一种离子型铱磷光配合物的合成及表征

以2-苯基吡啶(ppy)为环金属配体、4,4''-二叔丁基-2,2''-二吡啶(Dtbbpy)为N^N辅助配体,PF6^-为对阴离子,合成了一种离子型磷光配合物[Ir(ppy)2(Dtbbpy)]⁺PF6^-,产率为91.0%。通过元素分析(EA)、红外光谱(IR)、核磁共振谱(¹H-NMR和¹³C-NMR)和质谱(MS)对其组成和化学结构进行了确认和表征。采用紫外可见光谱(UV-Vis)和光致发光光谱(PL)研究了其光物理性能,该配合物在二氯甲烷中的最大发射波长为557 nm,属于黄绿光发射离子型铱磷光配合物。     

黄光铱配合物Ir(dmppy)2(popy)的合成及光物理性能研究

设计合成了一种新的中性铱磷光配合物Ir(dmppy)2(popy),该配合物以2,4-二(3,5-二甲基苯基)吡啶为环金属配体,2-(2-羟基苯基)吡啶为辅助配体。通过核磁共振氢谱和碳谱(¹H-NMR、¹³C-NMR)确证了配合物的化学结构,采用光致发光光谱和紫外可见光谱研究了配合物的光物理性能,采用热分析研究了配合物的热稳定性。该配合物在二氯甲烷中的最大发射波长为575 nm,为黄光发射铱磷光配合物。     

一种联吡啶类铱配合物的合成及光物理性能测试

以2-(2,4-二氟苯基)吡啶为主配体,2,2''-联吡啶为辅助配体,设计合成出了一种联吡啶铱配合物[Ir(dfppy)2(bpy)]PF6 (dfppy = 2-(2,4-二氟苯基)吡啶,bpy = 2,2''-联吡啶)。通过元素分析、质谱、核磁共振谱、红外光谱和X射线单晶测试表征了配合物的化学结构,通过光致发光光谱和紫外可见光谱研究了配合物的光物理性能。结果表明,配合物的最大发射波长为515 nm,发光颜色为绿光。     

离子型黄光铱磷光配合物的合成、结构及光物理性能研究

设计合成了一种新的离子型铱配合物[Ir(dmpmq)2(dtbpy)]PF6,该配合物以2-(3,5-二甲基苯基)-4-甲基喹啉为主配体,4,4''-二叔丁基-2,2''-联吡啶为辅助配体,六氟磷酸根为阴离子。通过核磁共振谱(¹H-NMR,¹³C-NMR)、质谱(MS)、单晶X射线衍射(XRD)确认了配合物的化学结构,采用光致发光光谱(PL)和紫外可见光谱(UV-Vis)对其光物理性能进行了研究。结果表明,该配合物为单斜晶系,空间群为C2/c;配合物在二氯甲烷溶液中的最大发射波长为579 nm,为典型的黄光发射离子型铱磷光配合物。     

铱磷光配合物Ir(dfppy)2(phbudio)的合成及表征

以氯桥二聚体[Ir(dfppy)2(μ-Cl2)]2、1-苯基-1,3-丁二酮为原料合成了一种铱磷光配合物Ir(dfppy)2(phbudio),产率86.0%,并通过元素分析、核磁共振谱、质谱和红外光谱表征确认了目标产物的化学结构。通过紫外-可见吸收以及荧光光谱对其光物理性质进行测试,其常温最大发射位于522 nm处,显示发射强烈的绿光,初步推测该铱磷光配合物发射可能来自金属铱到环金属配体和辅助配体的电荷转移(MLCT)跃迁。     

一种喹啉类铱配合物的合成及光物理性能研究

以2-(3,5-二甲基苯基)喹啉(dmpq)为主配体,4,4''-二叔丁基-2,2''-联吡啶(dtbby)为辅助配体,合成出一种新型离子型铱配合物[Ir(dmpq)2(dtbbpy)]PF6。通过元素分析、质谱、核磁共振谱(¹H和¹³C)、红外光谱和单晶X射线衍射表征了配合物的组成和化学结构,通过光致发光光谱和紫外可见光谱研究了配合物的光物理性能,通过热重分析测试了配合物的热稳定性。结果表明,所合成的苯基喹啉类铱配合物呈稍微扭曲的八面体配合物,其发射波长为587 nm,热分解温度为380℃,具有足够的热稳定性,是一种潜在的黄光材料。     

