Synthesis, sintering and characterization of PLZST perovskite prepared by a lactate precursor route

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Materials Characterization

Materials Characterization Materials characterization is a crucial aspect of scientific research and development. It involves the study and analysis of the physical, chemical, and mechanical properties of materials. By understanding these properties, scientists and engineers can design materials with specific characteristics and improve existing materials for various applications. In this response, I will discuss the importance of materials characterization from multiple perspectives, including scientific, engineering, and industrial. From a scientific perspective, materials characterization plays a vital role in advancing our understanding of the fundamental properties of matter. By studying the structure and composition of materials at the atomic and molecular level, scientists can gain insights into the behavior and properties of different materials. For example, techniques such as X-ray diffraction and electron microscopy can provide information about the crystal structure and morphology of materials, helping scientists understand how these factors influence material properties. This knowledge is essential for developing new materials with tailored properties for specific applications. From an engineering perspective, materials characterization is essential for designing and selecting materials that can withstand specific conditions and perform optimally in different applications. For instance, in the aerospace industry, materials used in aircraft components need to have high strength, low weight, and resistance to high temperatures. By characterizing the mechanical properties of different materials, engineers can determine which materials are suitable for specific applications. This ensures the safety and reliability of engineering structures and devices. From an industrial perspective, materials characterization iscrucial for quality control and product development. Manufacturers need to ensure that their materials meet certain specifications and standards to guarantee the performance and durability of their products. By characterizing the properties of materials, such as hardness, tensile strength, and corrosion resistance, manufacturers can assess the suitability of materials for different applications. This helps in improving product quality and reducing the risk of failure or malfunction. Moreover, materials characterization also plays a significant role in the field of nanotechnology. As materials are miniaturized to the nanoscale,their properties can change drastically. Therefore, it is essential to characterize the size, shape, and composition of nanoparticles accurately. This information is crucial for understanding their behavior and interactions with other materials. Nanoparticles find applications in various fields, such as electronics, medicine, and energy, and their properties need to be thoroughly characterized to ensure their safe and effective use. In addition to scientific, engineering, and industrial perspectives, materials characterization also has societal implications. For instance, the development of new materials with improved properties can lead to technological advancements that benefit society. Materials with higher strength and lighter weight can contribute to the development of more fuel-efficient vehicles, reducing carbon emissions and combating climate change. Similarly, the development of materials with enhanced electrical conductivity can lead to the production of more efficient electronic devices, improving communication and connectivity. In conclusion, materials characterization is of utmost importance from multiple perspectives. It enables scientists to understand the fundamental properties of matter, engineers to design and select materials for specific applications, and manufacturers to ensure product quality. Moreover, materials characterization plays a significant role in the field of nanotechnology and has societal implications, contributing to technological advancements and addressing global challenges. Therefore, continued research and development in materials characterization are crucial for the progress of science, engineering, and society as a whole.。

