followed by a brief analysis of several ab initio approaches that were developed to treat these rather complicated systems both at 0 K and at finite temperatures. Towards the end, we elucidate the role of exchange-correlation approximations such as local density approximations (LDA) and generalized gradient approximation (GGA) formulation in determining the MAE and M s by analyzing their corresponding density of states (DOS), and providing our results on a rather overlooked hard-magnetic material: LaCo 5 .

36 MATERIALS SCIENCE↗

Stored energy release in neutron irradiated silicon carbide

The purpose of this investigation is to experimentally quantify the stored energy release upon thermal annealing of previously irradiated high-purity silicon carbide (SiC.) Samples of highly-faulted polycrystalline CVD β-SiC and single crystal 6HSiC were irradiated in a mixed spectrum fission reactor near 60 °C in a fluence range from 5 × 10 23 to 2 × 10 26 n/m 2 (E > 0.1 MeV), or about 0.05–20 dpa, in order to quantify the stored energy release and correlate the release to the observed microscopic swelling, lattice dilation, and microstructure as observed through TEM. Within the fluence of this study the crystalline material was observed to swell to a remarkable extent, achieving 8.13% dilation, and then cross a threshold dose for amorphization at approximately 1 × 10 25 n/m 2 (E > 0.1 MeV) Once amorphized the material attains an as-amorphized swelling of 11.7% at this irradiation condition. Coincident with the extraordinary swelling obtained for the crystalline SiC, an equally impressive stored energy release of greater than 2500 J/g at the critical threshold for amorphization is inferred. As expected, following amorphization the stored energy in the structure diminishes, measured to be approximately 590 J/g. Generally, the findings of stored energy are consistent with existing theory, though the amount of stored energy given the large observed crystalline strain is remarkable. The overall conclusion of this work finds comparable stored energy in SiC to that of nuclear graphite, and similar to graphite, a stored energy release in excess of its specific heat in some irradiation conditions.

36 MATERIALS SCIENCE↗

Design considerations for high entropy alloys in advanced nuclear applications

The demanding operating environments of advanced nuclear reactors require the development of new nuclear materials that can withstand their increased physical, chemical, thermal, and radiation-related challenges. High-entropy alloys (HEAs) have shown often-impressive mechanical, thermomechanical, and corrosion-resistant properties, and offer a massive, unexplored compositional space which allows for the targeted development of application-specific materials. Furthermore, although still in a nascent stage, research has shown that HEAs may exhibit unique irradiation tolerance, including reduced defect production and resistance to irradiation-induced swelling and hardening. The mechanisms behind this increased tolerance are not yet well-understood, although the HEA-specific attributes of a complex energy landscape, reduced thermal conductivity, and shift in defect migration energies and pathways provide promising explanations. Here this work assesses the current and future challenges faced by structural nuclear materials, identifying the specific applications in which HEAs may provide a competitive advantage compared to industry-standard materials with the aid of Ashby material selection maps. Considerations are provided for the design of future nuclear HEAs, including calculations of nuclear-relevant properties to assist in the initial down-selection of elements depending on application requirements (e.g., low neutron capture for in-core applications), narrowing the existing compositional space of HEAs to a manageable scope.

36 MATERIALS SCIENCE↗

Ultraporous nitrogen-rich carbon nanosheets derived from the synergy of eutectic liquid and zeolitic imidazolate for energy applications

This report presents a unique and novel synthetic method for the preparation of highly porous nitrogen-rich carbon nanosheets from ZIF-8 (ZIF, zeolitic imidazolate framework) with the assistance of eutectic liquid. Due to the low melting temperature, a mixture of eutectic salts can provide a special atmosphere for the carbonization process and function as the template to support the ZIF-8 framework. The formation of the ultraporous nanosheets can be ascribed to the excellent miscibility between the eutectic salts and ZIF-8 framework, thus helping convert the ordered calcined intermediate species into extended carbon sheets at high temperature while inheriting the microporous structure from the prototypical ZIF-8. Furthermore, by controlling the ratio of eutectic liquid to ZIF-8 framework, the BET surface area of carbon nanosheets can be systematically tuned, with the highest BET surface area up to 2960 m 2 g -1 . In addition to this impressive high surface area, the pore size distribution follows well with the pristine ZIF-8. The nitrogen content varies from 9.9 wt. % to 13.4 wt. %. These characteristics contribute to the excellent performance of CO2 adsorption (5.45 mmol g -1 at 1atm and 273K) and oxygen reduction reaction (ORR) catalysis due to the large numbers of accessible active sites.