蓝光铱配合物的合成、结构表征及光物理性能测试

在碱性条件下,以铱的氯桥二聚体(dfppy)2Ir(μ-Cl2)Ir(dfppy)2和乙酰丙酮反应合成出高效磷光材料二[2-(2,4-二氟苯基)吡啶-C2,N'](乙酰丙酮)合铱(III)(Ir(dfppy)2(acac))。用核磁共振谱(1H NMR、13C NMR)、红外光谱和单晶X射线衍射等表征手段确定了分子结构,用高效液相色谱法测定了纯度,用光致发光光谱测试了光物理性能。结果表明,合成的配合物组成及结构与实际一致,Ir(dfppy)2(acac)为电中性八面体配合物,Ir-O、Ir-C、Ir-N键的平均长度分别为0.2160(14)、0.1998(11)、0.2030(15)nm,在484 nm处出现了较强的蓝光发射。方法的合成产率大于90%,纯度99.70%,适于批量制备。     

两种黄绿光铱配合物的合成及光物理性质研究

以2-苯基-6-(三氟甲基)-苯并噻唑和5,7-二氟-2-苯基苯并噻唑为主配体,分别与辅助配体三苯基膦合成了两种新型的环金属铱配合物(Ir1和Ir2)。用核磁共振氢谱(¹H-NMR)和质谱(MS)进行表征并确认其结构。用紫外吸收光谱以及荧光发射光谱研究了它们的光物理性质,Ir1和Ir2的最大发射波长分别为548和546 nm,发黄绿光,相对量子产率为41.1%和69.2%,荧光寿命分别为0.65和0.66 μs。密度泛函理论(DFT)计算表明紫外最大吸收峰和荧光发射峰均归因于MLCT/ILCT跃迁。     

蓝光材料FIrpic的合成、结构表征及光物理性能测试

以水合三氯化铱和 dfppy 为原料,在乙二醇单乙醚溶剂中反应得氯桥二聚体(dfppy)2Ir(μ-Cl2)Ir(dfppy)2,然后在碱性条件下与2-吡啶甲酸反应合成出 FIrpic。通过核磁共振谱(1HNMR、13CNMR)、质谱、红外光谱和单晶X射线衍射等确定了分子结构,高效液相色谱法(HPLC)测试了纯度,利用紫外-可见吸收光谱和光致发光光谱对其光物理性能进行了测试。结果表明：FIrpic为电中性八面体配合物,在476 nm处出现了较强的蓝光发射,其合成产率大于90%,纯度为99.22%,该方法适于FIrpic的批量制备。     

(1,5-环辛二烯)氯化钌(II)多聚体的合成及表征

在无水乙醇介质中,将水合三氯化钌与1,5-环辛二烯加热回流,一步合成了(1,5-环辛二烯)氯化钌(II)多聚体[Ru(cod)Cl2]n,产率96%。用元素分析、核磁共振(¹H-NMR、¹³C-NMR)和红外光谱(IR)等分析表明产物为目标化合物。     

Effects of Post-weld Heat Treatment on Microstructure,Mechanical Properties and the Role of Weld Reinforcement in 2219 Aluminum Alloy TIG-Welded Joints

In as-welded state, each region of 2219 aluminum alloy TIG-welded joint shows diff erent microstructure and microhardness due to the diff erent welding heat cycles and the resulting evolution of second phases. After the post-weld heat treatment, both the amount and the size of the eutectic structure or θ phases decreased. Correspondingly, both the Cu content in α-Al matrix and the microhardness increased to a similar level in each region of the joint, and the tensile strength of the entire joint was greatly improved. Post-weld heat treatment played the role of solid solution strengthening and aging strengthening. After the post-weld heat treatment, the weld performance became similar to other regions, but weld reinforcements lost their reinforcing eff ect on the weld and their existence was more of an adverse eff ect. The joint without weld reinforcements after the post-weld heat treatment had the optimal tensile properties, and the specimens randomly crack in the weld zone.     

The First Phase of the SRIF Industrialized Base in ＂West Area＂ Has Been Put into Operation

After nearly two years＇ tense construction, the first phase of industrialized base of Shenyang Research Institute of Foundry （SRIF）, located at the Tiexi Casting and Forging Industrial Park in the west of Tiexi District, has now been completed and formally put into operation.     