材料专业词汇大全

-可编辑材料科学专业学术翻译必备词汇编号中文英文1合金alloy 2材料material 3复合材料properties 4制备preparation 5强度strength 6力学mechanical 7力学性能mechanical 8复合composite 9薄膜films 10基体matrix 11增强reinforced 12非晶amorphous 13基复合材料composites14纤维fiber 15纳米nanometer 16金属metal 17合成synthesis 18界面interface 19颗粒particles 20法制备prepared 21尺寸size 22形状shape 23烧结sintering 24磁性magnetic 25断裂fracture 26聚合物polymer 27衍射diffraction 28记忆memory 29陶瓷ceramic 30磨损wear 31表征characterization 32拉伸tensile 33形状记忆memory 34摩擦friction 35碳纤维carbon36粉末powder 37溶胶sol-gel 38凝胶sol-gel 39应变strain 40性能研究properties 41晶粒grain 42粒径size 43硬度hardness 44粒子particles 45涂层coating 46氧化oxidation 47疲劳fatigue 48组织microstructure49石墨graphite 50机械mechanical 51相变phase 52冲击impact 53形貌morphology 54有机organic 55损伤damage 56有限finite 57粉体powder 58无机inorganic 59电化学electrochemical 60梯度gradient 61多孔porous 62树脂resin 63扫描电镜sem 64晶化crystallization 65记忆合金memory 66玻璃glass 67退火annealing 68非晶态amorphous 69溶胶-凝胶sol-gel 70蒙脱土montmorillonite 71样品samples 72粒度size73耐磨wear 74韧性toughness 75介电dielectric 76颗粒增强reinforced 77溅射sputtering 78环氧树脂epoxy 79纳米tio tio 80掺杂doped 81拉伸强度strength 82阻尼damping 83微观结构microstructure84合金化alloying 85制备方法preparation 86沉积deposition87透射电镜tem 88模量modulus 89水热hydrothermal90磨损性wear 91凝固solidification 92贮氢hydrogen 93磨损性能wear 94球磨milling 95分数fraction 96剪切shear 97氧化物oxide 98直径diameter 99蠕变creep 100弹性模量modulus 101储氢hydrogen 102压电piezoelectric 103电阻resistivity 104纤维增强composites 105纳米复合材料preparation 106制备出prepared 107磁性能magnetic 108导电conductive109晶粒尺寸size 110弯曲bending 111光催化tio-可编辑112非晶合金amorphous 113铝基复合材料composites 114金刚石diamond 115沉淀precipitation 116分散dispersion 117电阻率resistivity 118显微组织microstructure119sic 复合材料sic 120硬质合金cemented 121摩擦系数friction 122吸波absorbing 123杂化hybrid 124模板template 125催化剂catalyst 126塑性plastic 127晶体crystal 128sic 颗粒sic 129功能材料materials 130铝合金alloy 131表面积surface 132填充filled 133电导率conductivity 134控溅射sputtering 135金属基复合材料composites 136磁控溅射sputtering 137结晶crystallization 138磁控magnetron 139均匀uniform 140弯曲强度strength 141纳米碳carbon 142偶联coupling 143电化学性能electrochemical 144及性能properties 145al 复合材料composite 146高分子polymer 147本构constitutive148晶格lattice 149编织braided150断裂韧性toughness 151尼龙nylon 152摩擦磨损性friction 153耐磨性wear 154摩擦学tribological 155共晶eutectic 156聚丙烯polypropylene 157半导体semiconductor158偶联剂coupling 159泡沫foam 160前驱precursor 161高温合金superalloy 162显微结构microstructure163氧化铝alumina 164扫描电子显微镜sem 165时效aging 166熔体melt 167凝胶法sol-gel 168橡胶rubber 169微结构microstructure170铸造casting 171铝基aluminum 172抗拉强度strength 173导热thermal 174透射电子显微镜tem 175插层intercalation 176冲击强度impact 177超导superconducting 178记忆效应memory 179固化curing 180晶须whisker 181溶胶-凝胶法制sol-gel 182催化catalytic 183导电性conductivity184环氧epoxy 185晶界grain 186前驱体precursor 187机械性能mechanical188抗弯strength 189粘度viscosity 190热力学thermodynamic 191溶胶-凝胶法制备sol-gel 192块体bulk 193抗弯强度strength 194粘土clay 195微观组织microstructure196孔径pore 197玻璃纤维glass 198压缩compression199摩擦磨损wear 200马氏体martensitic 201制得prepared 202复合材料性能composites 203气氛atmosphere 204制备工艺preparation205平均粒径size 206衬底substrate 207相组成phase 208表面处理surface 209杂化材料hybrid 210材料中materials 211断口fracture 212增强复合材料composites 213马氏体相变transformation214球形spherical 215混杂hybrid 216聚氨酯polyurethane 217纳米材料nanometer 218位错dislocation 219纳米粒子particles 220表面形貌surface 221试样samples 222电学properties 223有序ordered 224电压voltage-可编辑225析出phase 226拉伸性tensile 227大块bulk 228立方cubic 229聚苯胺polyaniline 230抗氧化性oxidation 231增韧toughening232物相phase 233表面改性modification234拉伸性能tensile 235相结构phase 236优异excellent 237介电常数dielectric 238铁电ferroelectric 239复合材料力学性能composites240碳化硅sic 241共混blends 242炭纤维carbon 243复合材料层composite 244挤压extrusion 245表面活性剂surfactant 246阵列arrays 247高分子材料polymer 248应变率strain 249短纤维fiber 250摩擦学性能tribological 251浸渗infiltration 252阻尼性能damping 253室温下room 254复合材料层合板composite 255剪切强度strength 256流变rheological257磨损率wear 258化学气相沉积deposition 259热膨胀thermal 260屏蔽shielding 261发光luminescence 262功能梯度functionally263层合板laminates 264器件devices 265铁氧体ferrite 266刚度stiffness 267介电性能dielectric268xrd 分析xrd 269锐钛矿anatase 270炭黑carbon 271热应力thermal 272材料性能properties 273溶胶-凝胶法sol-gel 274单向unidirectional275衍射仪xrd 276吸氢hydrogen 277水泥cement 278退火温度annealing 279粉末冶金powder 280溶胶凝胶sol-gel 281熔融melt 282钛酸titanate 283磁合金magnetic 284脆性brittle 285金属间化合物intermetallic 286非晶态合金amorphous 287超细ultrafine 288羟基磷灰石hydroxyapatite 289各向异性anisotropy 290镀层coating 291颗粒尺寸size 292拉曼raman 293新材料materials294tic 颗粒tic 295孔隙率porosity 296制备技术preparation 297屈服强度strength 298金红石rutile 299采用溶胶-凝胶sol-gel 300电容量capacity 301热电thermoelectric302抗菌antibacterial 303聚酰亚胺polyimide 304二氧化硅silica 305放电容量capacity 306层板laminates 307微球microspheres 308熔点melting 309屈曲buckling 310包覆coated 311致密化densification 312磁化强度magnetization313疲劳寿命fatigue 314本构关系constitutive 315组织结构microstructure 316综合性能properties 317热塑性thermoplastic 318形核nucleation 319复合粒子composite 320材料制备preparation 321晶化过程crystallization 322层间interlaminar 323陶瓷基ceramic 324多晶polycrystalline 325纳米结构nanostructures 326纳米复合composite 327热导率conductivity 328空心hollow 329致密度density 330x 射线衍射仪xrd 331层状layered 332矫顽力coercivity 333纳米粉体powder 334界面结合interface 335超导体superconductor 336衍射分析diffraction 337纳米粉powders 338磨损机理wear 339泡沫铝aluminum-可编辑340进行表征characterized 341梯度功能gradient 342耐磨性能wear 343平均粒particle 344聚苯乙烯polystyrene 345陶瓷基复合材料composites 346陶瓷材料ceramics 347石墨化graphitization348摩擦材料friction 349熔化melting 350多层multilayer 351及其性能properties 352酚醛树脂resin 353电沉积electrodeposition 354分散剂dispersant 355相图phase 356复合材料界面interface 357壳聚糖chitosan 358抗氧化性能oxidation 359钙钛矿perovskite 360分层delamination 361热循环thermal 362氢量hydrogen 363蒙脱石montmorillonite 364接枝grafting 365导率conductivity 366放氢hydrogen 367微粒particles 368伸长率elongation 369延伸率elongation 370烧结工艺sintering 371层合laminated 372纳米级nanometer 373莫来石mullite 374磁导率permeability375填料filler 376热电材料thermoelectric377射线衍射ray 378铸造法casting 379粒度分布size 380原子力afm381共沉淀coprecipitation 382水解hydrolysis 383抗热thermal 