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ChemistrySelect · 2024 ·Vol. 9 ·期 2 ·e202304152 · IF 1.9

Effect of synthesis medium and synthesis conditions on physicochemical properties of hierarchical SAPO-11 molecular sieve synthesized via fractional crystallization method

Xiaojun Dai,Yan Cheng,Tingting Liu,Lingjuan Mao

Graphical The effects of synthesis medium and synthesis conditions on the physicochemical properties of SAPO-11 molecular sieve were explored by combining the hydrothermal crystallization method with the fractional crystallization method. SAPO-11 molecular sieve has been widely used as the support of bifunctional catalyst for hydroisomerization of n-alkanes because of its mild acidity and unique one-dimensional pore structure, and has been widely used in industry. However, how to further improve and improve the physicochemical properties of SAPO-11 molecular sieve is still worth studying. In this work, fractional crystallization method was used to synthesize graded SAPO-11 molecular sieve. The effects of medium system, feed SiO 2 /Al 2 O 3 , crystallization time and crystallization temperature of the second crystallization process on the physicochemical properties of SAPO-11 molecular sieve were investigated from the perspectives of crystallinity, textural properties and acidity. The suitable synthesis medium and the best synthesis conditions were determined. It is expected to provide reference for the fractional crystallization synthesis of high performance SAPO-11 molecular sieve.

研究领域: 材料科学 · 化学工程 · 催化
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CRYSTENGCOMM · 2019 ·Vol. 21 ·期 9 ·1352-1357 · IF 3.382

A fractional crystallization technique towards pure mega-size CsPb2Br5 single crystal films

Jian Yin,Guodong Zhang,Xutang Tao

A facile fractional crystallization technique was developed to prepare single crystalline CsPb2Br5 films using water as the solvent, and the films can be easily transferred onto various substrates for the device fabrication. The obtained films can be up to 600 × 600 μm2 and decrease to 50 nm in thickness with high crystalline quality as well as temperature and air stability.

研究领域: 材料科学 · 晶体学 · 光电子器件
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CRYSTAL GROWTH & DESIGN · 2020 · IF 4.089

Low-Temperature Solution Growth and Characterization of Halogen (Cl, I)-Doped CsPbBr3 Crystals

Fangbao Wang,Hongjian Zhang,Qihao Sun,Ahmed Ben Hafsia,Zhangxuan Chen,Binbin Zhang,Yadong Xu,Wanqi Jie

The all-inorganic halide perovskite CsPbBr3 exhibited extraordinary photoelectric properties as well as great potential for various optic-electronic devices. The introduction of a Cl/I dopant is an effective method to optimize their properties. However, it is still a challenge to grow doped CsPbBr3 single crystals from solution. In this work, we report on the crystal growth of Cl/I-doped CsPbBr3 crystals using the modified inverse temperature crystallization (ITC) method. The components of raw materials and solvent in precursors were precisely tailored. The resulting doping ratio between the actual content and the nominal content are 0.99 and 0.046 for Cl and I, respectively. It indicates that I ion doped crystals exhibit more severe stoichiometric deviation due to the lower decomposition energy. The crystal structure, morphology, and optical properties of doped crystals were also investigated systematically. The {101} and {010} facets of as-grown crystals were influenced by the doping process. PL and UV transmittance spectra exhibited changes in the band gap in Cl/I-doped crystals. Finally, the phase diagram of basic photoelectric properties was determined for CsPb(Br1–nCln)3 crystals and it reveals conductive type changes from the P type to N type with an increase in the doping content of the Cl element. The optimum component of CsPb(Br0.93Cl0.07)3 demonstrates the highest resistivity of 4.3 × 109 Ω cm, an on/off ratio of ∼40, and a mobility of 414 cm2 V–1 s–1 as well as the lowest carrier concentration of 3.57 × 107 cm–3. Our work provides a strategy to grow doped halide perovskite crystals and tailor their optical and electrical properties.

研究领域: 材料科学 · 光学
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CRYSTAL GROWTH & DESIGN · 2024 · IF 3.2

Reverse Temperature Solution to Grow High-Quality CsCu2I3 Single Crystal with Formic Acid for Radiation Detection

Jianming Lai,Lujia Yang,Wenzhen Wang,Shaohan Wang,Yingshen Lu,Feng Hong,Fei Xu,Junfeng Chen,Yan Zhu,Hui Zhang,Run Xu,Linjun Wang

