Synthesis and Photoluminescence of New Europium Complex Eu(DBM)_3(DPPZ) with Dipyridophenazine Ligand

Dipyrido [3, 2-a:2,3-c] phenazine moiety has been introduced as neutral ligand in europium complex. Therefore, a new europium complex with saturated emission, strong fluorescent intensity and good solubility was designed and synthesized for the first time. Its photoluminescence and UV properties were examined. The experimental results showed that this new Eu-complex could be used as red electroluminescent materials.

Red Electroluminescence and Photoluminescence from Novel Binuclear Europium Complex with Squaric Acid Ligand

A novel binuclear europium P-diketone complex with squaric acid ligand was synthesized for the first time. Its structure was elucidated by IR, UV, and Elemental Analysis. Red light emitting diode (LED) was fabricated by using the novel europium complex as an emitting layer, tris(8-quinolinolate) aluminum (III) (Alq(3)) as an electron-transporting layer, N, N'-diphenyl-N, N'-(3-methylphenyl)-1,1'-biphenyl-4,4'-diamine (TPD) as a hole-transporting layer. A cell structure of indium-tin-oxide/TPD/Eu-complex/Alq(3)/Mg: Ag was employed. Red electroluminescence was observed at room temperature with dc bias voltage of 2 V in this cell. 2 Red emission peaks at about 613 nm with maximum luminance of over 106 cd/m(2). Compared with the EL luminance from those europium complexes reported before, one from the Eu-complex is best in the same cells.

Red Mechanoluminescence and Photoluminescence from Novel Europium Complexes

Two new binuclear (europium and lanthanum) beta-diketone complexes Eu0.9La0.1(TTA)(3)Phen and Eu0.5La0.5(TTA)(3)Phen in which Phen is 1,10-phenanthroline, TTA is an anion of thenoyltrifluoroacetone (HTTA) were synthesized for the first time. They showed intense photoluminescence (PL) and mechanoluminescence (ML), and had their maximum PL and ML spectra peaked at 613.5 nm with half bandwidth of 10 nm respectively. Their PL and ML intensity were obviously stronger than these from Eu(TTA)(3)Phen. It is considered that binuclear (europium and lanthanum) beta-diketones complexes are promising ML and PL materials.

Photoluminescence and Ce^(3+)→Tb^(3+)→Eu^(3+) Energy Transfer Processes of the Ce^(3+)/Tb^(3+)/Eu^(3+)-doped β-NaYF_(4) Phosphors with Broadened Excitation Spectrum

Ce^(3+)/Tb^(3+) co-doped and Ce^(3+)/Tb^(3+)/Eu^(3+) tri-doped β-NaYF_(4) photoluminescent microcrystals using oleic acid as surfactant were synthesized using the solvothermal method.Their microstructural characteristics and photoluminescence properties were investigated in detail.They have the shape of hexagonal prism bipyramids with uniform particle size,which decreases with the concentrations of Tb^(3+) and Eu^(3+).The energy transfer processes of both the Ce^(3+)→Tb^(3+) and the Ce^(3+)→Tb^(3+)→Eu^(3+) were systematically studied.Compared with Eu^(3+) or Tb^(3+) single-doped β-NaYF_(4) microcrystals,the sensitization by Ce^(3+) for the photoluminescence of Tb^(3+) and Eu^(3+) leads to a broad excitation spectral bandwidth in the ultraviolet (UV) range.Meanwhile,the corresponding optical absorption efficiency is greatly enhanced.High energy transfer efficiencies have been observed from Ce^(3+) to Tb^(3+) and from Tb^(3+) to Eu^(3+).

