Synthesis and Crystal Structure of 1,6:3,4-Bis(1,2-xylyiene) tetrahydro-imidazo[4,5-d]imidazole-2,5(1H,3H)-dione

The compound 1,6∶3,4-Bis(1,2-xylyiene)tetrahydro-imidazo[4,5-d]imidazole-2,5(1H,3H)-dione(C20H18N4O2, Mr=346.38) has been synthesized for the first time. Complete assignments were achieved by 1H NMR, IR, EI-MS, elemental analysis and single-crystal X-ray diffraction technique. The crystal belongs to monoclinic, space group P2(1)/n with a=10.266 0(16), b=11.298 5(18), c=1.452 20(20) nm, β=97.923(3), V=1.668 4(5) nm3, Z=4, Dc=1.379 g/cm3, μ(MoKα)=0.092 mm-1, F(000)=728, R=0.053 2 and wR=0.112 3 for 3632 observed reflections with I>2σ(I). X-ray analysis reveals dimeric aggregates are formed through hydrogen bond and offset π-π stacking. In addition, the compound assembles to a three-dimensional networking structure by other hydrogen bond.     

Synthesis and Crystal Structure of a Novel Molecular Clip from Diphenylglycoluril

The compound 1,6∶3,4-Bis(4,5-dimethyl)tetrahydro-3a,6adiphenylimidazo[4,5-d]imidazole-2,5(1H,3H)-dione (C40H40Cl0.33N4O10, Mr=748.58) has been synthesized for the first time. Complete assignments were achieved by using 1H NMR, IR, EI-MS, elemental analysis and single-crystal X-ray diffraction technique. The crystal belongs to Orthorhombic, space group C 2/c with a=29.280(4), b=11.861 7(16), c=1.921 2(3) nm, β=91.240(3), V=6.670 7(16)) nm3, Z=6, Dc=1.118 g/cm3, μ(MoKα)=0.092 mm-1, F(000)=3 146, R=0.0670 and wR=0.187 9 for 6551 observed reflections with I>2σ(I). X-ray analysis reveals that dimeric aggregates are formed through C-H…π interactions and and offset π-π stacking. In addition, the compound assembles to a three-dimensional network.ing structure by other hydrogen bond.     

非线性光学晶体MMTWMP的热学和光学性质的测定

报道了一种新型非线性光学晶体：二水合二N-甲基-(-吡咯烷酮合硫氰酸汞锰(MMTWMP)。用热重分析法、差示扫描量热法、吸光光度法、红外和粉末衍射光谱研究了它的热学和光学性质。它属于四方晶系，晶胞参数为α-1．21294，C=0．822.38nm，V=1．21127nm^3。MMTFMP晶体具有较好的物理化学稳定性。它的紫外截止波长为360nm。比硫氰酸汞锰，MnHg(SCN)4(MMTC)紫移了13nm。它在404nm的透过率为44．82％，比MMTC高了17．46％。     

Nonlinear optical and electrooptical effects in 2-methyl-4-nitro N-methylaniline (MNMA) crystals

Single crystals of 2-methyl-4-nitro-N-methylaniline (MNMA) have been grown from the melt. The crystal structure was determined (orthorhombic, Pna2_I (2 mm), Z=4, a =17.788(6) Å, b=11.893(4) Å, c=3.907(2) Å). The refractive indexes n_a and n_c were measured between 500 and 700 nm [ n_a(633 nm)=2.148(10), n_c(633 nm)=1.520(3)]. The nonlinear optical susceptibilities coefficients r ₃₁=8 pm/V and r₃₃=7.5 pm/V were determined. Most optical properties can be explained in terms of molecular orientation and polarizability     

MnQ2（Q=S,Se,Te）and [Mn（en）3]Te4 Structures and Their Semiconductor Properties

The solvo-thermal technique is used for the synthesis of [Mn(en)3]Te4 (I).The crystal structure has been determined by single crystal X-ray diffraction techniques.The crystal belongs to the monoclinic, space group p21/c with unit cell:a=0.8461(1),b=1.5653(2), c=1.4269(2)nm, α=90°,β=91.37(1) (3)°, γ=90°,V=1.8893(4)nm3,and Z=4.The results show that the structure contains a linear chain Zintl anion,[Te4]2-and a complex cation,[Mn(en)3]2+. Optical studies have been performed on the powder sample of I, suggesting that the compound is a semiconductor with a band gap of 0.73eV. The semiconductor properties for MnQ2(Q=S,Se,Te) and [Mn(en)3]Te4 have been discussed by molecular orbital theory.     

