ANALYTICAL CHEMISTRY
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2019
·
IF 6.35
Heng Zhou,Feng Luo,Zhipu Luo,Dan Li,Cong Liu,Xueming Li
Microcrystal electron diffraction (MicroED) is becoming a powerful tool in determining the crystal structures of biological macromolecules and small organic compounds. However, wide applications of this technique are still limited by the special requirement for radiation-tolerated movie-mode camera and the lack of automated data collection methods. Herein, we develop a stage-camera synchronization scheme to minimize the hardware requirements and enable the use of the conventional electron cryo-microscope with a single-frame CCD camera, which ensures not only the acquisition of ultrahigh-resolution diffraction data but also low cost in practice. This method renders the structure determination of both peptide and small organic compounds at ultrahigh resolution up to ∼0.60 Å with unambiguous assignment of nearly all hydrogen atoms. The present work provides a widely applicable solution for routine structure determination of MicroED and demonstrates the capability of the low-end 120 kV microscope with a CCD camera in solving ultrahigh resolution structures of both organic compounds and biological macromolecules.
研究领域:
结构生物学
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生物物理学
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材料科学
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DOI
PubMed
高影响因子
Inorganic Chemistry Frontiers
·
2017
·Vol. 4
·期 10
·1654-1659
·
IF 4.036
Yilin Wang,Yunchen Wang,Jie Su,Xiaowei Song,Wei Wan,Jihong Yu
Silicogermanate (JU110) with an interrupted open-framework has been synthesized by using a hydrothermal method using 1,1′-(1,4-phenylenebis(methylene))bis(1-methylpyrrolidin-1-ium) hydroxide as an organic structure-directing agent (OSDA). Silicon and fluoride anions were introduced to the concentrated-gel synthesis system, and different synthetic parameters influencing the synthesis were discussed. The structure of JU110 was characterised by using rotation electron diffraction (RED) and high-resolution powder X-ray diffraction. JU110 crystallizes in the space group Fm2m (No. 42) with a = 13.9117(2) Å, b = 18.2980(3) Å and c = 32.7800(6) Å. The structure is constructed by the sti layers found in the STI framework that are pillared by D4R/Ge7 units to form a large cavity, showing 10-ring openings along [100] and 9-ring openings along [110]. Thermal stability studies showed that the framework was maintained with the loss of water molecules, but collapsed with the removal of charge-compensating cations.
研究领域:
材料科学
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晶体学
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DOI
高影响因子
Journal of the American Chemical Society
·
2025
·
IF 15.6
Chenyang Nie,Yuanhao Li,Xiaona Liu,Nana Yan,Chao Ma,Jiahui Zhu,Linlin Hao,Peng Guo,Zhongmin Liu
Small-pore aluminophosphate (AlPO) molecular sieves (MSs), particularly those in the ABC-6 family, have gained significant attention for their unique capabilities in selective adsorption and energy storage. However, developing new synthesis strategies for designing AlPOs with three-dimensional (3D) channel systems and determining the structures of nanosized novel AlPO MSs remain challenging tasks. In this study, we introduce a new small-pore AlPO with a 3D channel system, named DNL-17, synthesized by using a diquaternary ammonium compound as an organic structure-directing agent (OSDA). Its crystallographic structure was determined through advanced 3D electron diffraction (ED) techniques and further confirmed by emerging integrated differential phase contrast imaging. DNL-17 exhibits a remarkable 24-layer stacking sequence along the c-axis and features a variety of composite building units (CBUs), including d6r, can, cha, and eri. Significantly, a combination of 3D ED, theoretical calculations, and solid-state 13C NMR reveals that the employed OSDA adopts distinct conformations to stabilize different cages. This finding highlights a novel strategy for constructing AlPO MSs with diverse cage-based CBUs. Furthermore, DNL-17 demonstrates unique selective adsorption properties, particularly in the separation of n-butane and isobutane.
