CERAMICS INTERNATIONAL
·
2019
·
IF 3.45
Mithun Nath,Shengqiang Song,Hang Liu,Yawei Li
Despite huge potential, Al 2 O 3 –CaO–Cr 2 O 3 system has been one of the least investigated one due to the generation of carcinogenic and toxic Cr(VI) compounds. Herein, we investigated the system under air atmosphere varying Cr 2 O 3 while keeping Al 2 O 3 :CaO ratio constant in order to identify the Cr(VI) dominant region, eventually to avoid it. The Ca 4 Al 6 Cr VI O 16 phase predominantly formed in the air atmosphere with Cr 2 O 3 content up to ∼12 mol%. However, an unprecedented Cr(III) phase appeared under air at higher Cr 2 O 3 content (26.43 mol%). We then synthesized the new polycrystalline ternary Cr(III) compound (CaAl 2 Cr 2 O 7 ) at 1500 °C under air atmosphere for the first time. A trigonal symmetry of hexagonal crystal family with space group P3 (143), lattice parameters a = b = 7.7909 Å and c = 7.6506 Å were determined from the X-ray powder diffraction pattern study. Electron microscope studies revealed uniform hexagonal microcrystals with similar lattice parameters. Most significantly, the binding energies of 586.1 and 576.2 eV for Cr2p 1/2 and Cr2p 3/2 respectively implied the +3 oxidation state of Cr in this compound.
研究领域:
材料科学
·
化学
✓ 已验证
产品关联
DOI
高影响因子
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE
·
2016
·Vol. 642
·期 3
·255-259
·
IF 1.261
Luzia S. Germann,Robert E. Dinnebier,Xin Liu,Yaping Dong,Wu Li
Anhydrous zinc hydroxide sulfates are promising precursors for the preparation of pigments and ZnO nanomaterials. The crystal structure of one such compound 5[Zn(OH) 2 ] · 2[ZnSO 4 ] was determined from high resolution laboratory X-ray powder diffraction data by use of a combination of charge flipping, 18 simulated annealing, 26 and difference Fourier analysis. The material crystallizes in the space group P with the lattice parameters of a = 5.4559(2) Å, b = 8.0528(3) Å, c = 8.9275(3) Å, α = 112.697(2)°, β = 85.219(3)°, γ = 95.441(3)°, and a volume of V = 359.76(2) Å 3 . The basic crystal structure consists of brucite type Zn(OH) 2 layers where every sixth octahedral site is vacant. Tetrahedrally coordinated zinc ions are located above and below these vacancies and consecutive layers are bridged by sulfate molecules. The composition of this layered structure can be written as [Zn 5 VI □(OH) 4 · Zn 2 IV (OH) 6 · (SO 4 ) 2 ]. Its thermal decomposition was studied by X-ray powder diffraction and thermal analysis.
研究领域:
材料科学
·
化学
✓ 已验证
DOI
高影响因子
Engineering
·
2022
·
IF 12.834
Xiaoping Wang,Weiwei Dong,Peng Zhang,Haoqi Tang,Lanting Zhang,Tieying Yang,Peng Liu,Hong Wang,X.-D. Xiang
High-throughput powder X-ray diffraction (XRD) with white X-ray beam and an energy-dispersive detector array is demonstrated in this work on a CeO 2 powder sample on a bending magnet synchrotron beamline at the Shanghai Synchrotron Radiation Facility (SSRF), using a simulated energy-dispersive array detector consisting of a spatially scanning silicon-drift detector (SDD). Careful analysis and corrections are applied to account for various experimental hardware-related and diffraction angle-related factors. The resulting diffraction patterns show that the relative strength between different diffraction peaks from energy-dispersive XRD (EDXRD) spectra is consistent with that from angle-resolved XRD (ARXRD), which is necessary for analyzing crystal structures for unknown samples. The X-ray fluorescence (XRF) signal is collected simultaneously. XRF counts from all pixels are integrated directly by energy, while the diffraction spectra are integrated by d -spacing, resulting in a much improved peak strength and signal-to-noise (S/N) ratio for the array detector. In comparison with ARXRD, the diffraction signal generated by a white X-ray beam over monochromic light under the experimental conditions is about 10 4 times higher. The full width at half maximum (FWHM) of the peaks in q -space is found to be dependent on the energy resolution of the detector, the angle span of the detector, and the diffraction angle. It is possible for EDXRD to achieve the same or even smaller FWHM as ARXRD under the energy resolution of the current detector if the experimental parameters are properly chosen.