低温固相反应合成纳米Ba1-ySryTi1-xSnxO3

以TiCl4,SnCl4·5H2O,Sr(OH)2·8H2O和Ba(OH)2.8H2O为原料,采用低温固相反应合成了一系列纳米Ba1–yZnyTi1–xSnxO3(0≤x≤0.30,0≤y≤1.00)固溶体。XRD物相分析证明产品为立方晶系的完全互溶取代固溶体。TEM形貌观察,粒子为均匀球形,平均粒径50 nm。制陶实验发现,在BaTiO3纯相中掺入适量的Sn 4+和Sr2+,当(x=0.1,y=0.1)时,经1 150℃烧结的陶瓷片室温相对介电常数达到13 000,介质损失仅为0.008,烧结温度较之微米级粉体降低200～250℃。     

芴类衍生物有机电致发光器件中的激基复合物

利用紫外-可见光吸收光谱和荧光发光(PL)光谱,研究了新型芴类小分子材料2,3-bis(9,9-dihexyl-9H-flu-oren-2-yl)-6,7-difluoroquinoxaline(F2Py)的本征光谱特性,并制备了基于F2Py的有机电致发光器件(OLEDs),讨论了器件的电致发光(EL)光谱。结果表明,F2Py在溶液状态下的本征PL峰值位于452 nm,在薄膜状态下的本征PL峰值位于448 nm,而F2Py与NPB的混合物的PL发光峰在544 nm。在器件的EL光谱中,观察到了位于530~550 nm范围的激基复合物发光峰,以及来自F2Py与NPB激子发光的共同作用形成的位于430nm左右的肩峰。当F2Py层厚度为50 nm时,器件的启亮电压为17 V,最高亮度为58 cd/m2;而当F2Py厚度为20 nm并加入了Alq3(10 nm)做电子传输层(ETL)时,器件启亮电压为8 V,最高亮度为5030 cd/m2,EL性能大大提高。     

Gd_xY_(1-x)Ca_4O(BO_3)_3晶体非临界相位匹配产生1064nm三次谐波

通过研究生长不同Gd离子和Y离子配比组份的GdxY1 -xCa4 O(BO3) 3晶体 ,得到了室温下可以实现非临界相位匹配产生 10 64nm三次谐波的新型非线性光学晶体Gd0 .37Y0 .6 3Ca4 O(BO3) 3。报道了GdxY1 -xCa4 O(BO3) 3晶体实现10 64nm三次谐波的相位匹配角。用电光调Q的Nd∶YAG激光器对一块长 11mm ,Y 轴切割的Gd0 .37Y0 .6 3Ca4 O(BO3) 3晶体进行了转换效率的测量 ,其结果为 14 7%。     

Na_5Tm（WO_4）_4发光晶体的光谱特性研究

以Ｎａ２ＷＯ４为助熔剂，采用缓冷法成功地生长出新型发光晶体Ｎａ５Ｔｍ（ＷＯ４）４，晶粒尺寸为２ｍｍ×２ｍｍ×２ｍｍ。根据四方晶系面间距公式及最小二乘法，可以确定晶体的晶胞参数ａ＝１．１３８６ｎｍ，ｃ＝１．１２８３ｎｍ，测定并分析了该晶体室温下的红外光谱、吸收光谱、发射光谱及激发光谱。根据Ｊｕｄｄ－Ｏｆｅｌｔ理论计算了Ｔｍ３＋离子的吸收振子强度和配位场作用强度参数。结果表明该晶体有可能成为一类很重要的蓝色发光材料。     