研究领域:
材料科学
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化学
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DOI
PubMed
高影响因子
Nature Chemistry
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2025
·
IF 20.2
Hu Junyi,Dong Zhuoya,Chu Chaoyang,Ma Yanhang
Chirality in crystalline materials is a fundamental feature that has a dramatic influence on their properties. Yet, the quantitative determination of the ratio between two enantiomorphic crystals in chiral solids remains challenging. Here we present the quantitative analysis of chiral nanocrystals through a method based on three-dimensional electron diffraction. We developed a dual tilt-scan protocol for tomography data collection in both real and reciprocal space, determining the absolute structure and estimating the crystal volume. Combined with automated serial data collection from hundreds of nanocrystals, this strategy allows high-throughput chirality determination, as well as the overall enantiomorphic excess. The successful application of this method to chiral inorganic nanocrystals reveals the role of chiral ligands in the bias of two enantiomorphic structures. We further demonstrated the robustness of this method on one chiral drug, cinchonine, offering a transformative approach to studying chiral organic materials when they are not enantiopure.
研究领域:
材料科学
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结构化学
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纳米科技
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药物晶体学
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物理化学
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DOI
PubMed
高影响因子
POLYMER TESTING
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2018
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IF 2.247
Yue Zheng,Xiao Liu,Fengquan Liu,Jinxin Xue,Jianjun Zhou,Hong Huo,Lin Li
Poly(butylene succinate- co -butylene fumarate) (PBSF) copolymers with butylene fumarate (BF) molar ratio varies from 1% to 40% were synthesized and their single crystals were prepared using a self-seeding method. For PBSFs with low content of BF units, the single crystals are regular hexagonal shape. With the increase of BF molar ratio, the single crystal boundary turns rounded and the aspect ratio decreases. PBSF single crystals with different BF content were prepared at the same temperature, the supercooling degree of the PBSF increases with the increase of BF content, resulting the crystalline density increases and the single crystal size decreases. Selected area electron diffraction (SAED) was used to investigate the crystalline structures of the PBSF single crystals, and the results approve strict isomorphism between butylene succinate (BS) and BF in PBSF, verifying that preparing the single crystal and characterizing the crystalline structure by SAED is a direct method to check for isomorphic polymers. PBSFs can form ring-band spherulites at suitable crystallization temperatures . The band spacing of PBSF increases with the increase of isothermal crystallization temperature. At the same isothermal crystallization temperature, the band spacing PBSF decreases with the increase of BF molar ratios. The crystallization temperature range of forming ring-banded spherulites broadens with the increase of BF molar ratios.
研究领域:
材料科学
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高分子化学
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DOI
高影响因子
Frontiers in Molecular Biosciences
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2022
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IF 6.113
Chen Pohua,Liu Yang,Zhang Chaochao,Huang Fei,Liu Leifeng,Sun Junliang
The crystalline sponge method has shown to be a novel strategy for the structure determination of noncrystalline, oily, or trace amount of a compound. A target compound was absorbed and oriented orderly in the pregrown porous crystal for x-ray diffraction analysis. However, the diffusion in the micron-sized crystals is rather difficult. Lots of trial-and-error experiments are needed to optimize the guest-soaking process and to improve data quality. Nanocrystals are better in diffusion, yet it could not conduct a single crystal x-ray diffraction (SCXRD) analysis. Three-dimensional electron diffraction (3D-ED) is a powerful diffraction tool for the structure determination of small crystals. In this work, we successfully carried out the crystalline sponge method by 3D-ED technique using {(ZnI2)3-[2,4,6-tris(4-pyridyl)-1,3,5-triazine]2·x(guest)}n (1-Guest) porous complex nanocrystals. On account of the better diffuse ability of nanocrystals, the time needed for solvent exchange and guest soaking protocols are shortened 50-fold faster versus the original protocol. The crystal structure of the crystalline sponge incorporated with three different guests was fully resolved using a merged dataset. The structure model was identical to previously reported ones using x-ray, showing that the accuracy of the 3D-ED was comparable with SCXRD. The refinement results can also give the precise occupancy of the guest molecule soaked in the porous crystal. This work not only provides a new data collection strategy for crystalline sponge method but also demonstrates the potential of 3D-ED techniques to study host-guest interaction by solving the fine structure of porous material.
