Coulometric titrations of electrolytes in water by a solid state ionic device using Nafion and Tosflex membranes

A solid state ionic device to titrate electrolytes in water was produced, and the performance of the device was examined. The device named the coulometric titration apparatus is a three-component electrochemical cell like an electrodialyzer. The central component, the analyzing room, is a container of the sample solution. The sample solution, 10⁻¹ M H₂SO₄, NaOH, Na₂SO₄, or 10⁻⁷–10⁻² M Na₂SO₄, is separated from the cathode and the anode room solutions, 10⁻² M H₂SO₄, NaOH, or Na₂SO₄, by Nafion-117 and Tosflex IE-SF34 membranes working as the anion and the cation blocking electrodes, respectively. The quantity of electricity to extract whole electrolytes in the sample solution is evaluated from the peak area of the titration curve. The sample concentration is successfully determined by the calibration curve method, with the quantity of electricity and the sample volume (6 ml) in the range from 10⁻¹ to 10⁻⁵ M.     

Effect of Yb on red to blue conversion fluorescence of Tm in fluorozirconate glass

The mechanisms governing the upconversion fluorescence from the ¹G₄ level of Tm³⁺ ions have been investigated in fluorozirconate glass doped with Tm³⁺ only and codoped with Tm³⁺ and Yb³⁺ ions, under 649 (³H₄→¹G₄) and 684 nm (³H₆→³F₃) excitation wavelengths. The emission intensity depends on the excitation power quadratically in both samples, showing the two-photon absorption nature of the processes. An enhancement of the ¹G₄→³H₆ emission was observed in the codoped sample under 684 nm excitation. The upconversion emission in the single doped sample is mainly due to the E.S.A. process upon both excitations. The dominant mechanism was found to be the energy transfer processes between Tm³⁺ and Yb³⁺ ions in the codoped sample when the excitation was tuned at 684 nm. The upconverted emission intensity shows a different temperature dependence under the two excitations in the codoped sample. However, for the 649 nm excitation the dependence is the same in both samples. This confirms the dominance of the E.S.A. process under 649 nm excitation in both, singly and doubly doped samples.     

SrB4O7：Pr3+,Mn2+中的Pr→Mn能量传递

从能量传递的角度出发,利用同步辐射光源(德国HASYLAB实验室的SUPERLUMI实验站)对Pr³⁺和Mn²⁺掺杂的SrB₄O₇粉末样品进行了光谱研究.206nm激发下,在SrB₄O₇:Pr³⁺(0.1%,摩尔分数)样品中观察到了来自Pr³⁺离子1S0能级的光子级联发射.SrB₄O₇:Pr³⁺样品的发射谱与SrB₄O₇:Mn²⁺样品监测Mn²⁺离子640nm发射的激发谱在330~430nm的波长范围里存在显著的光谱重叠.这个光谱重叠有利于Pr³⁺→Mn²⁺的能量传递发生,从而将Pr³⁺离子级联发射中第一步不实用的紫外或近紫外光子转换为Mn²⁺的红光发射.双掺杂样品SrB₄O₇:Pr³⁺,Mn²⁺与单掺杂样品SrB₄O₇:Pr³⁺的发射谱比较揭示出Pr³⁺→Mn²⁺的能量传递的确存在,并且提供了一种传递效率的估算方法,表明通过“Pr³⁺-Mn²⁺”组合有可能获得量子效率大于1的高效真空紫外激发发光材料.     

金属玻璃的断裂机理与其断裂韧度的关系

本文选取了三种不同断裂韧度值的金属玻璃Zr41.25Ti13.75Ni10Cu12.5Be22.5,Ce68Al10Cu20Co2和Fe41Co7Cr15Mo14Y2C15B6,通过压缩实验测量了它们的应力-应变关系;样品断裂以后观察了其断口形貌,发现这三种金属玻璃具有不同的断裂模式.经过对这三种金属玻璃做缺口三点弯曲实验,利用数字散斑技术研究了缺口前端应变集中方向弹性应变场的演化过程.根据金属玻璃的屈服准则,阐述了不同断裂韧度值的金属玻璃的断裂机理.     

