不同球磨粉碎工艺对固相合成β-磷酸三钙纯度和粒度的影响

采用纳米球磨-超声搅拌工艺制备了β-磷酸三钙粉体,并与传统固相合成工艺进行了对比研究。采用差示扫描量热（DSC）、X射线衍射（XRD）、红外（FTIR）、纳米粒度测试、扫描电镜（SEM）、透射电镜（TEM）及X射线荧光光谱（XRF）等手段对两种工艺所制备粉体进行了纯度和粒度表征。结果表明：相比传统工艺,经过纳米球磨-超声搅拌工艺制备出的β-TCP粉体纯度可达97%以上,平均粒径为666 nm。粉体的纯度高、粒径分布更均匀。同时,纳米球磨加工后的原料平均粒度更小,分散性更好。该工艺有望用于粉体材料的固相合成。     

Solvent-deficient synthesis of cerium oxide: Characterization and kinetics

The reaction mechanism and kinetics of CeO₂ synthesis using a solvent-deficient method are investigated by simultaneous thermogravimetric analysis (TGA)/differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The decomposition process of the cerium(III) nitrate hexahydrate and ammonium bicarbonate precursor mixture with four observed stages is monitored using TGA/DSC measurements in a nonisothermal regime with heating rates of 5, 10, 15 and 20?°C min^?1. The proposed mechanism indicates a complex synthesis with several parallel reactions, some of which occur at room temperature. A detailed kinetic analysis is performed using isoconversional (expanded Friedman, modified Coats-Redfern and Kissinger) and model fitting (N^th order and nucleation and growth models) methods. The first three stages are best described by the N^th order model with activation energy values of 21, 53 and 90?kJ?mol^?1. The last stage, during which ammonium nitrate decomposition occurs, is best fit by the nucleation and growth model and has an activation energy of 129?kJ?mol^?1. The proposed mechanism, supported by the kinetic analysis in our study, indicates that CeO₂ has already formed before the reaction reaches 200?°C. The average crystallite size of CeO₂ synthesized at 300?°C, which was calculated from the XRD measurements and observed in the SEM and TEM data, is between 10 and 20?nm.     

Tannic acid coating and in situ deposition of silver nanoparticles to improve the antifouling properties of an ultrafiltration membrane

The construction of antifouling membranes has been a desirable approach for addressing membrane-fouling issues in the ultrafiltration (UF) process. Antifouling means antiadhesive and antimicrobial; however, few researchers have achieved both properties in a facile and effective manner. In this article, we report a direct tannic acid (TA) coating method combined with the in situ deposition of silver nanoparticles (Ag NPs); this was used to improve the antifouling properties of a positively charged polymeric UF membrane. The results show that the TA–Ag NP modified membranes showed improved protein resistance (flux recovery rate = 71.2% after modification vs 17.8% before modification) and less attachment of bacteria (Escherichia coli K1) on the membrane surface and reduced cell viability in the resulting bacterial suspension (reduced by ≥90%) because of the combined antimicrobial properties of both the TA and Ag NPs. This indicated that our modification method was promising for UF membrane antifouling applications. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47314.     

基于SOM-RBF神经网络的COD软测量方法

污水处理是一个复杂的非线性过程,化学需氧量（chemical oxygen demand,COD）是评价污水处理效果的关键指标之一。COD的传统测量方法耗时长、成本高,基于传统神经网络的软测量方法提高了COD参数的测量速度但精度较差。针对这些问题,设计一种结合自组织特征映射 (self-organizing map, SOM)和径向基函数(radial basis function, RBF)神经网络的COD参数软测量方法。该方法利用SOM网络聚类数据样本,根据所得聚类结果确定RBF网络的隐层节点数及节点的数据中心,综合提高RBF网络的收敛速度和拟合精度。利用污水处理厂部分水样数据建立COD软测量模型,模型仿真和硬件在线测试结果表明,相对于传统的BP、RBF等网络,基于SOM-RBF神经网络的COD软测量方法测量时间短、预测精度较高,具有较为广阔的应用前景。     

Microstructural evolution during high-temperature oxidation of spark plasma sintered Ti2AlN ceramics