研究领域:
材料科学
·
物理学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHEMICAL AND ENGINEERING DATA
·
2022
·
IF 3.119
Guangyu Xu,Fanyuan Zhang,Zhenghui Li
In this study, the solubility of 5-chloropyrazin-2-amine in four aqueous solutions (methanol, ethanol, n-propanol, and ethylene glycol (EG)) plus water was determined by a gravimetric method at temperatures ranging from T = 278.15 to 323.15 K at 101.2 kPa pressure. Experimental results indicated that 5-chloropyrazin-2-amine solubility positively increased with increasing temperature at a given solvent composition and decreased with increasing mass fraction of water in each system. The order of solubility from high to low on the mole fraction scale was as follows: methanol (0.02007, 323.15 K) > ethanol (0.01308, 323.15 K) > n-propanol (3.827 × 10–3, 323.15 K) > water (1.569 × 10–3, 323.15 K). Similarly, the solubility of 5-chloropyrazin-2-amine was higher in (methanol + water) than in the other three cosolvent mixtures. The solid phase crystal of 5-chloropyrazin-2-amine was tested by X-ray powder diffraction (XPRD) and the results showed no polymorphic transformation, solvate formation, or crystal transition during entire experiments. The experimental solubility values of 5-chloropyrazin-2-amine were correlated by three thermodynamic models. The results show that the largest relative average deviation (RAD) and root mean square deviation (RMSD) data were no more than 5.38% and 2.34 × 10–4, respectively. The Jouyban–Acree model gave the best correlation result in this study.
研究领域:
化学工程
·
药学
·
物理化学
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产品关联
DOI
高影响因子
MOLECULES
·
2023
·Vol. 28
·期 4
·1609
·
IF 4.6
Ruiqi Wang,Haichang Zhou,Shiyu Liao,Qi Tian,Zhengbing Lv,Kangde Bao,Lili Liu
During the trial production of Armillarisin A for injection (AA-I), unidentified needle-like yellow-brown crystals were occasionally observed. Here, we report an ultra-high performance liquid chromatography–tandem mass spectrometry (UPLC-MS) method for determining the source of the visible foreign bodies in the formulations of Armillarisin A active pharmaceutical ingredient (AA-API). AA-API, photolyzed samples, the intermediate polymer, and the excipient analyzed determined after the separation on a Waters Symmetry C18 (3.5 μm, 4.6 × 75 mm) column with a mobile phase consisting of a methanol/acetic acid (0.1 mol/L) aqueous solution (50:50). Furthermore, the crystal type of the visible foreign bodies, the intermediate polymer and AA-API were investigated by X-ray powder diffraction (XRD). The results revealed that the characteristics of the visible foreign solids were the same as those of AA-API as regards UPLC peak position (368 nm) and MS spectrum in negative ion detection mode. The visible foreign solids were thus identified as unpolymerized crystals of AA-API and were attributed to AA-API itself. The results showed that the production process could be improved by changing the stirring method and frequency as well as by optimizing the polymerization temperature to ensure the safety, stability, and control of the product quality in the stage of batch production.Keywords:Armillarisin A injection;visible foreign matter;ultra-high performance liquid chromatography–tandem mass spectrometry;X-ray powder diffraction