研究领域:
结构生物学
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材料科学
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化学晶体学
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产品关联
DOI
PubMed
高影响因子
Crystals
·
2023
·Vol. 13
·期 8
·1201
·
IF 2.7
Junkai Li,Donghan Jia,Guoliang Niu,Peiyang Mu,Huiyang Gou
Hexagonal boron nitride (h-BN) exhibits interesting optical and mechanical properties, including chemical and thermal stability. Extensive techniques have been applied for the realization of h-BN at high temperatures. Here, we propose a room-temperature preparation of h-BN at high pressure through the compression of ammonium azide and boron powder. The structure and morphology of the obtained h-BN are found to possess tubular-like features, and the selected-area electron diffraction and electron energy-loss spectroscopy support the formation of h-BN. Remarkably, h-BN grows gradually from the surface of boron particles to form a core–shell structure. This tubular morphology of h-BN with a size of 70 nanometers in length and 27 nanometers in width differs from the conventional lamellar h-BN generated with temperature assistance. Our results demonstrate a method for the room-temperature synthesis of tubular h-BN, which shows great promise for the preparation of other nitrides at high pressure and room temperature.Keywords:high-pressure synthesis;chemical reaction;hexagonal boron nitride
研究领域:
材料科学
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化学
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纳米技术
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DOI
高影响因子
APPLIED SURFACE SCIENCE
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2024
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IF 6.3
Jianhong Zhang,Junjie Yan,Zhikang Ao,Wei Li,Wei Wang,Yinong Lyu,Huifang Ma
The heterostructure moiré superlattice plays a crucial role in modulating electronic and optical properties through the formation of periodic potential patterns. However, the synthesis of ultrathin 2D heterostructures remains a significant challenge. In this work, ultrathin 2D CoSe/WSe 2 heterostructures were grown via a two-step vapor deposition route. The thickness of nonlayered hexagonal CoSe nanosheets was reduced to 1.7 nm through growth on a 0.79 nm thick WSe 2 nanosheet. Raman spectroscopy analyses indicate the formation of high-quality 2D CoSe/WSe 2 heterostructures. Selected area electron diffraction studies conclusively validate the high-quality single-crystal nature of CoSe and WSe 2 nanosheets within the resultant heterostructures. Scanning transmission electron microscopy studies show that the formed heterostructure exhibits a well-defined moiré superlattice with a periodicity of ∼ 3.96 nm. Additionally, the device based on CoSe/WSe 2 heterostructures with CoSe contacts demonstrates relatively higher on-state current and field-effect mobility compared to the WSe 2 device with Cr/Au contacts. The developed synthesis method for ultrathin CoSe/WSe 2 heterostructures provides a material platform for investigating their diverse properties.
研究领域:
材料科学
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纳米技术
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固体物理
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半导体器件
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产品关联
DOI
高影响因子
CERAMICS INTERNATIONAL
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2021
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IF 4.527
Shengtai Zhang,Lingkun Wang,Baoliang Xu,Jian Liu,Shilin Luo,Shiyin Ji,Yi Ding,Ling Zhang,Jianjun Ma,Tao Duan
The garnet structure is a promising solid material for nuclear waste because it can contain all kinds of actinides. Yttrium iron garnet Y 3 Fe 5 O 12 (YIG) is the model component of this kind of substitute. In this study, Nd-doped YIG ceramic samples were prepared by microwave sintering at different sintering temperatures (1100 °C, 1200 °C, and 1300 °C) for different sintering time (0.5 h, 2 h, 4 h, and 6 h). The effects of synthesis temperature and sintering time on the solubility and microstructure of Y 3-x Nd x Fe 5 O 12 (0 ≤ x ≤ 3.0) were evaluated. The X-ray diffraction (XRD), scanning electron microscopy (SEM) and backscattering scanning electron microscopy (EBSD) results show that single phase garnet structure can be synthesized and enhanced solubility of Nd in YIG was found at higher temperatures. The solubility of Nd in garnet is 50 mol% (x = 1.5) and 60 mol% (x = 1.8) at 1200 °C and 1300 °C, respectively. There is no significant dependence of the solubility on sintering time. The SEM analysis and Archimedes drainage test show that the relative density of Y 1.2 Nd 1.8 Fe 5 O 12 ceramics is 88.15% and 99.94% at 0.5 h and 6 h, respectively, indicating dense YIG could be obtained with a relatively long sintering time. The results show that microwave sintering can rapidly and efficiently synthesize the YIG ceramic samples.