Sol-gel Synthesis and Photoluminescence of InP Nanocrystals Embedded in Silica Glasses

III-Vsemiconductor nanocrystals rarely exist as spherical inclusions inside glasses, due to difficulties during their preparation, such as high toxic reagents or fast oxidation under usual glass technology temperatures. In this article a sol-gel method for synthesis of InP nanocrystals embedded in silica glasses was described. Gels were synthesized by hydrolysis of a complex solution of Si(OC 2 H 5 ) 4 , InCl 3 4H 2 O and PO(OC 2 H 5 ) 3 . Then, the gels were heated at 600 o C in the presence of H 2 gas to form fine cubic InP crystallites. Raman spectrum showed InP longitudinal-optic mode (342cm -1 ) and transverse-optic mode (303cm -1 ). The size of InP nanocrystals was found to be from 2 to 8 nm in diameter by transmission electron microscopy. A strong photoluminescence with peaks at, 606, 730nm 856 nm was observed from 3InP/100SiO 2 nanocompositions. The temperature-and excitation power-dependent PL spectra from the nanocomposition are measured in order to confirm the origin of the PL spectra. These behaviors of the three peaks emissions suggest that 606, 733, and 856 nm emissions do not have the same origin. The PL with peak at 856nm arise from the cubic InP nanocrystallites embedded in the SiO 2 gel glasses. The 605 and 732 nm emissions may arise from the SiO 2 gel glass matrix or the interface between the InP crystallite core and SiO2 glass matrix.

Synthesis and photoluminescence properties of Nd_2O_3 nanoparticles modified by sodium bis(2-ethylhexyl) sulfosuccinate

This paper reports that Nd2O3 nanoparticles modified by AOT（sodium bis（2-ethylhexyl） sulfosuccinate） were prepared using microemulsion method in the system of water and propanol/AOT/toluene. Transmission electron microscopy shows that the Nd2O3 nanoparticles take the shape of sphere with 18 nm and 31 nm with different preparation. The organic sol of Nd2O3 nanoparticles is very stable at room temperature. X-ray diffraction results show that the product has hexagonal phase structure. Two ultraviolet emission band at 344 nm and 361 nm corresponding to the transition of ^4 D3/2→4 I9/2 and 2P3/2→^4I 11/2 or ^4D 3/2→ ^4 I 13/2 were observed.

基于UV-Vis漫反射、Raman与PL光谱联用技术在黄色珍珠无损检测中的应用

应用紫外-可见(UV-Vis)漫反射、拉曼(Raman)与光致发光(PL)光谱就当前市售的大小各异、金色饱和度深浅不一的珍珠其致色属性予以对比分析。结果表明:基于珍珠UV-Vis漫反射光谱特征的差异将金黄色珍珠初分为两种类型:Ⅰ型珍珠其谱图在(360±5) nm处存在吸收带、在(420±10) nm处存在较弱的吸收峰或肩,该类珍珠为当前珍珠销售市场较为常见的自身致色珍珠;除Ⅰ型珍珠外,将其他金黄色系珍珠归属为Ⅱ型,其对应的UV-Vis反射光谱主吸收峰可位于340~430 nm区间,部分Ⅱ型样品在280~600 nm无明显吸收或仅存在较弱的吸收肩。进一步就Ⅱ型珍珠予以Raman光谱检测,在激发强度较低时经处理的Ⅱ型黄色珍珠在150~1 000 cm^(-1)区间可产生较强的荧光峰,且荧光峰的强度明显高于文石约1 086 cm^(-1)处的特征峰。同时,上述经处理的Ⅱ型珍珠对应的PL光谱同样表明在500~600 nm区间的荧光强度显著增大。此外,部分经处理的珍珠其Raman或PL光谱中可见与珍珠组成成分无关的特征峰位。上述珍珠的Raman与PL光谱中出现的异常荧光与外来特征峰可作为珍珠经处理的佐证依据。课题工作为当前金黄色珍珠颜色的形成属性及仿珍珠的鉴定提供理论与技术支撑,同时对于Raman光谱在其他类宝玉石、特别是有机宝石的检测鉴定中具有重要的借鉴意义。

Synthesis,Crystal Structure and Photoluminescence of Ethyl Coumarin-3-carboxylate Derivatives