One-dimensional (1D) CsCu2I3 single crystals (SCs) have been investigated as novel sensitive X-ray and γ-ray scintillators, which can be prepared by the Bridgman method and solution method. However, to date, no research team has studied the scintillation performance of CsCu2I3 single crystals grown using the solution method, and traditionally grown single crystals using the antisolvent method are of poor quality and small sizes. In this work, high-quality CsCu2I3 SC was synthesized with formic acid as an additive by using the inverse temperature crystallization solution method, and its optical properties and scintillation performance were measured. The experimental results indicate that the addition of formic acid can stabilize the growth of crystals in solution, and the selected solvent DMF is beneficial for the growth of rod-like single crystals instead of needle-like single crystals by the DMSO. The experiment resulted in high-quality CsCu2I3 single crystals reaching a length of 13 mm, with no visible inclusions in the crystal. The full width at half-maximum (fwhm) of the X-ray rocking curve was 0.028°, indicating its high crystalline quality. It exhibits stability in air and emits bright yellow light under ultraviolet irradiation. The CsCu2I3 SC shows a much shorter PL decay of 118 ns and afterglow of 0.01% @ 12 ms compared to commercial CsI: Tl single crystal. The light yield of CsCu2I3 SC is 21800 photons/MeV, showing great potential as a scintillation material.

研究领域: 材料科学 · 物理学
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Energies · 2013 ·Vol. 6 ·期 7 ·3466-3480 · IF 1.844

Acetylene Black/Sulfur Composites Synthesized by a Solution Evaporation Concentration Crystallization Method and Their Electrochemical Properties for Li/S Batteries

Haibo Tan,Shengping Wang,Du Tao,Zhigao Yang

A novel technique to prepare carbon/sulfur composites as cathode materials for Li/S batteries is proposed, which we call the ‘solution evaporation concentration crystallization’ method. Three composites with different S loadings were prepared, subject to two different solvent evaporation rates from acetylene black (AB)/sulfur in carbon disulfide solutions. X-ray diffraction, environmental scanning electron microscopy, transmission electron microscopy, and Brunauer-Emmett-Teller measurements all show that the porous AB structure is well-filled with S. Composites prepared at a lower solvent evaporation rate with 50 wt % S content, had good electrochemical properties, with 1609.67 mAh g−1in the initial cycle and 1115.69 mAh g−1after 100 cycles. Composites with better dispersibility at a low solvent evaporation rate can effectively prevent polysulfide from dissolving in the electrolyte, and serve to stabilize the structure of the S cathode during the charge-discharge process.Keywords:sulfur/carbon composites;solution evaporation concentration crystallization method;lithium sulfur batteries

CAS / MDL: 7704-34-9
研究领域: 材料科学 · 电化学
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JOURNAL OF MOLECULAR LIQUIDS · 2024 · IF 5.3

Determination and correlation of the solubility of magnesium sulfate in ethanol solutions with different concentrations: Application to the removal of magnesium from zinc electrolytic waste solution

Yaoshan Li,Yuan Liu,Yuwei Cao,Huatai Wang,Kaitao Li,Yanjun Lin

In this study, the solubility of anhydrous magnesium sulfate (MgSO 4 ) in ethanol solutions with concentrations ranging from 10 % to 50 % was determined at 15–50 °C. Next, the results were correlated by using the Apelblat model, polynomial empirical equation, ideal solution equation of state model, and Van’t Hoff–Jouyban–Acree model. The results indicated that all four models exhibited correlation coefficients greater than 97 %, and average relative deviations of 3.82 %, 4.24 %, 3.96 %, and 3.96 %, respectively. Notably, the Apelblat model was found to be more accurate and reliable in correlating the solubility of MgSO 4 in ethanol solutions with different concentrations. Further, the Van’t Hoff equation was applied to determine the enthalpy and entropy of dissolution. Herein, a certain amount of anhydrous ethanol was added to the zinc (Zn) electrolytic waste solution (ZEWS) to crystallize Zn 2+ and Mg 2+ through the solvent crystallization method, with the precipitation rates reaching 20.13 % and 39.38 %, respectively. The concentration of Mg 2+ reduced to below 15 g⋅L −1 , meeting the quality standard of ZEWS. The XRD, TG, and SEM analyses of the output salt mix crystallization confirmed the primary components to be MgSO 4 ·7H 2 O and ZnSO 4 ·7H 2 O, with the morphological features primarily consisting of short rods and some crystal agglomerates. This study shows that the removal of Mg 2+ from Zn smelting process can be effectively achieved by the proposed solvent crystallization method.

