以NH4HCO3为沉淀剂通过共沉淀法制备2Y-TZP纳米粉体

以NH_4HCO_3,ZrOCl_2·9H_2O和Y(NO_3)_3为原料,在乙醇溶液中通过共沉淀法制备2Y-TZP纳米粉体,并对其中的反应机理进行研究.在沉淀过程中,NH_4HCO_3和ZrOCl_2通过两步反应生成(NH_4)_3ZrOH(CO_3)_3·2H_2O对沉淀.首先NH_4HCO_3和ZrOCl_2反应生成Zr(OH)_4,其后Zr(OH)_4和NH_4HCO_3进一步反应生成(NH_4)_3ZrOH(CO_3)_3·2H_2O.(NH_4)_3ZrOH(CO_3)_3·2H_2O不稳定,在130℃即可分解生成ZrO_2,并放出氨气、水和二氧化碳.沉淀产物经300和450℃煅烧后得到的ZY-TZP粉体颗粒尺寸细小,不存在大的硬团聚,具有良好的烧结性,在1225℃即可实现高度致密化.     

Synthesis, growth and thermal and Fourier transform infrared spectral characterization of tetraethylammonium tetrachloro manganate (II) monohydrate crystals

Single crystals of a novel tetraethylammonium tetrachloro manganate (II) monohydrate (TEATC-Mn) were grown by slow evaporation solution technique at room temperature. These crystals belong to a class of interesting ferroelectric materials. The grown crystals were characterized through powder X-ray diffraction (XRD), thermogravimetry, differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC) studies and Fourier transform infrared (FTIR) spectra. While the results of the elemental analysis of the compound agree with the stoichiometry, its crystallinity is confirmed by the powder X-ray diffraction pattern. The weight losses observed were suitably explained based on the formulated decomposition pattern. The differential thermal analysis of the compound conforms to the thermogravimetric study. The endothermic peak observed in the high temperature differential scanning calorimetry suggests the occurrence of a phase transition in the compound between 300 and 370 °C while the corresponding low temperature study shows thermal anomalies at −41.7, −51.7 and at −52.4 °C. This suggests the occurrence of both first and second order phase transitions. The characteristic absorptions in the FTIR spectrum further characterize the compound. Further investigations on the ferroelectric behaviour of the compound at low temperatures are in progress.     

CMTD晶体(001)面的表面形貌观测及其结晶形态研究

用倒置相差显微镜观察了CdHg(SCN)4(H6C2OS)2(CMTD)晶体结晶过程的形态变化。同时用原子力显微镜(AFM)对CMTD的(001)面进行形貌观察，测得的初级台阶高度为1．411nm，是晶胞参数c的一半，发现了螺旋生长丘及缺陷．并对生长丘的中心孔芯作了初步分析，讨论了CMTD晶体所特有的“树杈状”和“一字形”缺陷及形成机理。     

H2SO4介质中邻磺酰苯甲酰亚胺对A3钢的缓蚀作用

用浸泡实验、动电位扫描极化曲线和交流阻抗法研究了邻磺酰苯甲酰亚胺在5%H2SO4介质中对A3钢的缓蚀作用及缓蚀机理,得出邻磺酰苯甲酰亚胺是一种缓蚀效果显著的混合型缓蚀剂,在A3钢表面发生了化学吸附,吸附过程为吸热过程,并计算出相应的吸附过程热力学数据.     

Investigating the Mechanism of Hysteresis Effect in Graphene Electrical Field Device Fabricated on SiO(2) Substrates using Raman Spectroscopy

The hysteresis effect is a common problem in graphene field-effect transistors (FETs). Usually, the external doping to graphene is considered to be responsible for the hysteresis behavior, but is not yet clearly understood. By monitoring the doping of graphene and the hysteresis in graphene FETs under different atmospheres using in situ Raman spectroscopy, it is confirmed that the electrochemical doping of O(2) /H(2) O redox couple to graphene is responsible for the hysteresis effect. In addition, Raman spectra of graphene on SiO(2) substrate show stronger doping than that suspended, which indicates that SiO(2) substrate plays an important role in the doping of graphene. Herein it is proposed that the doping species (H(2) O and O(2) ) are bounded at the interface of graphene/SiO(2) substrate by hydrogen-bonds with the silanol groups on SiO(2) substrate. The dynamic equilibrium process of the charge-transfer between H(2) O/O(2) redox couple and graphene under electrical field modulation is carefully analyzed using Marcus-Gerischer theory. This work provides a clear view to the mechanism of the hysteresis effect, and is of benefit to a reliable design to suppress the hysteresis in graphene FETs.     