激光蒸凝法制备氧化锰纳米粒子

以 15 0WCWCO2 激光器为光源 ,Mn(Ac) 2 ·4H2 O为靶材 ,采用激光蒸凝法制备出了氧化锰纳米粒子。初步研究了反应参数对纳米粒子性能的影响 ,并用X射线衍射、电子衍射、透射电镜等技术对纳米粒子的性能进行了表证 ,同时对纳米粒子的形成机理进行了初步探讨。实验结果表明 ,激光功率密度、反应压力、载气种类及流量等工艺参数对产品的粒度、晶型等性能均有影响。在惰性气氛下 ,产物主要是Mn3 O4 5 6F ,粒径分布范围较宽 (5～ 10nm和 30～ 10 0nm)且不均一 ;在氧气气氛下 ,产物主要是立方晶系的Mn3 O4 和少量的立方晶系的MnO ,粒径分布范围变窄了 (5～ 10nm和 15～ 6 0nm) ,也不均一。     

r(Nd)/r(Bi)对Ba0.75Sr0.25(NdxBi1-x)2Ti4O12微波陶瓷性能的影响

BaR2Ti4O12(R为稀土元素)系固溶体有很好的微波介电性能,尤其是Nd系材料有很高的介电常数(εr)和高品质因数(Q×f),该文研究了不同Nd/Bi比对Ba0.75Sr0.25(NdxBi1-x)2Ti4O12微波介质陶瓷结构性能的影响。当x=0.75时,即摩尔比x∶(1-x)=3∶1时(缩写为B13)有很好的介电性能:εr=118.5,Q×f=4 607(f=2.8GHz),谐振频率温度系数τf=-1.3×10-6℃-1。对不同Nd/Bi比的样品在1 250℃到1 400℃烧结3h后的陶瓷进行XRD分析后发现,陶瓷主相为BaNd2Ti4O12,有少量第二相Ba2Ti9O20。对Bi含量逐渐增加的陶瓷样品进行微观分析可知,Bi有助于致密度的提高和晶粒的增长,随着Nd/Bi比的减小,εr慢慢增大,τf渐渐趋向于0并向负方向移动,但同时降低了Q×f值。     

高效全固化钛宝石腔内倍频蓝光和四倍频紫外激光器的研究

用半导体抽运的Q开关YLF倍频激光器抽运钛宝石晶体，在平凹腔内加入组合的石英双折射滤光片压缩线宽，用LBO晶体腔内激发二次谐波，聚焦到BBO上产生四次谐波深紫外光。在抽运功率3．8w时，输出610mW．416nm蓝光。用长焦距的透镜聚焦二次谐波．得到64mW，208nm的紫外激光。基频光的谱线宽度是决定倍频效率的关键因素。实验观察到激光器的频谱宽度与双折射滤光片的带宽有一个数量级的差别，考虑到模式竞争和增益饱和效应，数值模拟了加入双折射滤光片后的钛宝石激光器的实际线宽，结果与实验中测量的数据基本一致。实验还分析了基频光的线宽对二次谐波效率的影响、二次谐波的线宽对四次谐波效率的影响、基频光的波长对四次谐波激发效率的影响。     

Synthesis,Structure, Electronic State,and Luminescent Properties of Novel Blue‐Light‐Emitting Aryl‐Substituted 9,9‐Di(4‐(di‐p‐tolyl)aminophenyl)fluorenes