研究领域: 化学工程 · 环境科学
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JOURNAL OF POROUS MATERIALS · 2024 · IF 2.5

Controlled synthesis of high performance SAPO-34 with sheet-like morphology and small particle size using concentrated gel system

Liang Ni,Wang Haiyan,Wang Yujia,Kang Lei,Bai Yingzhi,Sun Na

A strategy was devised for the synthesis of SAPO-34, which involved a concentrated gel system-assisted two-step crystallization method. This strategy effectively controlled the size and morphology of SAPO-34. The successful synthesis of SAPO-34 crystals with micron-scale cubic morphology and nano-scale sheets were achieved using triethylamine as a low-cost template. The paper thoroughly examined the growth evolution that occurs during the crystallization process, and it delved into the factors such as gel concentration and crystallization conditions in the synthesis. Furthermore, potential theories regarding nucleation and growth mechanisms were suggested. A systematic study was conducted to examine how the morphology and acidity of SAPO-34 zeolites impact their catalytic performance. The results confirmed that the SAPO-34 with low silicon content and lamellar structure was successfully synthesized through a two-step crystallization within a gel system of H 2 O/Al 2 O 3  = 30, with a thickness of approximately 50–300 nm. SAPO-34 nanosheets demonstrated a substantial enhancement in catalytic performance, with a catalytic life of 370 min and an 84.1% selectivity towards light olefins.

CAS / MDL: 121-44-8
研究领域: 材料科学 · 催化化学
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FUEL · 2025 · IF 7.5

Hydroisomerization performance of nanosized high-silica ZSM-48 catalysts synthesized via stepwise crystallization method

Wei Zhang,Yuting Wang,Jiangnan Xiang,Haiying Lu,Wenrui Jin,Yan Wang,Bo Qin,Weijiong Dai,Binbin Fan,Jiajun Zheng,Ruifeng Li

In this paper, a nanoparticle-stacked ZSM-48 molecular sieve is prepared by modifying the gel preparation process through stepwise crystallization. The corresponding bifunctional catalyst is developed for the hydroisomerization reaction of n -dodecane. The physicochemical properties of ZSM-48 are characterized and analyzed using XRD, SEM, NH 3 -TPD, N 2 adsorption–desorption and zero-length column (ZLC) method. The crystal size of Z-48-T2 synthesized via the stepwise synthesis method is reduced to as small as 0.6 μm, and its acidity is lower compared to that of Z-48-C. Meanwhile, Z-48-T2 exhibits the highest HF value and demonstrates excellent diffusion properties. Consequently, the Z-48-T2 catalyst shows superior catalytic activity and isomerization selectivity, achieving the highest iso -C 12 yield of 83.8 %. The outstanding diffusion performance of Z-48-T2 results in a monomethyl isomerization yield approximately 21 % higher than that of conventional ZSM-48 molecular sieves. Despite these improvements, the final mono-branched isomer product distribution remains unchanged, with 5-methylundecane being the predominant mono-branched isomer for both Z-48-T2 and Z-48-C.

CAS / MDL: 11138-49-1 18497-13-7
研究领域: 催化化学 · 材料科学
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CHEMISTRY OF MATERIALS · 2022 · IF 10.508

Precursor Engineering for Solution Method-Grown Spectroscopy-Grade CsPbBr3 Crystals with High Energy Resolution

Fangbao Wang,Ruichen Bai,Qihao Sun,Xin Liu,Yuanbo Cheng,Shouzhi Xi,Binbin Zhang,Menghua Zhu,Shuqing Jiang,Wanqi Jie,Yadong Xu

A CsPbBr3 single crystal exhibits great potentials in X-ray/gamma-ray spectroscopy and imaging. Here, an inverse temperature crystallization (ITC) method with modified precursor composition is proposed to prepare CsPbBr3 single crystals. The introduction of adduct PbBr2·2DMSO, synthesized by the antisolvent vapor-assisted crystallization method, in the precursor solution gives rise to superior crystallization with a lower impurity concentration and higher resistivity of 6.37 × 109 Ω·cm, as well as a higher hole mobility (50.7 cm2·V–1·s–1). Furthermore, a low dark current of 2.3 nA is obtained at a bias of −100 V based on an as-grown crystal with a thickness of 1 mm, according to the asymmetric Au/CsPbBr3/Sn structure. The resulting asymmetric planar detectors achieve the high peak-to-valley ratio pulse height spectra with an energy resolution of 7.66%, illuminated by an uncollimated 241Am@5.5 MeV α particle. Simultaneously, an energy resolution of 13.5% is realized when irradiated by a 59.5 keV 241Am γ-ray source at room temperature. The thermally stimulated current (TSC) spectra indicate that the density of deep energy-level trap is significantly reduced in the CsPbBr3 crystals grown by PbBr2·2DMSO-modified precursor solution, which is consistent with the high performance in radiation detection.