研究领域:
药学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
Journal of Materials Chemistry A
·
2020
·Vol. 8
·期 40
·21265-21272
·
IF 11.301
Lei Gao,Hao Zhang,Yuechao Wang,Shuai Li,Ruo Zhao,Yonggang Wang,Song Gao,Lunhua He,Hai-Feng Song,Ruqiang Zou,Yusheng Zhao
Sodium-rich antiperovskite (NaRAP) ionic conductors have been considered promising inorganic electrolytes for all-solid-state sodium batteries due to their low fabrication cost, high sodium ionic conductivity and good structural tolerance. The high structural flexibility of NaRAPs allows variety of chemical substitutions to improve conductivity; in particular, the substitution of the anion cluster has effectively proved promoting Na+ migration, both experimentally and theoretically. Herein, we report an unexpected boost in Na+ ionic conductivity that climbs to 0.37 mS cm−1 at 485 K by introducing NO2− groups in the antiperovskite Na3ONO2 system. Its mechanism was fully investigated by neutron powder diffraction and DFT calculations, proving that the NO2− group on the lattice center, can utilize its terminal O2− anion to facilitate the Na+ migration via the Na–O interaction, when thermally excited at 485 K. The detailed migration path is also discussed by both maximum entropy method (MEM) and DFT calculations.
研究领域:
材料科学
·
固态离子学
·
无机化学
·
能源材料
·
计算材料学
✓ 已验证
DOI
高影响因子
Energy Storage Materials
·
2023
·
IF 20.4
Zhewen Ma,Zhongyuan Huang,Zhao Li,Guojie Chen,Yinghui Li,Wen Zhu,Wenguang Zhao,Haocheng Ji,Hui Fang,Wen Wen,Wen Yin,Jianxin Zou,Yinguo Xiao
In this study, ultrafine Mg(In) solid-solution particles were successfully prepared through an arc plasma method and their deuterium uptake/release performances were systematically estimated with respect to the identically processed pure Mg particles. Thermodynamic destabilization and kinetic enhancement of Mg-In-D system were achieved simultaneously with lower deuterium ab/desorption enthalpies and decreased desorption temperatures. For the first time, an in-situ synchrotron X-ray diffraction (ISXRD) coupled with neutron powder diffraction (NPD) technique and density functional theory (DFT) calculations clearly substantiated that an indium diffusion-dominated phase transition is the driving force for the evolution from mixture of MgD 2 and Mg-In intermetallic to Mg-based solid solution during the deuterium release (DR). The ISXRD results clarified the real-time phase transition from MgIn to Mg 3 In at 515 K and the interreaction of MgD 2 and Mg 3 In at 640 K, by which the matrix could be destabilized to trigger an indium-diffusion governed DR reaction in deuteride. Moreover, with the aid of NPD experiment, the microstructure evolution of Mg-In-D system demonstrated the continuous diffusion of indium into Mg/MgD 2 upon desorption. The solubilized indium in MgD 2 effectively reduced the D -migration energy barrier and stabilized the lattice structure to restrain the constriction of Mg-D bonds, through which the noticeable improvement on both thermodynamic and kinetic performances of the Mg-In system was achieved. The combination of synchrotron X-ray and neutron diffraction offers a high-efficiency strategy to fathom the hydrogen discharging mechanism from the viewpoint of real-time phase transitions and crystalline structure evolutions.
