New horizon in mechanochemistry—high-temperature,high-pressure mechanical synthesis in a planetary ball mill—with magnesium hydride synthesis as an example

A new route of materials synthesis, namely, high-temperature, high-pressure reactive planetary ball milling (HTPRM), is presented. HTPRM allows for the mechanosynthesis of materials at fully controlled temperatures of up to 450 °C and pressures of up to 100 bar of hydrogen. As an example of this application, a successful synthesis of magnesium hydride is presented. The synthesis was performed at controlled temperatures (room temperature (RT), 100, 150, 200, 250, 300, and 325 °C) while milling in a planetary ball mill under hydrogen pressure ($>$50 bar). Very mild milling conditions (250 rpm) were applied for a total milling time of 2 h, and a milling vial with a relatively small diameter (φ = 53 mm, V = ～0.06 dm³) was used. The effect of different temperatures on the synthesis kinetics and outcome were examined. The particle morphology, phase composition, reaction yield, and particle size were measured and analysed by scanning electron microscopy, X-ray diffraction, differential scanning calorimetry (DSC) techniques. The obtained results showed that increasing the temperature of the process significantly improved the reaction rate, which suggested the great potential of this technique for the mechanochemical synthesis of materials.     

Development of high pressure membraneless alkaline electrolyzer

A technology for cyclic generation of hydrogen and oxygen using electrodes made of variable valency material that does not need the use of separating ion-exchange membranes is presented. The technological solution enables to fabricate electrolyzers for uninterrupted producing high-pressure hydrogen with reduced energy intensity of the production. The total work for compressing 1 m³ of hydrogen and 0.5 m³ of oxygen has been estimated. Results of investigation of influence of discrete supply of DC current to the electrolysis cell, in order to improve the processes of gas evolution and to simplify the power systems of the electrolysis plant, have been considered. There is also considered an electrolysis installation equipped with a thermosorption compressor in which LaNi₅ is used as a hydride-forming compound. The comparative characteristics of the developed electrolyzer and the currently used hydrogen generators are given.     

Fabrication of alumina ceramics with functional gradient structures by digital light processing 3D printing technology

Alumina ceramics with different unit numbers and gradient modes were prepared by digital light processing (DLP) 3D printing technology. The side length of each functional gradient structure was 10 mm, the porosity ratio was controlled to 70%, and the number of units were (1 × 1 × 1 unit) and (2 × 2 × 2 unit) respectively. The different gradient modes were named FCC, GFCC-1, GFCC-2 and GFCC-3. SEM, XRD, and other characterization methods proved that these gradient structures of alumina ceramics had only α-Al2O3 phase and good surface morphology. The mechanical properties and energy absorption properties of alumina ceramics with different functional gradient structures were studied by compression test. The results show that the gradient structure with 1 × 1 × 1 unit has better mechanical properties and energy absorption properties when the number of units is different. When the number of units is the same, GFCC-2 and GFCC-3 gradient structures have better compressive performance and energy absorption potential than FCC structures. The GFCC-2 gradient structure with 1 × 1 × 1 unit has a maximum compressive strength of 19.62 MPa and a maximum energy absorption value of 2.72 × 105 J/m3. The good performance of such functional gradient structures can provide new ideas for the design of lightweight and compressive energy absorption structures in the future.     

Noncentrosymmetric Tetrel Pnictides RuSi4P4 and IrSi3P3: Nonlinear Optical Materials with Outstanding Laser Damage Threshold

Noncentrosymmetric (NCS) tetrel pnictides have recently generated interest as nonlinear optical (NLO) materials due to their second harmonic generation (SHG) activity and large laser damage threshold (LDT). Herein nonmetal-rich silicon phosphides RuSi₄P₄ and IrSi₃P₃ are synthesized and characterized. Their crystal structures are reinvestigated using single crystal X-ray diffraction and ²⁹Si and ³¹P magic angle spinning NMR. In agreement with previous report RuSi₄P₄ crystallizes in NCS space group P1, while IrSi₃P₃ is found to crystallize in NCS space group Cm, in contrast with the previously reported space group C2. A combination of DFT calculations and diffuse reflectance measurements reveals RuSi₄P₄ and IrSi₃P₃ to be wide bandgap (E_g) semiconductors, E_g = 1.9 and 1.8 eV, respectively. RuSi₄P₄ and IrSi₃P₃ outperform the current state-of-the-art infrared SHG material, AgGaS₂, both in SHG activity and laser inducer damage threshold. Due to the combination of high thermal stabilities (up to 1373 K), wide bandgaps (≈2 eV), NCS crystal structures, strong SHG responses, and large LDT values, RuSi₄P₄ and IrSi₃P₃ are promising candidates for longer wavelength NLO materials.     