The ethyl coumarin-3-carboxylate （1） and its two derivatives, ethyl 7-methoxy-2- oxo-2H-chromene-3-carboxylate （2） and ethyl 7-（3-methylbut-2-enyloxy）-2-oxo-2H-chromene-3- carboxylate（3）, were synthesized, characterized and their UV-vis spectra and photoluminescence were investigated. Compound 2 crystallizes in the monoclinic system with space group C2/c, a = 25.884（4）, b = 6.8365（11）, c = 13.816（2） A, β = 104.876（2）°, V= 2362.9（7） A3, Z = 8, Dc= 1.396 g/cm3, Mr. = 248.23, F（000） = 1040 and g = 0.108 mm-1. Compound 3 crystallizes in the monoclinic system with space group P21/c, a = 15.685（6）, b = 8.373（3）, c = i3.063（5） A, β = 111.862（6）°, V= 1592.2（10） A3, Z = 4, Dc = 1.261 g/cm3, M,.= 302.31, F（000） = 640 and p = 0.093 mm^-1. Both the absorption and emission of the two derivatives were stronger than that of ethyl coumarin-3-carboxylate due to the larger conjugation of their electron donor group moiety at the 7-position. Under ultraviolet light excitation, the two derivatives exhibit strong blue-violet emission.

Intense Yellow Photoluminescence from Silicon Oxynitride Films Prepared by Dual Ion Beam Sputtering

In this work, results on the study of the structure and photoluminescence (PL) properties of SiOxNy thin films are presented. The films were deposited at room temperature using a dual-ion-beam co-sputtering system. The XRD and TEM results show that the deposited films have an amorphous structure. In the XPS result, we find N 1s spectra consist of one symmetric single peak at 397.8 eV, indicating that the nitrogen atoms are mainly bonded to silicon. It is in agreement to the result of FTIR. In SiOxNy films, an intense single PL peak at 590 nm is observed. Furthermore, with the increase of the N content in the SiOxNy films, the intensity of the PL peak at 590 nm increases a lot. The PL peak of 590 nm is suggested to originate from N-related defects.

Silicon carbide nanotubes with special morphology prepared by super critical hydrothermal method and photoluminescence character

Silicon carbide nanotubes（SiCNTs） with special morphology synthesized by supercritical hydrothermal method at 470 C and 8 MPa have been reported in this paper.SiCNTs with special morphology were characterized by transmission electron microscopy（TEM） and high-resolution TEM（HRTEM）.There are two kinds of silicon carbide with special morphology：One is oval SiCNTs with small aspect ratio,the other is bamboo cone-shape structure.SiCNTs have been analyzed by fluorescence spectrometer.The results indicate that the SiCNTs have strong photoluminescence（PL） property.The SiCNTs with oval shape are one kind of intermediate state of growth process of nanotube.The growth mechanism of silicon nanotubes has been proposed based on experiment data.The investigations of growth mechanism of SiCNTs with bamboo structure show that the defect produced in the growth process play the important role in SiCNTs with special structure.

Ethoxycarbonylmethyl Viologen Induced Metal Halide-based Hybrids:Structures,Photoluminescence and Photocurrent Response Behavior

Two new ethoxycarbonylmethyl viologen induced metal halide-based hybrids,(Ae V)(BiI)(DMF)(1)and(Ae V)(CoCl)(2)(AeV=N,N?-bis(ethoxycarbonylmethyl)-4,4?-bipyridinium)have been synthesized and structurally determined by X-ray diffraction method.Under the direction of a new template AeV,the(BiI)tetramer constructed from four edge-sharing BiIoctahedra(for 1)and(CoCl)mono-nuclear(for 2)were obtained.Furthermore,C–H···O and C–H···X(X=I,Cl)hydrogen bonds contribute to the extension of structures from 0-D to 1-D chains.Their energy band gaps of 2.18 and 2.41 eV indicate their semiconductor properties,and the photoluminescence was detected on 1.Interestingly,2 exhibits good photocurrent response behavior.Electronic structure analysis was executed to correlate the structure/property.