研究领域:
材料科学
·
物理化学
✓ 已验证
DOI
高影响因子
ADVANCED FUNCTIONAL MATERIALS
·
2025
·
IF 19
Lei Gao,Zhigang Zhang,Zheyuan Zhang,Yongrui Luo,Bolong Hong,Longbang Di,Haijin Ni,Jinlong Zhu,Ruqiang Zou,Enyue Zhao,Songbai Han
The halide solid-state electrolyte (SSE) Li 2 ZrCl 6 has emerged as a promising candidate for all-solid-state batteries (ASSBs) due to the abundance of Zr in the Earth's crust and its low cost. However, its relatively low ionic conductivity prevents it from meeting the essential performance threshold (> 1 mS cm −1 ) required for application in ASSBs. In this work, a novel strategy is presented to enhance ionic conductivity by incorporating high-valence Ta 5+ into the Li 2 ZrCl 6 framework, resulting in a series of Li-deficient Li 2– x Ta x Zr 1– x Cl 6 (LTZC, 0 ≤ x ≤ 0.4) SSEs. Remarkably, the LTZC ( x = 0.275) achieves a high ionic conductivity of 1.43 mS cm −1 at 30 °C, surpassing that of Li-rich Li 2 ZrCl 6 -based SSEs (e.g., Li 2+2 x Zr 1– x Mg x Cl 6 ). Neutron powder diffraction reveals a pronounced rearrangement of Li + ions upon Ta 5+ doping, and bond-valence site energy calculations indicate that this rearrangement enhances Li + transport within the lattice. Furthermore, ASSBs incorporating LTZC SSE with LiCoO 2 or LiNi 0.8 Co 0.1 Mn 0.1 O 2 cathode and Li-In anode exhibit excellent cycling performance. This work underscores the effectiveness of structural regulation in developing Li-deficient halide SSEs as a viable strategy for enhancing their electrochemical performance.
研究领域:
材料科学
·
电化学
·
储能
·
固态离子学
✓ 已验证
产品关联
DOI
高影响因子
Pharmaceutics
·
2025
·Vol. 17
·期 12
·1543
·
IF 5.5
Han Gao,Jun Ouyang,Zhi-Bo Hu,Wei-Jie Fang
Background : Despite the growing importance of polypeptide-based drugs in clinical therapy, studies investigating the stability of their freeze-dried formulations remain scarce. Crystalline excipients, such as mannitol, are commonly used in freeze-dried formulations of chemically synthesized drugs, but they often negatively impact the long-term stability of biological macromolecules like monoclonal antibodies (mAbs). This study bridges this knowledge gap by evaluating the effects of crystalline and amorphous excipients, surfactants, and amino acid-based stabilizers on the long-term stability of freeze-dried formulations using model polypeptides, glucagon and insulin. Methods : The freeze-dried formulations were prepared with crystalline and amorphous excipients, surfactants, and amino acid-based stabilizers. The crystallization behavior of the excipients and the thermal stability of the formulations were thoroughly characterized using X-ray powder diffraction (XRPD) and differential scanning calorimetry (DSC). Results : The crystallization of mannitol was directly correlated with a significant reduction in the long-term stability of both model polypeptides. This detrimental effect mirrors the instability observed in mAbs formulations, indicating a common mechanism of protein destabilization induced by crystalline excipients, independent of molecular size. Conclusions : This study provides the first direct evidence that crystalline excipients pose a significant risk to the stability of freeze-dried polypeptides. These findings offer critical insights for the rational design of stable freeze-dried formulations, guiding industrial development strategies for polypeptide-based therapeutics.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
DALTON TRANSACTIONS
·
2023
·Vol. 52
·期 21
·7322-7329
·
IF 4
Chengyu Zhuo,Zeyu Lyu,Dashuai Sun,Sida Shen,Taixing Tan,Shuai Wei,Zhijun Li,Pengcheng Luo,Hongpeng You
Na2MgScF7 (NMSF) was experimentally obtained for the first time by combining hydrothermal and high-temperature solid-state reactions. X-ray powder diffraction (XRD) combined with Rietveld refinement confirms that NMSF is crystallized in the space group Imma with the cell parameters a = 10.40860(18), b = 7.32804(12) and c = 7.52879(11) Å, α = β = γ = 90° and V = 574.256(24) Å3. Through doping with Tb3+ or Eu3+ ions, downshifting yellow-green or red emission could be achieved in NMSF-based phosphors, respectively. Upconversion emission could also be designed by doping with Yb3+–Er3+, Yb3+–Tm3+, Yb3+–Ho3+ or Er3+. Moreover, the NMSF:Er3+ phosphor exhibited green upconversion emission upon excitation at 980 nm, and it exhibited red emission upon excitation at 1532 nm. Finally, recognizable patterns were obtained under excitation at 254, 365 and 980 nm, indicating that the as-prepared phosphors can be applied to multicolor anti-counterfeiting. Moreover, our synthesis strategy opens up new avenues for the synthesis of novel fluorides.