超高效液相色谱-串联质谱法同时检测糕点中6种甜味剂

目的建立超高效液相色谱-串联质谱法同时测定糕点中6种常用合成甜味剂的分析方法。方法选用超纯水作为提取溶剂,涡旋和超声提取后,低温离心,取部分上清液加入正己烷除脂,Waters Atlantis■T3色谱柱、甲醇-5 mmol/L甲酸铵(含0.1%甲酸)作为流动相、亲水亲脂平衡型固相萃取柱HLB(hydrophile-lipophile balance)净化。结果6种甜味剂在质量浓度为10~200 ng/mL的曲线范围内呈良好线性关系,相关系数r均大于0.999,平均加标回收率在85.0%-98.2%之间,相对平均偏差(relative standard deviation,RSD)为1.3%~6.7%。结论该方法具有前处理简单、灵敏度高、检测速度快等优点,适合糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、纽甜的检测,但不适用于安赛蜜的检测。     

Thermal prehistory,structure and high-temperature thermodynamic properties of Y2O3-CeO2 and Y2O3-ZrO2-CeO2 solid solutions

Ceria-based solid solutions are important materials for high- and medium-temperature electrochemical applications. However, the stabilities of both binary and ternary ceria-based solid solutions are insufficient at elevated temperatures, which limits their application as solid electrolytes or SOFC cathodes. Data on the high-temperature stability of ceria-based ceramics are unavailable in the literature. In the present study, we report a thermodynamic stability investigation of Y₂O₃-CeO₂ and Y₂O₃-ZrO₂-CeO₂ solid solutions. The thermal prehistories of binary and ternary systems were investigated using STA, XRD, and ESCA techniques. The vaporization processes were investigated in the temperature range of 1577–2227°С via the Knudsen effusion mass spectrometry technique. Using data on the component activity in solid-phase thermodynamic properties of Y₂O₃-CeO₂ solid solutions, which is represented as the Gibbs energy, the excess Gibbs energy was calculated as a function of the ceria mol. %. It was shown that the reduction of Ce⁴⁺ to Ce³⁺ in Y₂O₃-CeO₂ and Y₂O₃-ZrO₂-CeO₂ solid solutions corresponds to less-negative Gibbs energy compared to ZrO₂-CeO₂ solid solutions.     

A new signal processing-based islanding detection method using pyramidal algorithm with undecimated wavelet transform for distributed generators of hydrogen energy

Machine learning-based fault detection methods are frequently combined with wavelet transform (WT) to detect an unintentional islanding condition. In contrast to this condition, these methods have long detection and computation time. Thus, selecting a useful signal processing-based approach is required for reliable islanding detection, especially in real-time applications. This paper presents a new modified signal processing-based islanding detection method (IDM) for real-time applications of hydrogen energy-based distributed generators. In the study, a new IDM using a modified pyramidal algorithm approach with an undecimated wavelet transform (UWT) is presented. The proposed method is performed with different grid conditions with the presence of electric noise in real-time. Experimental results show that oscillations in the acquired signal can be reduced by the UWT, and noise sensitivity is lower than other WT-based methods. The non-detection zone is zero and the maximum detection and computational time is also 75 ms at a close power match.     

Recent advances in carbon nanotubes-based microwave absorbing composites

With the blossom of information industry, electromagnetic wave technology shows increasingly potential in many fields. Nevertheless, the trouble caused by electromagnetic waves has also drawn extensive attention. For instance, electromagnetic pollution can threaten information safety in vital fields and the normal function of delicate electronic devices. Consequently, electromagnetic pollution and interference become an urgent issue that needs to be addressed. Carbon nanotubes (CNTs) have become a potential candidate to deal with these problems due to many advantages, such as high dielectric loss, remarkable thermodynamic stability, and low density. With the appearance of climbing demands, however, the carbon nanotubes combining various composites have shown greater prospects than the single CNTs in microwave absorbing materials. In this short review, recent advances in CNTs-based microwave absorbing materials were comprehensively discussed. Typically, we introduced the electromagnetic wave absorption mechanism of CNTs-based microwave absorbing materials and generalized the development of CNTs-based microwave absorbers, including CNTs-based magnetic metal composites, CNTs-based ferrite composites, and CNTs-based polymer composites. Ultimately, the growing trend and bottleneck of CNTs-based composites for microwave absorption were analyzed to provide some available ideas to more scientific workers.     

Characteristic tryptic peptides and gelling properties of porcine skin gelatin affected by thermal action

Thermal action in extraction process had effects on characteristic tryptic peptides identification and gelling properties of porcine gelatin. SDS-PAGE, HPLC-LTQ/Orbitrap high-resolution mass spectrometry, texture analyser and rheometer were used to evaluate collagen depolymerisation degree, characteristic tryptic peptides and gelling properties of gelatins prepared in various thermal actions. Results showed that with increasing temperature and time, depolymerisation degree enlarged, while gel strength, gelling and melting temperature decreased. Mass spectra showed that 47 and 49 common characteristic tryptic peptides were identified in gelatins extracted at 50 °C and 100 °C with various times, respectively. Moreover, 34 common characteristic tryptic peptides were identified in all gelatin samples. Further comparison between this work and our previous investigations yielded 20 common characteristic tryptic peptides, which stably exist in various thermal actions. These common characteristic tryptic peptides may be very helpful for the accurate authentication of porcine gelatin.