Novel blue‐light‐emitting fluorene derivatives 5a–c and 7a–c containing bulky and highly emissive groups, namely pyrene, 10‐phenylanthracene‐9‐yl and 10‐(4′‐diphenylaminophenyl)anthracene‐9‐yl groups, as well as hole‐injecting/transporting triarylamines were synthesized. Single crystals of compounds 5a , 5c , 7a , and 7c were grown and their crystal structures were determined by X‐ray diffraction. The four fluorene derivatives have nonplanar molecular structures, which reduce the intermolecular interaction and the likelihood of molecular aggregation or excimer formation. No unwanted long‐wavelength emission was observed in the photoluminescence (PL) spectra of the 5a–c and 7a–c thin films. Their PL spectra reveal excellent thermal stability after annealing treatment under air and ambient light. All of the six compounds show high fluorescence quantum yields and outstanding thermal stabilities. The 2‐aryl and 2,7‐diaryl substituents at the fluorene molecule have a significant effect on the photophysical properties and the thermal characteristics. The six compounds show almost the same energy levels for the highest occupied molecular orbitals (HOMOs) of about ?5.20 eV, which allows effective hole injection. The C2‐ and C7‐aryl substituents play a relatively less‐important role in the HOMO energy levels, which depend mainly on the triphenylamino groups at the C9 position. The molecular orbitals, excitation energy, and emission energy were calculated to explain the real origin of their photophysical characteristics. The HOMOs are mainly localized on the triphenylamino groups at the C9 position, while the lowest unoccupied molecular orbitals (LUMOs) have a significant orbital density at the C2‐ and/or C7‐aryl substituents. Pure‐blue‐light‐emitting diodes based on 2,7‐diaryl‐9,9‐di(triarylamino)fluorenes were fabricated.     

复合助烧剂对CaO-BaO-Li_2O-Sm_2O_3-TiO_2陶瓷低温烧结和性能的影响

采用传统固相反应法制备了CaO-BaO-Li_2O-Sm_2O_3-TiO_2(CBLST)陶瓷。研究了复合添加BaCu(B_2O_5)(BCB)和Li_2O-B_2O_3-SiO_2(LBS)对CBLST陶瓷的烧结特性、微观组织、相组成及介电性能的影响。结果表明:添加质量分数w(BCB)=60%和w(LBS)=0.5%～5.0%的CBLST陶瓷的相组成未改变,仍为正交钙钛矿相和BaSm_2Ti_4o_(12)(BST)相。通过添加w(BCB)=6.0%和w(LBS)=0.5%,可以使CBLST陶瓷的烧结温度从1325℃降到1050℃,并且在1050℃烧结2h的CBLST陶瓷介电性能优良:ε_r=81.9,tanδ=0.0062,τ_f=–3.75×10~(–6)/℃,其tanδ比纯CBLST陶瓷的tanδ(0.016)明显降低。     

GaAs抛光片腐蚀过程初步研究

采用Ｘ射线衍射、Ｘ射线双晶衍射和Ｘ射线荧光三种手段对经Ｈ２ＳＯ４：Ｈ２Ｏ２：Ｈ２Ｏ＝１６：１：１和３：１：１腐蚀液,在不腐蚀条件下得到的ＧａＡｓ片子进行近表层结晶完整性、片子表面的残留产物以及发射二次Ｘ射线情况测量,并初步分析了这些数据。     

Novel Bi-substituted Yttrium Iron Garnet Film／Crystal Composite for Magneto-optical Applications

The novel Bi-substituted rare-earth iron garnet films were grown by the modified liquid phase epitaxy (LPE) technique for use as a 45° Faraday rotator in optical isolators. First, single crystals of Y3 Fe5 O12(YIG), with a lattice constant of 1. 237 8 nm, were grown by means of the Czochralski method. Using the seed crystal of YIG instead of the conventional non-magnetic garnet of Gd3Ga5O12 (GGG) as a substrate,a film of BiYbIG was grown by means of the LPE method from Bi2O3 - B2O3 fluxes. The structural, magnetic and magneto-optical properties of BiYbIG LPE film/YIG crystal composite have been investigated using directional X-ray diffraction (XRD), electron probe microanalysis (EPMA), vibrating sample magnetometer (VMS) and near-infrared transmission spectrometry. The saturation magnetization 4πMs has been estimated to be about 1.2×10 6 A/m. The Faraday rotation spectrum was measured by the method of rotating analyzer ellipsometry (RAE) with the wavelength varied from 800 nm to 1 700 nm. The resultant Bi0.37 Yb2.63 Fe5 O12LPE film/YIG crystal composite showed an increased Faraday rotation coefficient due to doping Bi3 ions into the dodecahedral sites of the magnetic garnet without increasing absorption loss, therefore a good magnetooptic figure of merit,defined by the ratio of Faraday rotation and optical absorption loss, has been achieved of 21.5 and 30.2 (°)/dB at 1 300 and 1 550 nm wavelengths respectively and room temperature. Since Yb3 and Y3 ions provide the opposite contribution to the wideband and temperature characteristics of Faraday rotation,the values of Faraday rotation wavelength and temperature coefficients were reduced to 0.06 %/nm and 0.007(°)/℃ at 1 550 nm wavelength, respectively.     