基于近红外监测系统的天麻素干预糖尿病脑损伤显微组织的研究及HPLC法验证

目的糖尿病脑损伤早期病灶定位诊断和药物治疗难度大,本研究拟建立基于近红外监测系统的脑组织天麻素及其代谢物含量定量校正模型和脑中枢神经不同部位判别模型,并运用高效液相色谱(HPLC)技术对其进行验证。方法选用SPF级雄性昆明小鼠为对象构建糖尿病模型并观察组织病理学改变,利用近红外监测系统监测小鼠脑组织,并测定药物含量;使用偏最小二乘算法(PLS)及判别分析(DA)建立天麻素干预糖尿病鼠脑组织模型并进行比较研究,运用DAS2.0软件评价天麻素在脑中枢不同位置的药代动力学相关参数。结果以动物实验体外模型验证成功为基础,基于PLS算法的脑组织天麻素GAS及其代谢物对羟基苯甲醇HBA含量定量校正模型R_(p)和RMSEP分别为0.9579、3.28及0.9020、2.68;DA分析模型能够对脑中枢不同病变组织进行正确的分类,且近红外监测系统监测和HPLC法得到药代动力学相关参数无统计学差异,方法学验证表明所建立的分析方法具有较好的精密度、重现性和稳定性。结论本研究为探讨近红外监测系统作为快速判定脑中枢神经组织病灶位置和实时药代动力学研究新方法提供实验数据基础,具有广阔的应用前景。

Detection of Chlorpyrifos Residues in Akesu Red Fuji Apple based on Near Infrared Spectrum

[Objective] The paper was to explore a method for detecting chlorpyrifos residues in red Fuji apple. [Method] The original spectral data of apple samples sprayed with different volume fractions of chlorpyrifos were collected using near infrared spectrometer at the band of 4 000-10 000 cm^（-1）. The original spectra were pre-treated by a variety of methods, and partial least squares（PLS） model was established for predictive analysis. [Result] Near infrared spectrum showed sensitivity to apple samples sprayed with different volume fractions of chlorpyrifos, but had low precision on pesticide-free samples. Data of blank control group were further eliminated for modeling prediction. The results showed that the results were the best when pre-treated with first derivative（FD）： R=0.987 9; the square error of prediction（SEP） was 0.173 6; the root-mean-square error of cross-validation（RMSECV） was 0.120 5; and the precision was 0.923 4. [Conclusion] Near infrared spectrum can better predict chlorpyrifos residue, providing a new method for detecting chlorpyrifos residues in Akesu red Fuji apple.

基于近红外的PLS量化模型鉴定西湖龙井真伪的研究

对西湖龙井进行原产地精确鉴定是规范市场,打击假冒伪劣的迫切需求。文章利用近红外技术对西湖龙井的真伪鉴定进行了研究,提出了一种模型以进行西湖龙井鉴别的新方法。结果表明,利用西湖龙井茶和其他地区以龙井加工工艺制成的扁形茶全区域的近红外原始光谱,分别对其进行赋值,采用PLS法建立了西湖龙井的预测模型(主成分数为15),通过预测值和西湖龙井的临界值进行比对实现了对西湖龙井的真伪的准确鉴定。对70份定标样品和24份外部验证未知样品鉴定结果的准确率都达到了100%,证明利用定量分析的PLS法建立的模型能有效准确地进行西湖龙井的真伪鉴定。

纳秒脉冲激光制备黑硅及其光学性能的研究

利用纳秒脉冲激光器在常温常压室内环境下扫描刻蚀单晶硅片,通过改变扫描方式和扫描的线间距制备了各种不同结构的黑硅样品,重点研究了扫描方式、扫描间隔、高温吹氧退火时间等对黑硅光致发光(PL)特性的影响,以及不同参量制备的硅表面微结构对光吸收率的影响。利用透射电子显微镜、扫描电子显微镜、光学显微镜、拉曼和荧光光谱仪、吸收光谱仪等对制备的黑硅样品形貌、光吸收和PL发光特性进行了检测与表征,获得了吸收率高于90%且具有良好发光性能的黑硅结构样品。研究发现,采用线性扫描方式制备的黑硅样品的PL光谱主要分布在红光波段,而采用正交扫描方式制备的黑硅样品的PL光谱中在近红外900 nm附近有稳定的发光峰;此外,在黑硅样品中还观察到630 nm附近的电子局域态发光,并通过建立对应的物理模型解释了其发光机理。