THERMODYNAMICS STUDY ON THE DECOMPOSITION OF CHROMITE WITH KOH

Institute of Process Engineering, Chinese Academy of Sciences, China, has proposed a method for oxidative leaching of chromite with potassium hydroxide. Understanding the mechanism of chromite decomposition, especially in the potassium hydroxide fusion, is important for the optimization of the operating parameters of the oxidative leaching process. A traditional thermodynamic method is proposed and the thermal decomposition and the reaction decomposition during the oxidative leaching of chromite with KOH and oxygen is discussed, which suggests that chromite is mainly destroyed by reactions with KOH and oxygen. Meanwhile, equilibrium of the main reactions of the above process was calculated at different temperatures and oxygen partial pressures. The stable zones of productions, namely, K2CrO4 and Fe2O3, increase with the decrease of temperature, which indicates that higher temperature is not beneficial to thermodynamic reactions. In addition, a comparison of the general alkali methods is carried out, and it is concluded that the KOH leaching process is thermodynamically superior to the conventional chromate production process.     

INFLUENCE OF HEAT TREATMENT ON DAMPING BEHAVIOUR OF THE MAGNESIUM WROUGHT ALLOY AZ61

The effect of isochronal heat treatments for 1h on variation of damping, hardness and microstructural change of the magnesium wrought alloy AZ61 was investigated. Damping and hardness behaviour could be attributed to the evolution of precipitation process. The influence of precipitation on damping behaviour was explained in the framework of the dislocation string model of Granato and Lücke.     

新型的治疗阿尔茨海默氏症药物(1-二甲基磷酰基-2,2,2-三氯)-乙基-1-醇烟酸醋对体外神经细胞的作用

目的: 观察本实验室合成的一种治疗阿尔茨海默氏症(AD)的药物(1-二甲基磷酰基-2, 2, 2 -三氯)-乙基^-1-醇烟酸醋(NMF),对体外培养的皮层神经细胞活性的影响以及对海人藻酸(KA)所致的神经损伤的保护作用。方法: 采用体外培养皮层神经元的方法,解剖分离 15 d胚胎小鼠皮层神经细胞, 接种于 96孔板,48 h 后加药并培养 72 h,以 MIT 法 观察 NMF 对小鼠皮层神经细胞活性的影响;同时将接种于 24 孔板的细胞预先给予 NMF,d 3 时加或不加KA处理后,以台盼蓝染色鉴别并计数死、活细胞,可得出细胞的存活率。结果: NMF 明显促进胎鼠皮层神经元活性,其中 NMF1、0. 1、10nmol·L^-1促进神经元活性增殖率分别高达 34.7%、37.4%、36. 7%, NMF 明显促进正常胎鼠皮层神经元存活卒,与对照组比较,10nmol·L^-1 NMF 对皮层神经元的存活率分别提高 39.3%、73.5%。 NMF能显著 对抗 KA 所致的神经元损伤,与 KA 损伤组相比, NMF0.1、10、10nmol·L^-1对损伤皮层神经元的保护率分别为 77.30%、80.10%、84.15%。结论: NMF 明 显促进胎鼠皮层神经元的洁性、提高正常皮层神经元,的存活卒,并能有效地保护KA所致的神经元损伤,提示 NMF 是一种很有潜力的治疗 AD 的药物。     

Effect of Rare Earth Doping on Impedance,Modulus and Conductivity Properties of Multiferroic Composites:0.5(BiLa_xFe_(1-x)O_3)–0.5(PbTiO_3)

The Lanthanum-doped bismuth ferrite–lead titanate compositions of 0.5(Bi LaxFe1-xO3)–0.5(Pb Ti O3)(x = 0.05,0.10,0.15,0.20)(BLxF1-x-PT) were prepared by mixed oxide method.Structural characterization was performed by X-ray diffraction and shows a tetragonal structure at room temperature.The lattice parameter c/a ratio decreases with increasing of La(x = 0.05–0.20) concentration of the composites.The effect of charge carrier/ion hopping mechanism,conductivity,relaxation process and impedance parameters was studied using an impedance analyzer in a wide frequency range(102–106Hz) at different temperatures.The nature of Nyquist plot confirms the presence of bulk effects only,and non-Debye type of relaxation processes occurs in the composites.The electrical modulus exhibits an important role of the hopping mechanism in the electrical transport process of the materials.The ac conductivity and dc conductivity of the materials were studied,and the activation energy found to be 0.81,0.77,0.76 and 0.74 e V for all compositions of x = 0.05–0.20 at different temperatures(200–300 °C).     