Microstructures of Ti₂AlN ceramics synthesized and simultaneously consolidated from starting mixtures of Ti/Al/TiN powders by spark plasma sintering (SPS) were characterized using X-ray diffraction, scanning electron microscopy, focused ion beam (FIB) and transmission electron microscopy (TEM). When sintered for 10 min at 1300 °C, nearly single-phase Ti₂AlN ceramics with elongated (∼22 × 6 × 6 μm) grains were obtained. After sintering for 10 min at 1200 °C and chemical etching, Ti₂AlN nanowhiskers (150-200 nm dia., 1-5 μm long) were exposed in pores coexisting with TiAl, TiN and Ti₂AlN grains. FIB-TEM studies revealed single-crystal Ti₂AlN nanowhiskers in a TiAl matrix with orientation relationship [1 1 −2 0]_H//[−1 0 1]_γ, (0 0 0 1)_H//(1 1 1)_γ, γ = TiAl, H = Ti₂AlN. The nanowhiskers are believed to form by diffusion of TiN into TiAl during SPS and to be exposed during the chemical etch. Microstructural development during high-temperature oxidation of dense Ti₂AlN ceramics for 1 h at <1200 °C involves gradual formation on the surface of layered microstructures containing anatase, rutile and α-Al₂O₃. After 1 h at >1200 °C, more complex layered microstructures containing Al₂TiO₅, rutile, α-Al₂O₃ and continuous voids layers form. After heating to 1100 °C for 1 h and cooling to room temperature, planar defects are observed in surface TiO₂ grains identified as stacking faults bounded by partial dislocations. After heating for 1 h at 1400 °C and cooling to room temperature, cracks propagate in TiO₂ grains. It is believed that planar defects and cracks arise from stress generation in the oxide scale. Thermal stresses formed on cooling may arise from thermal expansion mismatch of phases (TiO₂, Al₂O₃ and Al₂TiO₅) in the oxide scale, the high anisotropy of thermal expansion in Al₂TiO₅ and thermal expansion mismatch between the oxide scale and Ti₂AlN substrate. Growth stresses formed during the isothermal oxidation treatment may arise from the volume changes associated with oxidation reactions of Ti₂AlN. An oxidation mechanism for Ti₂AlN ceramics is proposed, which involves initial reaction with atmospheric oxygen to form oxide phases, demixing of the mixed oxide phases, void formation due to the Kirkendall effect and gaseous NO_x release. Oxidation of Ti₂AlN <1200 °C with 1 h hold times is limited, while above this temperature the oxide scale grows rapidly, and Ti₂AlN ceramics undergo heavy oxidation.     

The effect of the particle size and the morphology of alumina powders on the processing of green bodies by electrophoretic deposition

The electrophoretic deposition (EPD) method was investigated for the preparation of compacts from nanosized alumina powders. Ethanol suspensions of commercially available nanosized transition alumina and α-alumina powders were used. In addition, submicron powders were also considered for comparison. Besides the influence of operational pH change, the influence of the addition of three different surfactants – two branched polyethylene imines with molecular masses 1800 and 10,000, and citric acid—on the zeta-potential of the particles in ethanol and afterwards on the EPD was investigated.The packing density of the green parts prepared by the EPD of nanosized α-alumina powders at 30 V/cm was low (the green density was 27 vol. % of the theoretical density—TD), and a bimodal pore size distribution was observed. In contrast, the packing density in deposits made with the transition alumina nanopowder was much higher (the green density was 42 vol. % of the TD) and a monomodal distribution of pores was observed. In general, for all the deposits made from nanosized alumina powders, the particle-packing density was found to be lower than for those made from the submicron alumina powders (a green density equal to 59 vol. % of the TD).     

钢轨表面缺陷漏磁检测的三维磁场分析

漏磁检测技术通常测量垂直和平行于缺陷表面的漏磁场分量,来实现对缺陷的定量分析。然而,对于钢轨表面的复杂裂纹,传统的方法很难准确检测。为了克服这种检测方法存在的不足,采用三维磁场测量方法以及有限元法对缺陷漏磁场的三维分布情况进行了分析。在此基础上设计了一套适合钢轨表面缺陷检测的三维漏磁检测系统,并对人工缺陷样例进行了检测。结果表明,漏磁信号垂直分量包含重要的缺陷信息,特别是对于与钢轨走向不垂直的缺陷。     

退火温度对21Cr-0.3Cu铁素体不锈钢组织性能的影响

通过光学显微镜、拉伸试验及背散射电子衍射,研究了退火温度对21Cr-0.3Cu超纯铁素体不锈钢显微组织、力学性能、成形性能和微观织构的影响。结果表明,试验钢经970 ℃退火时,晶粒细小且均匀,组织处于完全再结晶状态。退火温度低于970 ℃时,再结晶不完全;退火温度高于970 ℃时,再结晶晶粒异常长大,这两种情况均出现混晶组织。试验钢在970 ℃退火时,综合力学性能最佳,抗拉强度为473 MPa,屈服强度为315 MPa,伸长率35.7%。随退火温度的升高,试验钢的平均塑性应变比r_m值先增加后减少。当退火温度达到970 ℃时,r_m可以达到最大值1.82。γ纤维织构密度变化趋势与r_m值一致,退火温度为970 ℃时,γ纤维增强明显,此时其取向密度达到最大值f(g)=20.56,成形性能最佳。     

金刚烷甲酸纤维素酯的合成与表征

以N,N-二甲基乙酰胺/LiCl为溶剂,以对甲苯磺酰氯为共反应剂原位活化金刚烷甲酸,在均相反应体系中合成了新的纤维素高级脂肪酸酯——金刚烷甲酸纤维素酯。采用红外光谱、核磁共振谱进行了表征。热重分析表明,在纤维素链中引入金刚烷基可提高其热稳定性,取代度越高,热稳定性越好。金刚烷甲酸纤维素酯在有机溶剂中的溶解性随取代度增大而提高。