Near-interface oxide traps in 4H–SiC MOS structures fabricated with and without annealing in NO

Near-interface oxide traps(NIOTs)in 4H–Si C metal–oxide–semiconductor(MOS)structures fabricated with and without annealing in NO are systematically investigated in this paper.The properties of NIOTs in Si C MOS structures prepared with and without annealing in NO are studied and compared in detail.Two main categories of the NIOTs,the"slow"and"fast"NIOTs,are revealed and extracted.The densities of the"fast"NIOTs are determined to be 0.76×10~(11)cm~(-2)and0.47×10~(11)cm~(-2)for the N_2 post oxidation annealing(POA)sample and NO POA sample,respectively.The densities of"slow"NIOTs are 0.79×10~(11)cm~(-2)and 9.44×10~(11)cm~(-2)for the NO POA sample and N_2POA sample,respectively.It is found that the NO POA process only can significantly reduce"slow"NIOTs.However,it has a little effect on"fast"NIOTs.The negative and positive constant voltage stresses(CVS)reveal that electrons captured by those"slow"NIOTs and bulk oxide traps(BOTs)are hardly emitted by the constant voltage stress.     

12CaO·7Al2O3/5CaO·3Al2O3：Sm3+新型红色荧光粉的制备及发光性质

采用自蔓延燃烧法制备了不同Sm³⁺掺杂浓度的12CaO·7Al₂O₃（C12A7：x%Sm³⁺）荧光粉。在404 nm近紫外光激发下,观察到了位于565,599,648 nm附近的3个光发射峰,分别归属于Sm³⁺的⁴G_5/2→⁶H_J/2（J=5,7,9）能级跃迁。随着Sm³⁺掺杂浓度增加,红光发射强度呈现了先增大后减小的规律,优化的Sm³⁺掺杂摩尔分数为1.5%,发光的浓度猝灭效应可归因于Sm³⁺之间发生了交叉弛豫过程。采取混相策略,通过降低初始粉体的煅烧温度至900℃获得了12CaO·7Al₂O₃/5CaO·3Al₂O₃：1.5%Sm³⁺（C12A7/C5A3：Sm³⁺）混相荧光粉,进一步提高了红光发射强度。利用变温光致发光谱计算得到混相样品的热激活能约为200 meV,结果表明该混相荧光粉具有良好的热稳定性。     

β-SiC单晶块体拉伸变形行为分子动力学研究

用分子动力学方法研究面心立方SiC(β-SiC)、C元素置换掺杂β-SiC单晶块体体系[001]向拉伸变形行为,对体系的拉伸断裂微观机理和5×10⁸/s,1×10⁹/s,1×10¹⁰/s三种应变速率下的力学行为进行分析.发现当拉伸应变量达到某个临界值后,Si-C sp³,C-C sp³键会分别向Si-C sp²和C-C sp²弱键转化.形成一定量sp²键后,β-SiC内部出现孔洞并发生断裂.由于C-C sp³键比Si-C sp³键更易向sp²弱键转化,导致C元素掺杂会降低SiC的强度、弹性模量和拉伸断裂应变.此外还发现此三种应变速率不影响β-SiC的杨氏模量,但影响其拉伸强度.     

ZBLAN玻璃中Pr3+掺杂离子3P0和1D2能级的发光特性和寿命

对ZBLAN氟锆酸盐玻璃中Pr³⁺掺杂离子³P₀和¹D₂能级的寿命和发光特性进行了较详细的光谱学研究。首先测量了两种掺杂浓度(质量分数分别为1×10^-3,5×10^-3)的Pr³⁺:ZBLAN玻璃的吸收光谱,然后运用时间分辨激光光谱技术测量了³P₀和¹D₂能级在激光单光子共振激发下的荧光发射谱和能级寿命。将不同荧光发射谱带的强度和文献报道的Judd Ofelt理论计算辐射跃迁几率数值做了比较分析,证明了文献中理论计算结果的可靠性。由于浓度猝灭效应,在相同的激发条件下,掺杂浓度为1×10^-3样品的荧光发射强度明显大于5×10^-3样品的荧光发射强度。但是从我们的测量结果看,掺杂浓度对³P₀和¹D₂ 的能级寿命值无显著影响。掺杂浓度为1×10^-3时,Pr³⁺离子³P₀和¹D₂能级的寿命值分别为46,322μ_s。     