研究领域:
材料科学
·
光学
·
化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Materials Chemistry Frontiers
·
2021
·Vol. 5
·期 14
·5336-5343
·
IF 6.482
Shuyuan Li,Zhongyuan Huang,Yinguo Xiao,Chunwen Sun
Solid-state electrolytes (SSEs) are expected to replace liquid electrolytes in lithium metal batteries (LMBs) with good safety and mechanical strength. However, the existing problems of the Li1.3Al0.3Ti1.7(PO4)3 (LATP) electrolyte, like its poor contact with electrodes, serious side reactions and low ionic conductivity, limit its practical application. In this work, a chlorine (Cl)-doped LATP electrolyte showing a high ionic conductivity of 0.423 mS cm−1 was successfully synthesized. Neutron powder diffraction (NPD) results reveal that the change of the Li+ coordination environment after Cl doping has an effect on the ion diffusion path in the bulk LATP. The fabricated Li symmetric battery with the Cl-doped LATP exhibits long-term compatibility and electrochemical stability against the lithium metal anode. The enhanced performance may be attributed to the in situ formed stable solid electrolyte interphase (SEI) layer. Meanwhile, compared to the LATP electrolyte, the Li|LiFePO4 (LFP) full battery with Cl-doped LATP as an electrolyte has an improved rate performance and cycling performance. This work demonstrates that Cl doping may be an effective approach for improving the performance of the LATP electrolyte.
研究领域:
材料科学
·
电化学
·
电池技术
✓ 已验证
DOI
高影响因子
RSC Advances
·
2018
·Vol. 8
·期 56
·32325-32332
·
IF 2.936
Yuhan Zhu,Yu Pan,Wenjun Wang,Haibing Xu,Liqun Zhou,Xiaoguang Liu,Ling Li
The local crystal sites occupied by Eu3+ in Ca5(BO3)3F:1% Eu3+ phosphor were investigated experimentally and theoretically. Ca5(BO3)3F:1% Eu3+ was synthesized by high-temperature solid-state method in air. The crystal structure and optical properties of the phosphor were studied by X-ray powder diffraction and photoluminescence, respectively. Two different O2− → Eu3+ CT broad bands with the peaks at 266 and 283 nm in Ca5(BO3)3F:1% Eu3+ were detected, indicating the Eu3+ sites occupied Ca2 and Ca1, respectively. The different sharp f–f emission spectra under the excitation of 283 and 266 nm proved that there are two different local lattice environments around Eu3+ existing in Ca5(BO3)3F:1% Eu3+. Environmental factor he, the standard deviation of environmental factor (EFSD) and the bond energy were used to illustrate and explain the site occupancy mechanism of Eu3+ into the host lattice. By comparing the intensity ratios of 5D0 → 7F2 transition to the 5D0 → 7F1 transition, I(5D0/7F2)/I(5D0/7F1) of Eu3+ at Ca2 (7.381) was found to be 2.5 times stronger than that of Eu3+ at Ca1 site (2.933). was calculated to analyze the I(5D0/7F2)/I(5D0/7F1) value. On the basis of the bond valence model, a bond-energy method was used to study the occupancy of the Eu ion, which indicated that the preferential sites of Eu ion occupancy in the Ca5(BO3)3F are the Ca2 and Ca1 sites. All three theoretical calculation results are consistent with each other.
研究领域:
材料科学
·
固体化学
·
光学
·
晶体学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）