384高能球ball 385干摩擦friction 386聚合物基polymer 387疲劳裂纹fatigue 388分散性dispersion 389硅烷silane 390弛豫relaxation 391物理性能properties 392晶相phase 393饱和磁化强度magnetization 394凝固过程solidification 395共聚物copolymer 396光致发光photoluminescence 397薄膜材料films 398导热系数conductivity399居里curie 400第二相phase 401复合材料制备composites 402多孔材料porous 403水热法hydrothermal404原子力显微镜afm 405压电复合材料piezoelectric406尼龙6nylon 407高能球磨milling 408显微硬度microhardness 409基片substrate 410纳米技术nanotechnology 411直径为diameter 412织构texture 413氮化nitride414热性能properties 415磁致伸缩magnetostriction 416成核nucleation 417老化aging 418细化grain 419压电材料piezoelectric 420纳米晶amorphous421si 合金si 422复合镀层composite 423缠绕winding 424抗氧化oxidation 425表观apparent 426环氧复合材料epoxy 427甲基methyl 428聚乙烯polyethylene 429复合膜composite 430表面修饰surface 431大块非晶amorphous 432结构材料materials 433表面能surface 434材料表面surface 435疲劳性能fatigue 436粘弹性viscoelastic437基体合金alloy 438单相phase 439梯度材料material 440六方hexagonal 441四方tetragonal 442蜂窝honeycomb 443阳极氧化anodic 444塑料plastics 445超塑性superplastic446sem 观察sem 447烧蚀ablation 448复合薄膜films 449树脂基resin 450高聚物polymer 451气相vapor-可编辑452电子能谱xps 453硅烷偶联coupling 454团聚particles 455基底substrate 456断口形貌fracture 457抗压强度strength 458储能storage 459松弛relaxation 460拉曼光谱raman 461孔率porosity 462沸石zeolite 463熔炼melting 464磁体magnet 465sem 分析sem 466润湿性wettability 467电磁屏蔽shielding 468升温heating 469致密dense 470沉淀法precipitation471差热分析dta 472成功制备prepared 473复合体系composites 474浸渍impregnation 475力学行为behavior 476复合粉体powders 477沥青pitch 478磁电阻magnetoresistance 479导电性能conductivity480光电子能谱xps 481材料力学mechanical 482夹层sandwich 483玻璃化glass 484衬底上substrates 485原位复合材料composites 486智能材料materials 487碳化物carbide 488复相composite 489氧化锆zirconia490基体材料matrix 491渗透infiltration 492退火处理annealing 493磨粒wear 494氧化行为oxidation 495细小fine 496基合金alloy 497粒径分布size 498润滑lubrication 499定向凝固solidification500晶格常数lattice 501晶粒度size 502颗粒表面surface 503吸收峰absorption504磨损特性wear 505水热合成hydrothermal506薄膜表面films 507性质研究properties 508试件specimen 509结晶度crystallinity510聚四氟乙烯ptfe 511硅烷偶联剂silane 512碳化carbide 513试验机tester 514结合强度bonding 515薄膜结构films 516晶型crystal 517介电损耗dielectric 518复合涂层coating 519压电陶瓷piezoelectric520磨损量wear 521组织与性能microstructure 522合成法synthesis 523烧结过程sintering 524金属材料materials 525引发剂initiator 526有机蒙脱土montmorillonite527水热法制hydrothermal528再结晶recrystallization 529沉积速率deposition 530非晶相amorphous531尖端tip 532淬火quenching 533亚稳metastable 534穆斯mossbauer 535穆斯堡尔mossbauer 536偏析segregation 537种材料materials 538先驱precursor 539物性properties 540石墨化度graphitization541中空hollow 542弥散particles 543淀粉starch 544水热法制备hydrothermal545涂料coating 546复合粉末powder 547晶粒长大grain 548sem 等sem 549复合材料组织microstructure550界面结构interface 551煅烧calcined 552共混物blends 553结晶行为crystallization554混杂复合材料hybrid 555laves 相laves 556摩擦因数friction 557钛基titanium 558磁性材料magnetic 559制备纳米nanometer 560界面上interface 561晶粒大小size 562阻尼材料damping 563热分析thermal 564复合材料层板laminates 565二氧化钛titanium-可编辑566沉积法deposition567光催化剂tio 568余辉afterglow 569断裂行为fracture 570颗粒大小size 571合金组织alloy 572非晶形成amorphous 573杨氏模量modulus 574前驱物precursor 575过冷alloy 576尖晶石spinel 577化学镀electroless 578溶胶凝胶法制备sol-gel 579本构方程constitutive 580磁学magnetic 581气氛下atmosphere 582钛合金titanium 583微粉powder 584压电性piezoelectric585sic 晶须sic 586应力应变strain 587石英quartz 588热电性thermoelectric589相转变phase 590合成方法synthesis 591热学thermal 592气孔率porosity 593永磁magnetic 594流变性能rheological 595压痕indentation 596热压烧结sintering 597正硅酸乙酯teos 598点阵lattice 599梯度功能材料fgm 600带材tapes 601磨粒磨损wear 602碳含量carbon 603仿生biomimetic 604快速凝固solidification605预制preform 606差示dsc 607发泡foaming 608疲劳损伤fatigue 609尺度size 610镍基高温合金superalloy 611透过率transmittance 612溅射法制sputtering 613结构表征characterization 614差示扫描dsc 615通过sem sem 616水泥基cement 617木材wood 618tem 分析tem 619量热calorimetry 620复合物composites 621铁电薄膜ferroelectric 622共混体系blends 623先驱体precursor 624晶态crystalline 625冲击性能impact 626离心centrifugal 627断裂伸长率elongation 628有机-无机organic-inorganic 629块状bulk 630相沉淀precipitation631织物fabric 632因数coefficient 633合成与表征synthesis 634缺口notch 635靶材target 636弹性体elastomer 637金属氧化物oxide 638均匀化homogenization 639吸收光谱absorption640磨损行为wear 641高岭土kaolin642功能梯度材料fgm 643滞后hysteresis 644气凝胶aerogel 645记忆性memory 646磁流体magnetic 647铁磁ferromagnetic648合金成分alloy 649微米micron 650蠕变性能creep 651聚氯乙烯pvc 652湮没annihilation 653断裂力学fracture 654滑移slip 655差示扫描量热dsc 656等温结晶crystallization 657树脂基复合材料composite 658阳极anodic 659退火后annealing 660发光性properties 661木粉wood 662交联crosslinking 663过渡金属transition 664无定形amorphous 665拉伸试验tensile 666溅射法sputtering 667硅橡胶rubber 668明胶gelatin 669生物相容性biocompatibility 670界面处interface 671陶瓷复合材料composite 672共沉淀法制coprecipitation 673本构模型constitutive674合金材料alloy 675磁矩magnetic 676隐身stealth 677比强度strength 678改性研究modification 679采用粉末powder-可编辑680晶粒细化grain 681抗磨wear 682元合金alloy 683剪切变形shear 684高温超导superconducting 685金红石型rutile 686晶化行为crystallization 687催化性能catalytic 688热挤压extrusion 689微观microstructure690tem 观察tem 691缺口冲击impact 692生物材料biomaterials 693涂覆coating 694纳米氧化nanometer695x 射线光电子能谱xps 696硅灰石wollastonite 697摩擦条件friction 698衍射峰diffraction699块体材料bulk 700溶质solute 701冲击韧性impact 702锐钛矿型anatase 703凝固组织microstructure704磨损试验机tester 705丙烯酸甲酯pmma 706raman 光谱raman 707减振damping 708聚酯polyester 709体材料materials 710航空aerospace 711光吸收absorption 712韧化toughening 713疲劳裂纹扩展fatigue 714超塑superplastic715凝胶法制备gel716半导体材料semiconductor717剪应力shear 718发光材料luminescence719凝胶法制gel 720甲基丙烯酸甲酯pmma 721硬质hard 722摩擦性能friction 723电致变色electrochromic724超细粉powder 725增强相reinforced 726薄带ribbons 727结构弛豫relaxation 728光学材料materials729sic 陶瓷sic 730纤维含量fiber 731高阻尼damping 732镍基nickel 733热导thermal 734奥氏体austenite 735单轴uniaxial 736超导电性superconductivity 737高温氧化oxidation 738树脂基体matrix 739含能energetic 740粘着adhesion 741穆斯堡尔谱mossbauer 742脱层delamination 743反射率reflectivity 744单晶高温合金superalloy 745粘结bonded 746快淬quenching 747熔融插层intercalation 748外加applied 749钙钛矿结构perovskite 750减摩friction 751复合氧化物oxide 752苯乙烯styrene 753合金表面alloy 754爆轰detonation755长余辉afterglow 756断裂过程fracture 757纺织textile。