Pr~(3+)离子及Na_5Pr(WO_4)_4晶体的光谱性质

本文报道了新型发光晶体Na_5Pr(WO_4)_4的生长及Pr~(3+)离子的光谱性质。测定了该晶体的结构以及吸收光谱、荧光光谱和激发光谱。研究表明,该晶体有可能成为继Na_5Nd(WO_4)_4晶体之后又一激光晶体新品种。     

用于红外激光传输及光纤传感应用的矩形Y_2O_3-ZrO_2单晶光波导

通过精确的切割和良好的抛光 ,从Y2 O3 稳定的ZrO2 块状单晶制得可用于红外激光传输及光纤高温传感的高品质Y2 O3 ZrO2 单晶矩形光波导 .获得的矩形波导截面大于 1mm× 1mm ,长度在 4 5mm～ 6 5mm之间 .波导的光学性能比用常规LHPG系统生长的Y2 O3 ZrO2 单晶光纤优越得多 ,在 90 0nm波长处的光学损耗小于 0 .0 3dB cm ,对 1.0 6 μmNd :YAG激光脉冲的损伤阈值为 0 .98MW cm2 ,并且能耐受 2 30 0℃的高温 .实验结果表明 ,这些波导有望在红外激光传输和 2 0 0 0℃以上的高温光纤传感等领域得到应用 .     

A new organic electrooptic crystal:2,6-dibromo-N-methyl-4-nitroaniline (DBNMNA)

A new organic electrooptic crystal, 2,6-dibromo-N-methyl-4-nitroaniline, is reported. The crystal structure was determined by X-ray diffraction (orthorhombic, space group Fdd2, point group mm2, Z=16, a=11.745 Å, b=29.640 Å, c=10.807 Å). The refractive indexes were measured at several wavelengths between 500 and 1100 nm (at 632.8 nm, n_a=1.90, n_b=1.62, and n_c=1.48) and fit the data to a single oscillator Sellmeier equation. A report is presented on measurements of the linear electrooptic effect, yielding the combined coefficients n_a ³r₁₃-n_c³ r₃₃, as well as the first known measurements of the quadratic electrooptic effect in an organic crystal, yielding the coefficients r₄₂ and r₅₁ at 514.5, 632.8, and 810 nm. Good agreement is found between the observed dispersion in the electrooptic coefficients and that predicted by the simple two-level dispersion model     

Au点阵模板控制生长ZnO堆垒单晶棒

采用磁控溅射技术在Si(111)衬底上溅射Au薄膜,900℃退火生成Au点阵模板,在Au点阵模板上溅射ZnO薄膜,O2气氛下1 000℃退火制备了ZnO堆垒单晶棒。研究了不同直径Au点阵模板对ZnO单晶棒结构性能的影响。采用扫描电镜(SEM)、高分辨透射电子显微镜(HRTEM)、X射线衍射(XRD)、X射线光电子能谱(XPS)对样品结构形貌进行了分析。结果表明,生成有序排列的ZnO棒均由诸多六方纤锌矿单晶堆垒而成,较小Au点阵生成单晶棒的直径约为100nm。室温光致发光PL谱表明在376nm出现一个较强近紫外发射,在488nm附近出现一个较宽的深能级绿光发射,说明所制备样品具有良好的发光特性。