高脉冲功率能量PLD法制备MgZnO薄膜中的沉积机理

用PLD法成功制备了一系列高质量的MgZnO薄膜。实验中发现高脉冲能量沉积薄膜的结构和发光特性随基片温度的变化规律与低脉冲能量下的结果不一样:基片在室温时高脉冲能量制备薄膜的XRD峰的半峰全宽比高基片温度时的结果相对更小;AFM显示其颗粒变大,柱状生长突出;PL谱紫峰与绿峰强度比最大,结晶质量反而提高。另一方面,与低脉冲能量时相反,增大氧气压强后高脉冲能量沉积的薄膜XRD半峰全宽变窄。结合实验现象和表征,合理解释了高脉冲能量沉积的机理。室温制备高质量MgZnO薄膜的PLD沉积机理对于以后在柔性衬底上沉积薄膜的研究有重要的参考价值。

天然红独玉与染色红独玉光谱学特征及其差异性研究

针对产自河南南阳的天然红独玉及经过染色处理的红独玉,分别开展了常规宝石学特征测试、红外光谱测试、拉曼光谱测试、紫外-可见吸收光谱测试、电子顺磁共振波谱测试及光致发光光谱测试,以揭示两者的物质组成差异、颜色成因差异及科学鉴定特征。分析结果显示,染色红独玉折射率及相对密度值均较为集中,与斜长石较为接近;天然红独玉在不同位置显示斜长石及黝帘石两个折射率值。红外光谱结合拉曼光谱分析表明天然红独玉粉色部分与黝帘石特征谱峰一致,表明黝帘石化程度较高,白色及绿色部分则以基性斜长石为主;染色红独玉黝帘石化程度低,因此常规宝石学参数与斜长石较为接近,常需染色处理,显示黄白色长波紫外荧光异常。天然样品紫外光谱显示522 nm附近的宽缓吸收带,揭示Mn为天然红独玉粉色的主要致色原因;电子顺磁谱进一步揭示出Mn^(2+)的六重超精细结构,为八面体场中Mn^(2+)的^(6)A_(1)→^(4)T_(1)(^(4)G)自旋禁戒跃迁。而染色红独玉则显示549 nm附近的染色剂吸收,并与光致发光光谱中578~589 nm处强发光中心相呼应。紫外荧光灯、紫外-可见光谱及光致发光光谱可视为天然红独玉与染色红独玉有效的无损检测方法。

基于BP-ANN和PLS的近红外光谱无损检测李果实品质的研究

可溶性固形物(SSC)和可滴定总酸(TA)含量是影响李果实品质的重要指标,经典的破坏性检测方法不适用于果实按品质分级,近红外光谱(NIRS)检测方法具有速度快、操作简便、可无损检测果实品质。为实现NIRS无损快速检测安哥诺李果实可溶性固形物和可滴定总酸含量,利用NIRS采集李果实的漫反射光谱,同时采用糖度计测定安哥诺李果实的SSC,采用滴定法测定了李果实TA含量,使用杠杆值和F概率值剔除异常样品,采用软件优化结合人工筛选光谱波段,使用了消除常数偏移量、减去一条直线、矢量归一化(SNV)、最大-最小归一化、多元散射校正(MSC)、一阶和二阶导数结合平滑处理、一阶导数结合减去一条直线和平滑处理、以及一阶导数结合SNV或MSC校正等光谱预处理方法,分别采用偏最小二乘法(PLS)和主成分分析结合反向传播人工神经网络(BP-ANN)建立李果实SSC、TA的定量分析模型。结果表明,李果实SSC和TA的最佳PLS建模效果波段范围分别为4000~8852和4605~6523 cm^(-1)。SSC的PLS模型的最佳光谱预处理方法为MSC校正,最佳模型校正相关系数(R_(c))为0.9144,预测相关系数(R_(p))为0.8785,校正均方根误差(RMSEC)为0.91,预测均方根误差(RMSEP)为1.00。经一阶微分结合SNV和9点平滑的方法预处理后,TA的PLS模型效果最佳,R_(c),R_(p),RMSEC,RMSEP分别为0.8603,0.8196,0.80和0.86。提取了李果实SSC和TA光谱数据的主成分,并基于前10个主成分得分建立了李果实SSC和TA最佳BP-ANN定量分析模型,其R_(c),R_(p),RMSEC和RMSEP分别为0.9767,0.8897,0.75和0.99;TA的BP-ANN模型的相应参数值依次为0.9743,0.8977,0.62和0.83,与采用PLS算法建立的定量模型相比较,BP-ANN模型具有较高的R_(c),R_(p)和较低的RMSEC,RMSEP,因此BP-ANN模型对SSC和TA指标的定量分析结果更佳。