科技英语交流(第2版)Lecture 5 How to write Methods

To give the readers enough information to judge whether the methods are appropriately used or not.
Basic components
Generalization or introduction Materials or subjects Methods or procedures Data analysis
The experimental apparatus for...is shown in Fig.2.
5.4.3 Typical expressions of equipment and apparatus
The experimental system was based on a ... A fine wire screen is installed at the ... Example: The experimental system was composed of
vehicles 3. Decoupling PF dynamic model
… 4. Case study
…
3. Organization-related data selection
3.1 Fixed and dynamic keywords sources
3.2 Known accounts sources 3.3 Org keyusers sources 3.4 Two-class SUM
5.3 Specific analyses: generalization and introduction
This part is a general introduction of the principal activity, sometimes presenting the purpose of the research. For example, “In this letter we present the first systematic study on the electrical and magnetic effects of hole compensation.” It also introduces some background information related to the methods or the author’s hypothesis to the research. Study the example on page 87-89.

浅谈多孔陶瓷

浅谈多孔陶瓷08 化本黄振蕾080900029摘要：随着控制材料的细孔结构水平的不断提高以及各种新材质高性能多孔陶瓷材料的不断出现，多孔陶瓷的应用领域与应用范围也在不断扩大，目前其应用已遍及环保、节能、化工、石油、冶炼、食品、制药、生物医学等多个科学领域，引起了全球材料学关键词：多孔陶瓷制备应用发展0. 引言多孔陶瓷是一种经高温烧成、内部具有大量彼此相通, 并与材料表面也相贯通的孔道结构的陶瓷材料。

多孔陶瓷的种类很多, 可以分为三类: 粒状陶瓷烧结体、泡沫陶瓷和蜂窝陶瓷[ 1]。

多孔陶瓷由于均匀分布的微孔和孔洞、孔隙率较高、体积密度小, 还具有发达的比表面, 陶瓷材料特有的耐高温、耐腐蚀、高的化学和尺寸稳定性, 使多孔材料可以在气体液体过滤、净化分离、化工催化载体、吸声减震、保温材料、生物殖入材料, 特种墙体材料和传感器材料等方面得到广泛的应用[ 2]。