Three-Dimensional Growth of Coherent Ferrite in Austenite: A Molecular Dynamics Study

Coherent second phase often exhibits anisotropic morphology with specifi c orientations with respect to both the second and the matrix phases. As a key feature of microstructure, the morphology of the coherent particles is essential for understanding the second-phase strengthening eff ect in various industrial alloys. This letter reports anisotropic growth of coherent ferrite from austenite matrix in pure iron based on molecular dynamics simulation. We found that the ferrite grain tends to grow into an elongated plate-like shape, independent of its initial confi guration. The fi nal shape of the ferrite is closely related to the misfi t between the two phases, with the longest direction and the broad facet of the plate being, respectively, consistent with the best matching direction and the best matching plane calculated via the Burgers vector content(BVC) method. The strain energy calculation in the framework of Eshelby's inclusion theory verifi es that the simulated orientation of the coherent ferrite is energetically favorable. It is anticipated that the BVC method will be applicable in analysis of anisotropic growth and morphology of coherent second phase in other phase transformation systems.     

Using Finite Element and Contour Method to Evaluate Residual Stress in Thick Ti-6Al-4V Alloy Welded by Electron Beam Welding

This work was to reveal the residual stress profile in electron beam welded Ti-6Al-4V alloy plates(50 mm thick) by using finite element and contour measurement methods.A three-dimensional finite element model of 50-mmthick titanium component was proposed,in which a column–cone combined heat source model was used to simulate the temperature field and a thermo-elastic–plastic model to analyze residual stress in a weld joint based on ABAQUS software.Considering the uncertainty of welding simulation,the computation was calibrated by experimental data of contour measurement method.Both test and simulated results show that residual stresses on the surface and inside the weld zone are significantly different and present a narrow and large gradient feature in the weld joint.The peak tensile stress exceeds the yield strength of base materials inside weld,which are distinctly different from residual stress of the thin Ti-6Al-4V alloy plates presented in references before.     

Microstructures and Tensile Properties of Ultrafine-Grained Ni–(1–3.5) wt% SiC_(NP) Composites Prepared by a Powder Metallurgy Route

Silicon carbide nanoparticle-reinforced nickel-based composites(Ni–Si CNP),with a Si CNPcontent ranged from1 to 3.5 wt%,were prepared using mechanical alloying and spark plasma sintering.In addition,unreinforced pure nickel samples were also prepared for comparative purposes.To characterize the microstructural properties of both the unreinforced pure nickel and the Ni–Si CNPcomposites transmission electron microscopy(TEM) was used,while their mechanical behavior was investigated using the Vickers pyramid method for hardness measurements and a universal tensile testing machine for tensile tests.TEM results showed an array of dislocation lines decorated in the sintered pure nickel sample,whereas,for the Ni–Si CNPcomposites,the presence of nano-dispersed Si CNPand twinning crystals was observed.These homogeneously distributed Si CNPwere found located either within the matrix,between twins or on grain boundaries.For the Ni–Si CNPcomposites,coerced coarsening of the Si CNPassembly occurred with increasing Si CNPcontent.Furthermore,the grain sizes of the Ni–Si CNPcomposites were much finer than that of the unreinforced pure nickel,which was considered to be due to the composite ball milling process.In all cases,the Ni–Si CNPcomposites showed higher strengths and hardness values than the unreinforced pure nickel,likely due to a combination of dispersion strengthening(Orowan effects) and particle strengthening(Hall–Petch effects).For the Ni–Si CNPcomposites,the strength increased initially and then decreased as a function of Si CNPcontent,whereas their elongation percentages decreased linearly.Compared to all materials tested,the Ni–Si CNPcomposite containing 1.5% Si C was found more superior considering both their strength and plastic properties.     

Directional Growth of Tin Crystals Controlled by Combined Solute Concentration Gradient Field and Static Magnetic Field

A new method was introduced to achieve directional growth of Sn crystals. Microstructures in liquid(Pb)/liquid(Sn) diffusion couples were investigated under various static magnetic fields. Results show that the β-Sn crystals mainly reveal an irregular dendritic morphology without or with a relatively low static magnetic field(B0.3 T). When the magnetic field is increased to 0.5 T, the β-Sn dendrites close to the final stage of growth begin to show some directional character. With a further increase in the magnetic field to a higher level(0.8–5 T), the β-Sn dendrites have an enhanced directional growth character, but the dendrites show a certain deflection. As the magnetic field is increased to 12 T, the directional growth of the β-Sn dendrites in the center of the couple is severely destroyed. The mechanism of the directional growth of the β-Sn crystals and the deflection of the β-Sn crystals with the application of static magnetic field was tentatively discussed.