Effects of growth conditions on the domain structure and dielectric properties of (1 − x)Pb(Sc1/2Nb1/2)O3–xPbTiO3 single crystals

The studies of the (1 − x)Pb(Sc_1/2Nb_1/2)O₃–xPbTiO₃ (PSN–PT) single crystals reveal that the chemical and physical properties of the materials are affected by the growth conditions. By the measurements of the dielectric constant as a function of temperature upon cooling, it is found that crystals grown from the same charged stoichiometric composition (x = 0.425), but under different flux environments (i.e. the composition of flux and the flux to PSN–PT ratios are varied), show anomalies (i.e. phase transitions) at different temperatures. This phenomenon is attributed to the complex local chemical structure of the PSN–PT solid solution single crystals with B-site random occupancy of three different cations (Sc³⁺, Nb⁵⁺ and Ti⁴⁺). The dielectric and domain structure of the PSN–PT crystals with composition near the morphotropic phase boundary (MPB) are investigated, showing much more complex situations compared with Pb(Sc_1/2Nb_1/2)O₃.     

尿素改性对钠离子电池负极材料NaTi_2(PO_4)_3电化学性能的影响

为提高水溶液钠离子电池负极材料NaTi_2(PO_4)_3(NTP)的导电性和倍率性能,以尿素(CO(NH_2)_2)为碳源采用溶剂热法合成了CO(NH_2)_2/NaTi_2(PO_4)_3(C/NTP)复合负极材料。采用XRD、SEM、TEM、Raman和恒流充放电等手段分析了材料的结构、C/NTP形貌和电化学性能。研究了不同阶段升温速率对C含量、包覆层石墨化程度及对电化学性能的影响。实验结果表明,低于400℃升温速率越小,C/NTP残碳量越高;400~650℃之间升温速率越小,包覆层石墨化程度越高,并提高了其电化学性能;在5C倍率下2℃/min热处理的样品首圈放电比容量为114.9mAh·g~(-1),循环30次后容量保持在91.9mAh·g~(-1);10C下放电比容量为87mAh·g~(-1),20C下放电比容量仍保持在71mAh·g~(-1),展现出高倍率下优异的循环性能。     

Polar nanodomains and relaxor behaviour in (1 − x)Pb(Mg1/3Nb2/3)O3–xPbTiO3 crystals with x = 0.3–0.5

Phase transitions and dielectric properties of the (1 − x)Pb(Mg_1/3Nb_2/3)O₃–xPbTiO₃ crystals with x = 0.3–0.5 are studied. The solid solutions in this composition range are shown to be relaxor ferroelectrics. The crystals with low x demonstrate a diffused maximum in the temperature dependences of the dielectric permittivity at T_m. T_m varies with frequency according to the Vogel–Fulcher law. The polarizing microscopy investigations reveal a first-order phase transition from the relaxor phase to the low-temperature ferroelectric phase at T_C, which is several degrees below T_m. The permittivity peak in the crystals with x = 0.5 is sharp, and T_m is equal to T_C and does not depend on frequency, as is typical of the transition from a ferroelectric to an ordinary paraelectric phase. Nevertheless, the relaxor, but not the paraelectric, phase is observed at T > T_m. This conclusion is confirmed by the observation of the temperature behaviour of complex dielectric permittivity at T > T_m, which is typical of relaxors and related to the existence of polar nanodomains.     

Effect of the orientation on the ferroelectric-antiferroelectric behavior of sol-gel deposited (Pb,Nb)(Zr,Sn,Ti)O3 thin films

The (Pb,Nb)(Zr,Sn,Ti)O₃ (PNZST) antiferroelectric thin films were prepared on two different substrates by sol-gel methods. Films derived on the LNO/Pt/Ti/SiO₂/Si substrates showed a strong (100) preferred orientation. The dependence of electrical properties derived on the Pt/Ti/SiO₂/Si and LNO/Pt/Ti/SiO₂/Si substrates have been studied, with the emphasis placed on field-induced phase switching from the antiferroectric to the ferroelectric state. The PNZST thin films deposition on two kinds of substrates show different phase transition behavior and associated properties such as antiferroelectric (AFE) to ferrroelectric (FE) switching field E_AFE-FE, FE to AFE switching field E_FE-AFE and the hysteresis ΔE=E_AFE-FE−E_FE-AFE.     