因此, 多孔陶瓷材料及其制备技术受到广泛关注。

1 多孔陶瓷材料的制备方法1. 1 挤压成型法挤压是一种塑性变形工艺, 可分为热挤压和冷挤压。

一般是在压力机上完成, 使工件产生塑性变形, 达到所需形状的一种工艺方法。

其过程是将制备好的泥条通过一种预先设计好的具有蜂窝网格结构的模具挤出成形, 经过烧结后就可以得到典型的多孔陶瓷。

目前, 我国已研制出并生产使用蜂窝陶瓷挤出成型模具达到了400孔/ 2. 54 cm X 2. 54 cm 的规格。

美国与日本已研制出了600孔/ 2. 54 cm X 2. 54 cm、900孔/ 2.54 cm X 2. 54 cm 的高孔密度、超薄壁型蜂窝陶瓷。

我国亦开始了600 孔/ 2. 54 cm X2. 54 cm 挤出成型模具的研究, 并取得了初步成功[ 3]。

例如, 现在用于汽车尾气净化的蜂窝状陶瓷, 它是将制备好的泥条通过一种预先设计好的具有蜂窝网格结构的模具挤出成型, 经过烧结后得到典型的多孔陶瓷。

其工艺流程为：原料合成+水+有机添加剂T混合练混T挤出成型T干燥T烧成T制品。

基于壳聚糖的分子印迹聚合物的制备和应用

化工进展 2016年第35卷·846·of Mn，Fe，Co，Ni，Cu and Zn：relationship to the 3-methyl analogs[J].Inorg. Chim. Acta，2000，300-302：1082-1089.[36] GHASSEMZADEH M，FALLAHNEDJAD L，HERA VI M M，et al.Synthesis，characterization and crystal structure of new silver(I) andpalladium(Ⅱ) complexes containing 1,2,4-triazole moieties[J]. Polyhedron，2008，27（6）：1655-1664.[37] ROBIN J Blagg R J，L´Opez-G´Omez M G，CHARMANT J P H，et al. The oxidative conversion of the N,S-bridged complexes[{RhLL’(μ-X)}2] to [(RhLL’)3(μ-X)2]+ (X = mt or taz)：acomparison with the oxidation of N,N-bridged analogues[J]. Dalton.Trans.，2011，40（43）：11497-11510.[38] CASTIN E A，GARCI´A-SANTOS I，DEHNEN S，et al. Synthesis，characterization and DFT calculations of a novel hexanuclear silver(I)cluster-complex containing 4-ethyl-5-pyridin-2-yl-2,4-dihydro-[1,2,4]triazol-3-thione as a result from the cyclization of 2-pyridinformamideN-4-ethylthiosemicarbazone [J]. Polyhedron，2006. 25（18）：3653-3660.[39] BHARTI A，BHARTY M K，KASHY AP S，et al. Hg(Ⅱ) complexesof 4-phenyl-5-(3-pyridyl)-1,2,4-triazole-3-thione and 5-(4-pyridyl)-1,3,4-oxadiazole-2-thione and a Ni(Ⅱ) complex of 5-(thiophen-2-yl)-1,3,4-oxadiazole -2-thione：synthesis and X-ray structural studies[J].Polyhedron，2013，50（1）：582-591.[40] YU H X，MA J F，XU G H，et al. Syntheses and crystal structures offour new organotin complexes with Schiff bases containing triazole[J].J. Organomet. Chem.，2006，691（16）：3531-3539.[41] PATIL S A，MANJUNATHA M，KULKARNI A D，et al. Synthesis，characterization，fluorescence and biological studies of Mn(Ⅱ)，Fe(Ⅲ)and Zn(Ⅱ) complexes of Schiff bases derived from Isatin and 3-substituted-4-amino-5-mercapto-1,2,4-triazoles[J]. Complex. Met.，2014，1：128-137.[42] CAMMI R，LANFRANCHI M，MARCHIO L，et al. Synthesis andmolecular structure of the dihydrobis (thioxotriazolinyl) boratocomplexes of zinc(Ⅱ)，bismuth(Ⅲ)，and nickel(Ⅱ). M…H-Binteraction studied by Ab initio calculations[J]. Inorg. Chem.，2003，42（5）：1769-1778.[43] CHU W J，YAO H C，MA H C，et al. Syntheses，structures，andcharacterizations of two coordination polymers assembled from zinc(Ⅱ) salts with 1,2-bis[3-(1,2,4-triazolyl)-4-amino-5-carboxylmethylthio]ethane[J]. J. Coord. Chem.，2010，63（21）：3734-3742.[44] CHU W J，YAO H C，FAN Y T，et al. Anion exchange inducedtunable catalysis properties of an uncommon butterfly-liketetranuclear copper(Ⅱ) cluster and magnetic characterization[J].Dalton. Trans.，2011，40（11）：2555-2561.[45] CHU W J，HE Y，ZHAO Q H，et al. Two 3D network complexes ofY(Ⅲ) and Ce(Ⅲ) with 2-fold interpenetration and reversibledesorption-adsorption behavior of lattice water[J]. Journal of SolidState Chemistry，2010，183（10）：2298-2304.[46] CHU W J，HOU X W，ZHAO Q H，et al. Four novel lanthanide(Ⅲ)coordination polymers with 3D network structures containing 2-foldinterpenetration[J]. Inorg. Chem. Commun.，2010，13（1）：22-25. [47] AIN Q，PANDEY S K，PANDEY O P，et al. Synthesis，spectroscopic，thermal and antimicrobial studies of neodymium(Ⅲ) and samarium(Ⅲ) complexes derived from tetradentate ligands containing N and Sdonor atoms[J]. Spectrochim. Acta，Part A，2015，140：27-34.[48] BAHEMMAT S，GHASSEMZADEH M，AFSHARPOUR M，et al.Synthesis，characterization and crystal structure of a Pd(Ⅱ) complexcontaining a new bis-1,2,4-triazole ligand：a new precursor for thepreparation of Pd(0) nanoparticles[J]. Polyhedron，2015，89：196-202. [49] ZHANG R F，WANG Q F，LI Q L，et al. Syntheses andcharacterization of triorganotin(IV) complexes of Schiff base derivefrom 4-amino-5-phenyl-4H-1,2,4-triazole-3-thiol and 5-amino-1,3,4-thiadiazole-2-thiol with p-phthalaldehyde[J]. Inorg. Chim. Acta，2009，362（8）：2762-2769.[50] BHAT K S，POOJARY B，PRASAD D J，et al. Synthesis andantitumor activity studies of some new fused 1,2,4-triazole derivativescarrying 2,4-dichloro-5-fluorophenyl moiety[J]. Eur. J. Med. Chem.，2009，44：5066-5070.2016年第35卷第3期CHEMICAL INDUSTRY AND ENGINEERING PROGRESS ·847·化工进展基于壳聚糖的分子印迹聚合物的制备和应用许龙1，黄运安1，朱秋劲1，2，叶春1（1贵州大学酿酒与食品工程学院，贵州贵阳550025；2贵州大学食品科学工程研究中心，贵州贵阳550025）摘要：壳聚糖具有良好的生物相容性和独特的分子结构，基于其制备的分子印迹聚合物因亲和性和选择性高、应用范围广等特点引起了广泛的关注。