2018年10期 电子期刊

采用自蔓延燃烧法结合高温热处理方法制备了镝离子掺杂浓度不同的七铝酸十二钙（12CaO·7Al₂O₃:x% Dy³⁺,C12A7:x% Dy³⁺） X射线荧光粉材料。实验发现,该系列荧光粉在350 nm激发下,可观察到位于486 nm和575 nm的两个发光峰,其分别来源于Dy³⁺离子的⁴F_9/2→⁶H_15/2和⁴F_9/2→⁶H_13/2跃迁。当镝掺杂摩尔分数为0.3%时,两个发光峰的发射强度最大。在氮气气氛下,1 300℃热处理C12A7:x% Dy³⁺荧光粉后,与未热处理样品相比,笼中OH^-基团减少,导致其光激励发光强度显著增大,并产生了更多的深陷阱。通过使用氮气气氛热处理后的C12A7:0.3% Dy³⁺粉末制成的成像板,以包覆有绝缘层细电线为成像目标,发现在合适的X射线吸收剂量下（0.54 Gy）,可以实现高质量的X射线成像。以上实验结果表明,镝掺杂的七铝酸十二钙X射线荧光粉材料在数字化静态X射线图像目标检测技术中有潜在的应用前景。     

Experimental optimum design and luminescence properties of NaY(Gd)(MoO_4)_2:Er~(3+)phosphors

Three-factor orthogonal design(OD) of Er~(3+)/Gd~(3+)/T(calcination temperature) is used to optimize the luminescent intensity of Na Y(Gd)(MoO_4)_2:Er~(3+)phosphor.Firstly,the uniform design(UD) is introduced to explore the doping concentration range of Er~(3+)/Gd~(3+).Then OD and range analysis are performed based on the results of UD to obtain the primary and secondary sequence and the best combination of Er~(3+),Gd~(3+),and T within the experimental range.The optimum sample is prepared by the high temperature solid state method.Photoluminescence excitation and emission spectra of the optimum sample are detected.The intense green emissions(530 nm and 550 nm) are observed which originate from Er~(3+)~2H_(11/2)→~4I_(15/2)and~4S_(3/2)→~4I_(15/2),respectively.Thermal effect is investigated in the optimum NaY(Gd~(3+))(MoO_4)_2:Er~(3+)phosphors,and the green emission intensity decreases as temperature increases.     

共沉淀法制备Y2O2S：Eu3+,Mg2+,Ti4+红色长余辉材料

用共沉淀法制备了Y₂O₂S:Eu³⁺,Mg²⁺,Ti⁴⁺红色长余辉材料。测量了材料的电子显微形貌、晶体结构和发射光谱。通过与固相法制备的Y₂O₂S:Eu³⁺,Mg²⁺,Ti⁴⁺长余辉材料比较,发现两种方法都可以制备粒度基本相同的纯相Y₂O₂S基质晶体,但共沉淀法样品的颗粒结构更松散。研究了Eu³⁺浓度对两种方法制备样品的谱线发射强度的影响,通过比较共沉淀法和高温固相法制备的样品中Eu³⁺的⁵D₁→⁷F₃较高能级跃迁的587.6nm谱线强度随Eu³⁺浓度的变化,发现共沉淀法更有利于Eu³⁺均匀进入Y₂O₂S基质晶格而形成有效的发光中心。     

Thermal stability and electrical transport properties of Ge/Sn-codoped single crystalline β-Zn_4Sb_3 prepared by the Sn-flux method

This study prepares a group of single crystalline β-Zn_4Sb_3 with Ge and Sn codoped by the Sn-flux method according to the nominal stoichiometric ratios of Zn_(4.4)Sb_3 Ge_xSn_3(x = 0–0.15). The prepared samples possess a metallic luster surface with perfect appearance and large crystal sizes. The microscopic cracks or defects are invisible in the samples from the back-scattered electron image. Except for the heavily Ge-doped sample of x = 0.15, all the samples are single phase with space group R3c. The thermal analysis results show that the samples doped with Ge exhibit an excellent thermal stability.Compared with the polycrystalline Ge-substituted β-Zn_4Sb_3, the present single crystals have higher carrier mobility, and hence the electrical conductivity is improved, which reaches 7.48×10~4S·m~(-1) at room temperature for the x = 0.1 sample.The change of Ge and Sn contents does not improve the Seebeck coefficient significantly. Benefiting from the increased electrical conductivity, the sample with x = 0.075 gets the highest power factor of 1.45×10~(-3)W·m~(-1)·K~(-2) at 543 K.     