镀锌钢板蒸镀镁层的耐腐蚀机理

采用真空蒸镀技术在镀锌钢板上蒸镀镁,制得了蒸镀镁层,将其在5%NaCl溶液中浸泡,运用XRD,SEM和电化学方法等对其腐蚀产物进行了分析.对2种材料的的腐蚀行为进行了研究,探讨了其耐腐蚀机理.结果表明:镀锌钢板蒸镀镁层是以MgZn2和Mg2Zn11.金属间化合物的形式存在;其腐蚀产物是以致密且具有良好绝缘性的ZnCl2·4Zn(OH)2·H2O和致密的Zn4CO3(OH)6·H2O为主体,而纯锌镀层的腐蚀产物是以疏松且具有N型半导体性质的ZnO为主体;蒸镀镁层的形成可以抑制Zn(OH)2向ZnO的转化,能促进Zn(OH)2向ZnCl2·4Zn(OH)2·H2O和Zn4CO3(OH)6·H2O的转化,后二者能够牢固地覆盖在基体表面,从而延缓了锌的腐蚀进程;在宏观上表现为镀锌钢板蒸镀镁层腐蚀产物相对于纯锌镀层更加致密,在电化学行为上表现为镀锌钢板蒸镀镬层具有更小的腐蚀电流和更高的极化电阻.     

Effect of Functional Group Modifications on the Photocatalytic Performance of g-C3N4

In recent years, photocatalysis has received increasing attention in alleviating energy scarcity and environmental treatment, and graphite carbon nitride (g-C₃N₄) is used as an ideal photocatalyst. However, it still remains numerous challenges to obtain the desirable photocatalytic performance of intrinsic g-C₃N₄. Functional group functionalization, formed by introducing functional groups into the bulk structure, is one of the common modification techniques to modulate the carrier dynamics and increases the number of active sites, offering new opportunities to break the limits for structure-to-performance relationship of g-C₃N₄. Nevertheless, the general overview of the advance of functional group modification of g-C₃N₄ is less reported yet. In order to better understand the structure-to-performance relationship at the molecular level, a review of the latest development of functional group modification is urgently needed. In this review, the functional group modification of g-C₃N₄ in terms of structures, properties, and photocatalytic activity is mainly focused, as well as their mechanism of reaction from the molecular level insights is explained. Second, the recent progress of the application of introducing functional groups in g-C₃N₄ is introduced and examples are given. Finally, the difficulties and challenges are presented, and based on this, an outlook on the future research development direction is shown.     

Bi3+、Y3+掺杂对Gd2(MoO4)3:Eu3+发光性能的影响

采用高温固相法制备Bi3+、Y3+掺杂LED用小颗粒红色荧光粉Gd2(MoO4)3∶Eu3+.通过X粉晶衍射仪、F-4500荧光分光光度计、JSM-35CF型扫描电子显微镜对离子掺杂后的红色荧光粉进行检测和表征.结果表明,经过Bi3+、Y3+掺杂,红色荧光粉Gd2(MoO4)3∶Eu3+的相对发光强度提高,荧光粉晶体的结构完整、颗粒细小均匀,平均粒径约为2靘,具有较好的涂覆性能,能满足白光LED用红色荧光粉的要求.     

Effect of oxygen plasma treatment of PPTA and PBO fibers on the interfacial properties of single fiber/epoxy composites studied by Raman spectroscopy

The interfacial micromechanics of single poly(p-phenylene terephthalamide (PPTA) and poly(p-phenylene benzobisoxazole (PBO) fibers embedded in an epoxy resin has been investigated by determining the interfacial shear stress distributions along the fiber length. The effects of an oxygen plasma treatment on the interfacial shear stress of the fiber-epoxy systems are analyzed. Raman spectroscopy was used to map the stress distributions along the fiber when the composite is subjected to a small axial tensile strain (3.5% for PPTA and 2.5% for PBO). The quality of the interface or adhesion was improved after the surface treatment, supporting the ability of plasma oxidation to enhance the adhesion of high-performance fibers to epoxy resins. The tensile behavior of fiber-reinforced systems was different in each case. PPTA reinforcements underwent fragmentation, likely by fiber microfailure, whereas debonding or bridging is the most probable fragmentation mechanism in the case of PBO.     

柠檬酸溶胶燃烧工艺参数对Ca_3(VO_4)_2:Eu~(3+)发光性能的影响

采用柠檬酸溶胶燃烧法合成了Ca3(VO4)2:Eu3+红色发光材料。利用XRD、SEM、荧光分光光度计等测试分析方法研究了合成温度、柠檬酸用量以及Eu3+含量等对合成样品组成、结构、显微特征和发光性能的影响。结果表明,采用柠檬酸溶胶燃烧法可以在700～1000℃范围内合成纯度高、结晶度好、粒度均匀的Ca3(VO4)2:Eu3+红色发光粉。优化条件为温度900℃、n(柠檬酸):n(Ca2++V5+)=0.8、Eu3+摩尔分数6%,合成产物的红光发光效果最好。     