苯甲叉基丙二腈中间体合成黄酮类化合物及表征

第 20 卷第 1 期湖南理工学院学报（自然科学版）V ol.20 No.12007 年 3 月Jour n al of Hu n a n Ins titu te of Sc ien ce a nd Tech n o lo gy (N atu ral Sc ien ce s)Mar .2007苯甲叉基丙二腈中间体合成黄酮类化合物及表征杨涛，周从山，谢芳（湖南理工学院化学化工系，湖南岳阳 414000）摘要：本文采用苯甲叉基丙二腈作为中间体，与间苯二酚在无水 ZnCl 2 和 HCl 气体的催化作用下制得亚胺盐，再水解,脱羧,分离得到产物,通过液相色谱、紫外、红外等手段对中间产物和最终产物进行分析鉴定，确定最终产物是 7-羟基二氢黄酮。

关键词：苯甲叉基丙二腈；黄酮；间苯二酚；7-羟基二氢黄酮中图分类号：O623.76文献标识码：A文章编号：1672-5298(2007)01-0080-03Synthesis using Phenylmethylenepropanedinitriles as intermediate and characterization of flavonoids compoundY ANG Tao, ZHOU Cong-shan, XIE Fang(Department of Chemistry and Chemical Engineering, Hunan Institute of Science and Technology, Y ueyang 414000, C hina)Abstract: Two imino-compounds were obtained by the catalysis of ZnCl 2 and HCl using benzylidenemalononitrile and resorcinol as intermediate, which were directly hydrolyzed and decarboxylated without apart. The product was abstracted. All the intermediate and final product were analyzed and characterized by liquid chromatography, ultraviolet Spectrophotometer, infrared Spectrophotometer, we make sure that the final product is 7-hydroxy-2,3-dihydro-2-flaconoid.Key words: benzylidenemalononitrile ； falconoid ；resorcinol ；7-hydroxy-2,3-dihydro-2-flaconoid黄酮类化合物是一类广泛存在于自然界的天然有机化合物。

Synthesis and Characterization of Li(Li0.23Mn0.47Fe0.2Ni0.1)O2 Cathode Material for Li-ion Batteries

retention
Li(Li0.23Mn0.47Fe0.2Ni0.1)O2 compound synthesized easily at low temperature by the proposed citric acid assisted sol-gel process is a promising cathode material for Li-ion batteries.
57
EP
TE D
(1−z)Li[Li1/3Mn2/3]O2−(z)Li[Mn0.5−yNi0.5−yCo2y]O2
M AN U
[11]. to
2
Li2MnO3–LiCo1/3Ni1/3Mn1/3O2
SC
The 4.0~4.5V)
storage power station applications. Therefore, new cathode materials with high capacity, low cost and environment friendly have been investigated thoroughly in recent years [1]. Among them the layered Li2MnO3-based solid solution materials have attracted more attention of the researchers, such as Li2MnO3-LiMO2 (M = Ni, Cr and Co) [2–5], LiNiO2–Li2MnO3–LiCoO2 [8], and [6], Li2MnO3–LiNi1−xCoxO2 [7], [9], [10], above-mentioned

Synthesis(怎样写Synthesis)

How write a synthesis
整理人：报告人：
Definition
Definition of synthesis essay
A synthesis is a combination, usually a shortened version, of several texts. A synthesis is not a summary. A synthesis is an opportunity to create new knowledge out of already existing knowledge.
sources.
Difference between summary and synthesis
Shows what the original authours wrote.
Not only reflects your knowledge about what the original authors wrote, but also creates something new out of two or more pieces of writing.
one unified entity.
Presents a cursory overview.
Forcuses on both main ideas and details.
Demonstrates an understanding of the overall
meaning.
Achieves new insight.
Addresses one set of information(eg.article,chapte r,document) at a time Each

三联吡啶的合成及其金属配合物研究进展

三联吡啶的合成及其金属配合物研究进展1刖言配位化学早期是在无机化学基础上发展起来的一门边沿学科，如今，配位化学在有机化学与无机化学的交叉领域受到化学家门广泛的关注。