研究领域:
材料科学
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核废料管理
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陶瓷
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产品关联
DOI
高影响因子
JOURNAL OF ALLOYS AND COMPOUNDS
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2017
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IF 3.133
Bo Huang,Hsueh-Liang Chu,Moo-Chin Wang,Cheng-Li Wang,Weng-Sing Hwang,Chao Liu,Horng-Huey Ko,Xiujian Zhao
Crystallization kinetics evaluated by the modified formula and optical properties of CdO and ZnO in 0.5ZnO-0.5CdO thin films have been investigated. The characterization used grazing incidence X-ray diffraction (GIXRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution TEM (HRTEM) and ultraviolet–visible (UV–Vis) spectrophotometry. When the thin films are annealed at temperatures from 573 K to 773 K for 10–60 min, the GIXRD results show that all the films are composed of CdO and ZnO as major and second phases, respectively. In addition, a trace phase of CdSiO 3 appeared for thin films annealed at 723 K and 773 K for 45 and 60 min, respectively, while CdSiO 3 also appeared when annealing at 773 K for 30 min. The crystallinity of CdO increases with annealing temperature and duration, whereas the crystallinity of ZnO increases only slightly with temperature and duration. The activation energies of ZnO and CdO crystallization in 0.5ZnO-0.5CdO thin films are 49.51 kJ/mol and 112.45 kJ/mol, respectively. The crystallization of CdO and ZnO can be described by a modified formula: ln ( 1 1 − α ′ ) = [ 30 t × exp ( − 49.51 × 10 3 R T ) ] 0.24 and ln ( 1 1 − α ′ ) = [ 104820 t × exp ( − 112.45 × 10 3 R T ) ] 0.27 , for 573 K ≤ T ≤ 773 K and 10 min ≤ t ≤ 60 min, respectively. All films have an average optical transparency of nearly 80% in the wavelength range greater than 500 nm in the visible range, and the band gap energy of the thin films increases from 2.68 eV to 3.10 eV as the crystallinity of ZnO increases from 5.12% to 20.91% when the thin films are annealed for 60 min at 573 K–773 K and shows a blueshift effect.
研究领域:
材料科学
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固体物理学
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光学
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DOI
高影响因子
Nanoscale
·
2013
·Vol. 5
·期 22
·10982-10988
·
IF 6.233
Lijian Chen,Kaifang Sun,Peipei Li,Xianzhong Fan,Jianchao Sun,Shiyun Ai
LDH nanosheets were obtained via continuous impaction and exfoliation by herring sperm DNA molecules using a constant vibration method. DNA–LDH nanohybrids were composed by electrostatic forces and they exhibited DNA-enhanced peroxidase-like activity. The morphology and structure of DNA–LDH nanohybrids were analyzed by transmission electron microscopy (TEM), selected-area electron diffraction (SAED), X-ray diffraction (XRD), and atomic force microscopy (AFM) characterization. On the basis of the high catalytic activity of DNA/CuAl–LDH nanosheets, a rapid, sensitive, and convenient approach was developed for colorimetric detection of H2O2 and blood glucose. This method can be potentially applied in medical diagnostics and biotechnology fields.
研究领域:
纳米技术
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生物传感器
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催化
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材料科学
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医学诊断
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产品关联
DOI
PubMed
高影响因子
ACTA PHYSICO-CHIMICA SINICA
·
2017
·Vol. 33
·期 5
·993-1000
·
IF 0.767
YANG Kun,YAO Qi-Lu,LU Zhang-Hui,KANG Zhi-Bing,CHEN Xiang-Shu
Noble-metal-free CuMo nanoparticles (NPs) without surfactant or support have been facilely prepared using NaBH4 as a reducing agent. The as-prepared CuMo nanocatalysts were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution
transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), inductively coupled plasma-atomic emission spectroscopy (ICP-AES), X-ray photoelectron spectroscopy (XPS), and Brunauer-Emmett-Teller (BET) surface area measurements, and used as catalysts for the hydrolysis
of ammonia borane (AB, NH3BH3) at room temperature. The as-synthesized Cu0.9Mo0.1 NPs exhibited a high activity towards the hydrolysis of AB with a turnover frequency (TOF) of 14.9 min-1, a higher value than that reported for Cu catalysts.
Our synthesis is not limited to CuMo NPs alone, but can easily be extended to CuW (3.6 min-1), CuCr (2 min-1), NiMo (55.6 min-1), and CoMo (21.7 min-1) NPs, providing a general approach to Cu-M (M = Mo, W, Cr) and TM-Mo (TM = Cu, Ni, Co) NPs as a
series of novel catalysts for the hydrolysis of AB. The enhanced activity of bimetallic NPs may be attributed to the synergistic effects of the Cu-M NPs induced by the strain and ligand effects.
研究领域:
催化
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材料科学
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纳米技术
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化学工程
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）