Yb3+,Er3+共掺BaGd2ZnO5材料的制备及其上转换发光效率

采用溶胶-凝胶法制备了含有不同Yb³⁺,Er³⁺掺杂浓度的BaGd₂ZnO₅上转换发光材料,测量了这些样品在不同激发光密度下的上转换光发射功率及上转换效率。实验结果表明:在不同激发光密度下,所有样品的光发射功率都存在极大值,其中Yb³⁺掺杂摩尔分数为4%,Er³⁺掺杂摩尔分数为1%时样品的最大发射光功率可达20 mW;样品的上转换绝对效率也存在极大值,随着Yb³⁺和Er³⁺浓度增加,绝对效率的极大值向较低激发光密度方向移动,在Yb³⁺掺杂摩尔分数为9%,Er³⁺掺杂摩尔分数为3%时样品的上转换效率达到最高,绝对效率为3.2%,极值效率最大值为6.9%。     

Effects of W~(6+) occupying Sc~(3+) on the structure,vibration, and thermal expansion properties of scandium tungstate

We experimentally investigate effects of W~(6+)occupying the sites of Sc~(3+)in the unit cell of Sc_2 W_3 O_(12)(Sc_8 W_(12) O_(48))on the structure, vibration and thermal expansion. The composition and structure of the doped sample(Sc_6 W_2)W_(12) O_(48±δ)(with two W~(6+)occupying two sites of Sc~(3+)in the unit cell of Sc_8 W_(12) O_(48)) are analyzed and identified by combining the x-ray photoelectron spectroscopy and the synchronous x-ray diffraction with first-principles calculations based on density functional theory. Results show that the crystal with even W~(6+)occupying even Sc~(3+)in the unit cell is stable and maintains the orthorhombic structure at room temperature. The structure of the doped sample is similar to that of Sc_2 W_3 O_(12), and with even W occupying even positions of Sc in the unit cell and constituting the WO_6 octahedra. Raman analyses show that the doped sample possesses stronger W–O bonds and wider Raman linewidths than those of Sc_2 W_3 O_(12). The sample doped with W also exhibits intrinsic negative thermal expansion in the measured range of 150 K–650 K.     

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The molecular dynamics simulation of interaction between CH⁺ with various energy and fusion material tungsten is conducted. The simulated results show that in the incident process, the sputtering rates of C and H atoms change suddenly at the different exposure doses when the incident energy is 50, 100 and 150eV respectively, a few of W atoms are sputtered in the interaction process, but the sputtering rate is less than 0.24%. When the exposure dose is about 3.92×10¹⁶cm⁻², the incident energy is 50eV, a hydrocarbon firm without W atom is formed on the sample surface bombarded by the ions. A mixed film of W, C and H is formed at the other energy. The deposited rates of C and H atom first decrease then increase with the incident energy increament, the minimum deposited rats appear at 250 and 200eV respectively. The density profiles of C, H atoms, C−H, C−C, W−C bonds in the sample after bombardment move towards the inside of sample, and the C sp³ dominated the sample.     

Three-party reference frame independent quantum key distribution protocol

We present a three-party reference frame independent quantum key distribution protocol which can be implemented without any alignment of reference frames between the sender and the receiver. The protocol exploits entangled states to establish a secret key among three communicating parties. We derive the asymptotic key rate for the proposed protocol against collective attacks and perform a finite-size key security analysis against general attacks in the presence of statistical fluctuations. We investigate the impact of reference frame misalignment on the stability of our protocol, and we obtain a transmission distance of 180 km, 200 km, and 230 km for rotation of reference frames β=π/6, β=π/8 and β=0, respectively. Remarkably, our results demonstrate that our proposed protocol is not heavily affected by an increase in misalignment of reference frames as the achievable transmission distances are still comparable to the case where there is no misalignment in reference frames (when β=0). We also simulate the performance of our protocol for a fixed number of signals. Our results demonstrate that the protocol can achieve an effective key generation rate over a transmission distance of about 120 km with realistic 10⁷ finite data signals and approximately achieve 195 km with 10⁹ signals. Moreover, our proposed protocol is robust against noise in the quantum channel and achieves a threshold error rate of 22.7%.     