CaO-MgO-Al_2O_3-SiO_2-P_2O_5-F系微晶玻璃初晶相Ca_5(PO_4)_3F析晶过程的研究

本文应用透射电镜:选区电子衍射和微区成份分析并结合扫描电镜形貌观察,深入研究了 CaO-MgO-Al_2O_3-SiO_2-P_2O_5-F 系可切削生物微晶玻璃初晶相 Ca_5(PO_4)_3F 的析晶机理。研究表明,玻璃首先发生二液分离,形成了能够析出初晶相 Ca_5(PO_4)_3F 晶体的富 P~(5+)、Ca~(2+)、Mg~(2+)、Ti~(4+)的液滴相。在进一步的热处理中,液滴相发生整体核化,并逐步形成由大量细小晶粒镶嵌生长构成的球形 Ca_5(PO_4)_3F 聚集体。随着热处理温度的提高,这些球形 Ca_5(PO_4)_3F 聚集体逐渐转变为广泛分布于微晶玻璃另一主晶相氟金云母中的六方短柱状 Ca_5(PO_4)_3F 微小晶体。     

含铅氧空位对的PbWO4晶体光学性质及其偏振特性的模拟计算

利用完全势缀加平面波局域密度泛函近似,按照能量最低原理采用共轭梯度方法,对含铅氧空位对的PbWO4晶体进行结构优化处理。在此基础上,计算了含铅氧空位对的PbWO4晶体的电子结构、复数折射率、介电函数及吸收光谱的偏振特性,并与完整的PbWO4晶体进行了比较。结果表明PWO晶体中铅氧空位对的存在不会引起在可见和近紫外区域的吸收。     

氧空位对Ga_(1.5)In_(0.5)O_3透明导电氧化物性能的影响

Ga1.5In0.5O3是一种潜在的紫外透明导电材料。用第一性原理计算了含氧空位的Ga1.5In0.5O3的结构参数、生成焓、能带结构、态密度、光吸收和光反射。氧空位的位置影响Ga1.5In0.5O3化合物的晶格常数和生成焓,含氧空位的Ga1.5In0.5O3是间接带隙半导体,其带隙宽度较本征Ga1.5In0.5O3带隙值变宽。氧空位VO(1)、VO(2)和VO(3)在Ga1.5In0.5O3中分别引入0.237eV、0.239eV和1.384eV的施主杂质能级,在吸收光谱中出现杂质吸收现象。氧空位降低Ga1.5In0.5O3吸收主峰和反射主峰的强度,在近红外区含VO(1)和VO(2)的Ga1.5In0.5O3的吸收系数和反射率较大,含VO(3)的Ga1.5In0.5O3的吸收系数和反射率较小。     

4-羟基丁酸含量对聚 3-羟基丁酸 与 4-羟基丁酸共聚物性能和结构的影响

目的对3-羟基丁酸4-羟基丁酸共聚酯P(3HB-co-4HB)进行酶解测试。方法通过力学性能测试、失重率分析、热失重分析、X-射线衍射分析、扫描电镜等测试和表征手段对样品的物理性能及生物降解情况进行评价。结果 P(3HB-co-4HB)分子中4HB单体(文中均用摩尔分数表示)的引入提高了材料的柔韧性,材料的脆性下降;失重率方面,4种材料的降解速率从高到低依次为P(3HB)P(3HB-co-5%4HB)(3HB-co-10%4HB)P(3HB-co-15%4HB);酶解前期,材料的热稳定性增强,而酶解后期材料的热稳定性逐渐下降;XRD结果表明材料降解过程中结晶度的变化不明显;P(3HB-co-4HB)分子中随着4HB单体含量的增加,材料表面粗糙度降低,酶解后材料表面被侵蚀,降解速率与失重率结果一致。结论 P(3HB-co-4HB)分子中4HB单体的引入显著影响了材料的机械性能,随着4HB含量的增加,材料的失重率越来越大,热稳定性呈现先上升后下降的趋势,材料表面粗糙度逐渐降低,由于酶解过程属于从表面侵蚀开始,因此酶解过程中样品的结晶度变化不大。     

Raman scattering analysis of Cu-poor Cu(In,Ga)Se2 cells fabricated on polyimide substrates: Effect of Na content on microstructure and phase structure

This work reports the Raman scattering surface and in-depth resolved analysis of Cu-poor Cu(In,Ga)Se₂ (CIGS) grown on polyimide substrates. In order to study the effect of Na on the formation and microstructure of the CIGS and the corresponding Cu-poor ordered vacancy compound (OVC) phases, a NaF precursor layer with different thicknesses was deposited on the Mo-coated substrates before growing of the samples. The Raman spectroscopy data are correlated with the analysis of the samples by Auger electron spectroscopy and scanning electron microscopy. These data corroborate the significant role of Na on the inhibition of Ga-In interdiffusion and on the formation of the MoSe₂ interfacial phase at the back region of the layers. Presence of Na also leads to an enhancement in the formation of the chalcopyrite CIGS phase and a decrease in the occurrence of the dominant OVC phase at the surface region. This study confirms the strong dependence of the microstructure and phase distribution in CIGS absorber layers on the Na available during their growth.