36 MATERIALS SCIENCE↗

Modeling assisted synthesis of Zr-doped Li 3-x In 1-x Zr x Cl 6 with ultrahigh ionic conductivity for lithium-ion batteries

All-solid-state lithium-ion batteries (ASSLBs) are an important milestone for the future of energy storage because of their capability of impressive energy density and outstanding safety. However, oxide and sulfide solid-state electrolytes (SSEs) suffer from either low ionic conductivity or poor chemical stability. In contrast, halide-based SSEs, are promising as candidate materials owing to high conductivity, good stability, and broad cathode compatibility. Though element doping of the SSEs is an effective and common approach to further improve their electrochemical properties, dopant exploration and optimization through solely experimental trials are both costly and time-consuming. For this aspect, computational simulations for dopant element and concentration screening are adopted in this research and zirconium is selected as a suitable dopant for Li 3 InCl 6 . Further, the synthesized Li 2.75 In 0.75 Zr 0.25 Cl 6 exhibited Li ionic conductivity of 5.82 x 10 -3 Scm -1 at room temperature, which is the highest among reported halide SSEs. The ASSLB formed with Li 2 CoO 2 -Li 2.75 In 0.75 Zr 0.25 Cl 6 -Li/In delivers a high initial capacity of 129.3 mAh∙g -1 . Conclusively, this work provides an effective approach which combines computational modeling and experimental verification for the development of halide SSEs with improved stability and conductivity. The successful design approach and compelling results provide further possibilities and capabilities in future SSE research.

25 ENERGY STORAGE↗

Recycled graphite enabled superior performance for lithium ion batteries

Recycling graphite attracts growing attention since cumulative amount of spent Li-ion batteries and the shortage of graphite supply chain. Although various recycling methods have been reported, the recycled graphite cannot reach the strict commercial standards of purity, scalability, efficiency, and capacity, preventing it from battery manufacturing. Herein, the important roles of defects and functional groups on the graphite surface are deeply studied, and a closed-loop graphite recycling process with the surface recovery and modification for the graphite from the end-of-life batteries is demonstrated. The recovered graphite delivers a purity of over 99.9 % and an average initial coulombic efficiency of 91.5 %. Compared with commercial graphite in industrial standard battery testing parameters, full cells with recovered graphite possess enhanced rate reversibility, doubled cycle life, over 10 % higher capacity along with half anode material cost. In conclusion, these impressive results not only underscore the transformative potential of surface reconstruction and modification in graphite recycling, but also present economic feasibility and sustainable pathway for significantly improving battery performance and addressing global resource challenges via integration with the hydrometallurgical recycling process.

25 ENERGY STORAGE↗

One-pot solvothermal synthesis of dual-phase titanate/titania Nanoparticles and their adsorption and photocatalytic Performances

Dual phase titanate/titania nanoparticles undergo phase transformation gradually with the increase of solvothermal synthesis temperature from 100 °C to 200 °C, and eventually are fully transformed into anatase TiO{sub 2}. The crystal structure change results in the changes of optical absorption, sensitizer/dopant formation and surface area of the materials which finally affect the overall dye removal ability. Reactions under dark and light have been conducted to distinguish the contributions of surface adsorption from photocatalytic degradation. The sample synthesized at 160 °C (S160) shows the best performances for both adsorption under dark and photocatalytic degradation of methylene blue (MB) under visible light irradiation. The adsorption mechanism for S160 is determined as monolayer adsorption based on the adsorption isotherm test under dark condition, and an impressive adsorption capacity of 162.19 mg/g is achieved. For the photocatalytic application, this sample at 0.1 g/L loading is also able to degrade 20 ppm MB within 6 hours under the visible light (>420 nm) condition. - Graphical abstract: The effect of solvothermal synthesis temperature on the formation and dye removal performance of dual phase titanate/titania nanoparticles was unveiled and optimized. - Highlights: • Low temperature one-pot solvothermal synthesis of dual-phase photocatalysts. • Correlation of the synthesis temperature is made with the phase composition. • Adsorption isotherm, kinetics, photocatalytic degradation were studied. • Synthesis at 160 °C yields the best material for adsorption of MB in dark. • The same sample also shows the best visible light degradation of MB.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