PLS-DA优化模型的马铃薯黑心病可见近红外透射光谱检测

马铃薯黑心病是一种马铃薯主要内部缺陷,严重损害薯条、薯片、全粉等加工制品的质量和产率。目前对马铃薯的分级主要侧重于外部品质检测,针对内部缺陷检测的研究很少。旨在开发一种马铃薯黑心病的快速无损检测技术,为此搭建了马铃薯可见近红外透射光谱分析平台,分析健康与黑心病马铃薯的透射光谱特性并优化光谱判别模型参数。基于现有马铃薯分级线和复享PG2000高速光谱仪,采用左右透射方式(光源与光纤探头位于分级线果盘左右两侧),采集470个马铃薯(其中健康薯234个、黑心薯236个)的透射光谱图,建立偏最小二乘判别模型(PLS-DA),并利用主成分分析(PCA)与光谱形态特征相结合的方法选择特征波长,优化模型。分析发现,健康薯与黑心薯的可见近红外透射光谱在吸光度值和光谱形态特征方面均存在明显区别。黑心薯的平均光谱吸光度值高于健康薯(650~900 nm范围内),但黑心薯的平均光谱曲线较为平缓,无明显吸收峰,而健康薯平均光谱曲线在665,732和839 nm附近有明显吸收峰,并且健康薯与黑心薯的平均光谱差值在705 nm处达到最大值。基于PLS-DA法建立了马铃薯黑心病判别模型,对黑心病的判别效果显著,分类器特性曲线(ROC)下面积(AUC)值为0.9942,黑心薯识别总正确率能够达到97.16%,RMSE CV和RMSE P分别为0.28和0.26。此外,成功利用PCA与光谱形态特征相结合的方法对模型进行简化,最终得到由6个波长(658,705,716,800,816和839 nm)组成的特征波长组合,简化后的模型总正确率能够达到96.73%,接近全波段模型判别水平。研究表明,左右透射的方式能够准确识别黑心马铃薯,实现对马铃薯内部缺陷的快速无损检测。对我国马铃薯产业的发展起到一定的促进作用,为马铃薯内部缺陷在线检测技术的提高提供了重要的理论基础和实践依据。

基于多元散射校正和偏最小二乘(MSC/PLS)的傅里叶变换近红外光谱检测蜂蜜中还原糖

为快速无损测定蜂蜜的还原糖,提出一种用近红外光谱技术进行检测的新方法。选用SN/T0852——2000铁氰化钾滴定法作为光谱还原糖测定的标定方法,用不同光谱预处理方法对模型的影响进行比较。首先用MSC对光谱数据进行校正,在经过Norris导数平滑法对原始光谱进行预处理消除噪声。利用光谱专用分析软件TQAnalyst7.2,建立偏最小二乘(PLS)校正模型。最优光谱模型校正相关系数(R)、校正相关均方差(RMSEC)、预测相关均方差(RMSEP)、交互验证相关系数(RCV)、交叉验证均方差(REMSECV)分别为0.97056,1.21,1.54,0.96267,1.36。结果表明,应用多元散射校正(MSC)处理,并经过Norris二阶导数平滑后的PLS模型优于经典PLS算法所建立的模型。