有机-金属配合物在气体分离、选择性催化、药物运输和生物成像等方面都有潜在的应用前景，因此日益成为化学研究的热点领域［1-4］。

多联吡啶金属配合物在现代配位化学中占据着不可或缺的位置，常见的多联吡啶配体包括2,2'-二联吡啶（bpy ）和2,2':6'2'-三联吡啶（tpy ）（Fig. 1），Hosseini 就把bpy 称为“最广泛应用的配体” ［5］，与其类似的具有三配位点的tpy 的合成及其金属配合物的研究同样是化学家们研究的热点［6-8］。

Fig 1.三联吡啶的三个吡啶环形成一个大的共轭体系，具有很强的（7给电子能力，配合物中存在金属到配体的d 一 n *反馈成键作用，因而能与大多数金属离子均形成稳定结构的配合物。

然而，三联吡啶金属络合物的特殊的氧化还原和光物理性质受其取代基电子效应的影响。

因此，通过引入不同的取代基，三联吡啶金属络合物可用于荧光发光装置以及光电开关等光化学领域［9-10］。

在临床医学和生物化学领域中，不管是有色金属的测定还是作为DNA 的螯合试剂，三联吡啶衍生物都具有非常广泛的应用前景［11-12］。

2三联吡啶的合成研究进展正因为三联吡啶在许多领域都具有潜在的应用价值，所以对其合成方法的研究十分重要。

三联吡啶的合成由来已久，早在 1932年，Morgan 就首次用吡啶在FeCR 存在下反应合成分离出了三联吡啶，并发现了三联吡啶与Fe （ II ）的配合物［13］。

目前，合成三联吡啶terpyridine tpy的方法主要有成环法和交叉偶联法两种。

2.1成环法成环法中最常用的反应是Kr? hnke 缩合反应( Scheme 1)[14]，首先2-乙酰基吡啶溴化得到化合物2, 2与吡啶反应生成吡啶溴盐3, 3与a 3■不饱和酮4进行Michael加成反应得到二酮5，在醋酸铵存在下进而关环得到三联吡啶。