Probability of a ductile fracture

The present paper studies ductile fracture by a random fractal and calculates the fracture probability q of a ductile fracture. The fracture probability q is sensitive to the number n (microvoid size) and the probability p of forming microvoids. There are two critical probabilities p_c1 and p_c2. When pp_c2 = 1-1/n², the fracture probability q is 100%, the ductile fracture occurs with probability 1; when p_c2 > p>p_c1, there is a positive probability q (1>q>0), the fracture probability q increases with increasing probability p and/or decreasing number n; when p<p_c1, the fracture probability q is zero (in fact less than 0.00001), the fracture does not occur. The critical probabilities p_c1 and p_c2 increase with increasing n. When 1-1/n²>p>1-1/n, though a ductile fracture does not occur, there is at least a macrovoid which passes through the transverse plane of the specimen.     

三维自组装Eu3+-石墨烯复合材料的制备及其磁性研究

采用一锅水热法在180 ℃ 下制备三维Eu³⁺-石墨烯自组装复合材料. 通过X射线衍射、 扫描电子显微镜、透射电子显微镜表征了合成样品的物相及形貌特征. 结果表明: 合成的样品具有多孔性结构, 层与层之间堆叠成三维结构, 并且结果显示产物中没有Eu³⁺的团聚体. 经过拉曼光谱, 傅里叶红外光谱分析表明, Eu³⁺通过含氧官能团与石墨烯复合. 通过振动样品磁强计测定样品的磁滞回线, 对其磁学性能进行研究, 剥离顺磁信号后, 测得相应的矫顽力H_c ≈ 39.61 Oe(1 Oe=79.5775 A/m), 饱和磁化强度M_s ≈ 0.08 emu/g, 发现该产物具有弱的铁磁性, 与石墨烯相比, Eu³⁺的加入使得产物的铁磁性有较大提高. 关键词： 三维石墨烯 3+')" href="#">Eu³⁺ 水热法 磁性     

实验优化设计Sr_2MgSi_2O_7:Eu~(2+),Dy~(3+)的合成及长余辉特性

为了得到最长有效余辉时间的Sr_2MgSi_2O_7:Eu~(2+),Dy~(3+)荧光粉,应用二次通用旋转组合设计对实验进行全程优化,建立了稀土离子掺杂浓度Eu~(2+),Dy~(3+)和有效余辉时间的二元二次回归方程模型,应用遗传算法计算得到有效余辉时间的理论最大值.采用高温固相法合成了最优掺杂浓度Sr_2MgSi_2O_7:0.5mol%Eu~(2+),1.0mol%Dy~(3+)的荧光粉,在370nm激发下观察到了465nm的特征发射,这归因于Eu~(2+)的4f65d1—4f7跃迁.测量了最优荧光粉的热释发光特性,计算得到了陷阱深度为0.688eV,讨论了长余辉发光的特性.     

[Ca_(24)Al_(28)O_(64)]~(4+):4e~-电子化合物的制备及其电输运特性

金属氧化物电子化合物[Ca_(24)Al_(28)O_(64)]~(4+):4e~-(C12A7:e~-)因其天然的纳米尺度笼腔结构带来的新奇物理化学特性而在阴极电子源材料、超导和电化学反应等领域有着独特的应用价值.本文系统研究了以CaCO_3和Al_2O_3粉末为原料,采用固相反应-放电等离子烧结-活性金属Ti还原相结合的方法制备C12A7:e~-的工艺条件及其电输运特性.实验结果表明:在封装石英管真空度为10~(-5)Pa,还原温度为1100?C,还原时间为10—30 h条件下,成功制得载流子浓度为约10~(18)—10~(20)cm~(-3)的C12A7:e~-块体材料.第一性原理计算得到的C12A7:e~-能带结构和态密度表明,笼腔内的O~(2-)完全被e-取代后,C12A7:e~-费米能级明显穿过笼腔导带,说明位于笼腔内自由运动的电子使C12A7从绝缘体转变成导体,同时费米面附近的笼腔电子易于从笼腔导带跃迁至框架导带,在电场或热场的作用下电子更容易逸出,这也是C12A7:e~-逸出功低的主要原因.