研究领域: 材料科学 · 物理化学 · 辐射探测技术
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JOURNAL OF POROUS MATERIALS · 2022 ·Vol. 29 ·期 5 ·1479-1487 · IF 2.523

Pd@silicate-1 synthesized by steam-assisted-crystallization strategy for high-efficient catalytic hydrogenation of furfural

Ye Tiantian,Liu Hanfang,Wang Fupeng,Xie Huijie,Ran Saisai,Xu Wei,Liu Jia,Li Bin,Lin Haifeng,Chai Yongming,Wang Lei

Here, we demonstrate a simple in situ synthesis of Pd@silicate-1 (S-1), using [Pd(NH 2 CH 2 CH 2 NH 2 ) 2 ]Cl 2 as a metal precursor and steam-assisted crystallization (SAC) method. The ultra-small Pd nanoparticles (NPs) (~ 1 nm) can be successfully in situ encapsulated into the silicate-1 matrix with well dispersion. The obtained Pd@S-1 catalyst possesses high crystallinity, a large specific surface area and pore volume. More importantly, Pd NPs encapsulated into silicate-1 matrix can avoid the aggregation and sintering during catalytic reaction. Meanwhile, micropores of silicate-1 can improve the selectivity of the products in the hydrogenation of biomass furfural. Consequently, Pd@S-1 catalyst shows excellent catalytic activity in the selective hydrogenation of biomass furfural with selectivity of 95.7% and activity of 83.7% in the condition of relatively low temperature (458 K). Therefore, this strategy provides a new idea for the synthesis of molecular sieve supported metal catalysts.

研究领域: 催化化学 · 材料科学
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CERAMICS INTERNATIONAL · 2024 · IF 5.1

Millimeter-scale Na2SiF6:Mn4+ red-emitting crystals with intense zero phonon line at 617 nm and enhanced hydrolysis resistance

Lulu He,Mingxin Zhang,Xiaoliang Dong,Liying Zhang,Ce Shi,Haipeng Ji

Macroscopic Mn 4+ -activated fluoride crystals can exhibit improved resistance to hydrolysis and higher quantum efficiency compared to their micro-sized powder counterparts. Among various Mn 4+ -doped fluorides, Na 2 SiF 6 :Mn 4+ is exceptional for its dominant photoluminescence at 627 nm, a notably short wavelength for this class of materials. While traditionally available only as micro-sized powder, this paper presents, for the first time, the growth of Na 2 SiF 6 :Mn 4+ in the form of millimeter-sized crystals. Utilizing a cooling-induced crystallization technique, we have obtained Na 2 SiF 6 :Mn 4+ crystals that exhibit columnar morphology with single-crystal-like characteristics and pronounced zero phonon line emission at 617 nm. The synthesis was meticulously optimized regarding the cooling protocol, cooling rate, and Mn 4+ doping concentration. With increasing dosage of K 2 MnF 6 in the precursor, a phase transformation from Na 2 SiF 6 :Mn 4+ to (Na,K) 2 SiF 6 :Mn 4+ and K 2 SiF 6 :Mn 4+ was observed for the product crystals. The incorporation of Mn 4+ was hindered during the cooling-induced crystallization of the crystals as the nominal Si/Mn concentration ratios significantly exceed the measured values. Comparison of the deterioration behavior in water suggests that the as-grown Na 2 SiF 6 :Mn 4+ crystals displayed significantly improved stability against water attack compared to the Na 2 SiF 6 :Mn 4+ powder phosphor. This work may inspire the development of more durable phosphor crystals for long-lasting white light LED technologies.

研究领域: 材料科学 · 光学工程
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Water · 2020 ·Vol. 12 ·期 4 ·946 · IF 2.544

The Recovery of Phosphorus from Acidic Ultra-High Phosphorous Wastewater by the Struvite Crystallization

Qiang Li,Song Wang,Lifang Wang,Li Zhang,Xiaohui Wan,Zhiguo Sun

Phosphorus recovery from industrial wastewater has attracted considerable interest. In this study, struvite crystallization method has been used for treatment of high phosphorus wastewater. The new combination agents of Mg5(CO3)4(OH)2·4H2O and NH4Cl were used as the precipitant. The effects of initial pH, n(Mg):n(P), n(N):n(P), and reaction time on the removal of total phosphorus (TP) in wastewater were investigated. The results showed that under the condition of initial pH = 4, Mg:N:P = 1.2:1.1:1, reaction time for 30 min, and static storage for 20 min, the residual amount of TP in wastewater was 2.98 mg /L, and the removal rate of TP reached 99.99%. The mass fraction of P2O5in the generated sediment reached 25.22%, equivalent to high grade phosphate ore and slow-release fertilizer, so as to realize the recycling and utilization of phosphorus in ultra-high phosphorous wastewater. This work will have practical application potential in treatment of high phosphorus wastewater and environmental management.Keywords:struvite crystallization method;environmental management;ultra-high phosphorus wastewater;basic magnesium carbonate;phosphorus recovery

CAS / MDL: 1066-33-7
研究领域: 环境工程 · 废水处理 · 资源回收
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