Synthesis and Characterization of Alumina Nanoparticles

This article was downloaded by: [Cold and Arid Regions Environmental and Engineering Research Institute] On: 01 April 2014, At: 00:59Publisher: Taylor & FrancisInforma Ltd Registered in England and Wales Registered Number: 1072954 Registered office: Mortimer House, 37-41 Mortimer Street, London W1T 3JH, UKMaterials and Manufacturing ProcessesPublication details, including instructions for authors and subscription information:/loi/lmmp20Synthesis and Characterization of AluminaNanoparticles by Igepal CO-520 Stabilized ReverseMicelle and Sol-Gel ProcessingJ. Chandradass a & Dong-Sik Bae aa School of Nano and Advanced Materials Enginneering , Changwon National University ,Gyeongnam, South KoreaPublished online: 21 Jun 2008.PLEASE SCROLL DOWN FOR ARTICLEMaterials and Manufacturing Processes ,23:494–498,2008Copyright ©Taylor &Francis Group,LLC ISSN:1042-6914print/1532-2475online DOI:10.1080/10426910802104211Synthesis and Characterization of Alumina Nanoparticles by IgepalCO-520Stabilized Reverse Micelle and Sol-Gel ProcessingJ.Chandradass and Dong-Sik BaeSchool of Nano and Advanced Materials Enginneering,Changwon National University,Gyeongnam,South KoreaNanosized alumina powders have been prepared via reverse micelle and sol-gel processing.By stepwise hydrolysis using aqueous ammonia as the precipitant,hydroxide precursor was obtained from nitrate solutions dispersed in the nanosized aqueous domains of microemulsion consisting of cyclohexane as the oil phase,poly(oxyethylene)nonylphenyl ether (Igepal CO-520)as the non-ionic surfactant,and an aqueous solution containing aluminium nitrate as the water phase.The synthesized and calcined powders were characterized by thermogravimetry-differential thermal analysis,transmission electron microscopy,and scanning electron microscopy.The XRD analysis showed that the complete transformation from -Al 2O 3nanocrystalline to -Al 2O 3was observed at 1100 C.The resulting alumina nanopowder exhibits particle agglomerates of 135–200nm in average diameter occur when they calcined at 1200 C.The average particle size was found to increase with increase in water to surfactant (R )molar ratio.Keywords Al 2O 3;Ceramics;Characterization methods;Crystallization;Differential thermal analysis;Microemulsion;Nanopowder;Scanning electron microscopy;Sol-gel processing;Thermogravimetric analysis;Transmission electron microscopy;X-ray diffraction.IntroductionIn recent years,there has been an increasing interest in the synthesis of nanocrystalline metal oxides [1–5].Such nanocrystals are important for a variety of applications including fabrication of metal-ceramic laminate composites and as a reinforcement phase in polymer and brittle matrix composites.Corundum ( -Al 2O 3 is one of the most important ceramics materials.Nanocrystalline -Al 2O 3powder has considerable potential for a wide range of applications including high strength materials,electronic ceramics,and catalyst [6,7].In particular high quality nanocrystals of corundum are used as electronic substrates,bearing in watches and other ﬁne precision equipment [8]. -Al 2O 3powders prepared by conventional methods require high temperatures 1300–1600 C for solid-state thermally driven decomposition of the hydrates of alumina [7].Various methods for synthesizing -Al 2O 3include mechanical milling [9],vapor phase reaction [10],precipitation [11],sol-gel [12],hydrothermal [13],and combustion methods [14].Mechanical synthesis of -Al 2O 3requires extensive mechanical ball milling and easily introduces impurities.Vapor reaction for preparing ﬁne -Al 2O 3powder from a gas phase precursor demands high temperature above 1200 C.The precipitation method suffers from its complexity and time consuming (long washing times and aging time).The direct formation of -Al 2O 3via the hydrothermal method needs high temperature and pressure.The combustion method has been used to yield -Al 2O 3powders,whereas the powder obtained from the process is usually hard aggregated but contains nanosized primary particles.The sol-gel method based on molecularReceived November 11,2007;Accepted March 20,2008Address correspondence to Dong-Sik Bae,School of Nano and Advanced Materials Enginneering,Changwon National University,Gyeongnam 641773,South Korea;Fax:+82-55-262-6486;E-mail:dsbae7@changwon.ac.krprecursors usually makes use of metal alkoxides as raw materials.However,the high prices of alkoxides and long gelation periods limit the application of this method.Among all the chemical processes that were developed for the preparation of ﬁne ceramic powder a wide array of metal and metal oxide compounds [15–17],the microemulsion process involving reverse micelles has been demonstrated as a superior method [18]in terms of being able to deliver homogeneous and nanosized grains of a variety of oxides.A microemulsion system consists of an oil phase,a surfactant,and an aqueous phase.It is thermodynamically stable isotropic dispersion of the aqueous phase in the continuous oil phase [19].The size of the aqueous droplets is in the range of 5–10nm,rendering the microemulsion systems optically transparent.Chemical reactions,such as precipitation,will take place when droplets containing the desirable reactants collide with each other.The group of these aqueous droplets involving the microemulsion system will thus be acting as a nanosized reactor yielding nanosized particles.Recently,reverse micelle and sol-gel processing [20–22]have successfully prepared several important nanosized ceramic powder systems.Many of the processing parameters such as the concentration of inorganic salts in the aqueous phase and water to surfactant ratio R in the microemulsion,affect the characteristics including the particle size,particle size distribution,agglomerate size,and phases of the resulting ceramic powders.The objective of the present study is to investigate the feasibility of preparing ultraﬁne alumina nanoparticles by combining reverse micelle and sol-gel processing and to study the effect of water to surfactant ratio R .Experimental procedureTypically,microemulsions of total volume 20mL were prepared at ambient temperature in a 30mL vial with rapid stirring:these consisted of 4mL of nonionic surfactant poly(oxyethylene)nonylphenyl ether (Igepal CO-520,Aldrich Chemical Co.,USA),10ml of cyclohexane,494D o w n l o a d e d b y [C o l d a n d A r i d R e g i o n sE n v i r o n m e n t a l a n d E n g i n e e r i n g R e s e a r c h I n s t i t u t e ] a t 00:59 01 A p r i l 2014SYNTHESIS AND CHARACTERIZATION OF ALUMINA NANOPARTICLES 4950.65–1.32mL of 5×10−1M Al(NO 3 2·9H 2O solution (Aldrich Chemical Co.,USA)and deionized water.The size of the resulting particles was controlled by the ratio R =[water]/[surfactant].The microemulsion was mixed rapidly,and after 5minutes of equilibration,one drop (∼0.05ml)of hydrazine hydrate (9M N 2H 4·xH 2O,Aldrich Chemical Co.,USA)was added as a reducing agent.After nanosized water droplets were formed while stirring,NH 4OH (28%)(Dae Jung chemicals,Korea)was injected into the microemulsion.The microemulsion was then centrifuged to extract the particles,which were subsequently washed by ethanol to remove any residual surfactant.The thermal characteristics of alumina precursors were determined by thermogravimetry and differential thermal analysis (TA 5000/SDT 2960DSC Q10).The phase identiﬁcation of calcined powders was recorded by X-ray diffractometer (Philips X’pert MPD 3040).The size and morphology of the resulting powders were examined by transmission electron microscopy (TEM)and Scanning electron microscopy (SEM).Results and discussionTernary systems of cyclohexane/Igepal CO 520/water offer certain advantages:they are spheroidal and monodisperse aggregates where water is readily solublized in the polar core,forming a “water pool”characterized by the molar ratio of water to surfactant concentration R .Another important property of reverse micelle is their dynamic character;the “water pool”can exchange their contents by collision process.The aggregation and self-assembly of the alumina/surfactant/water species is complex and very little is known about the cluster growth and ﬁnal nanostructure as a function of synthesis condition.The molar ratio of water to surfactant can determine the size of the micro-emulsion water core [23].Therefore,the R -value can control the diameter of the nanoparticle in the micro-emulsion.The average size of the cluster was found to depend on the micelle size,the nature of the solvent,and the concentration of reagent.During the preparation of alumina nanoparticles,the following reaction might occur.Thermal behavior of the precursor determined by TG-DTA in oxygen up to 1200 C at a heating rate of 10 C/min is shown in Figs.1and 2,respectively.NH 3·H 2O →NH +4+OH (1)OH +Al +3→Al OH 3(2)Al OH 3→Al 2O 3+H 2O(3)In the temperature region between RT-180 C,a broad endothermic peak with a weight loss of 9%is attributed to the adsorption of physisorbed water.In the temperature region between 180–600 C,three exothermic peaks were observed at 208,288,and 390 C with a weight loss of 50%corresponding to the decomposition of organic residuals from the precursor.From the TGA curve it is also observed that the precursor exhibit weight loss at <600 C,and at >600 C the weightbecomesFigure 1.—DTA curve of alumina precursor ramped at 10 C/min in air.almost constant.The peak around 1200 C is attributed totransformation of -Al 2O 3from -Al 2O 3.X-ray diffraction (XRD)analysis of precursor powder calcined at 1000,1100,and 1200 C are shown in Fig.3.Diffraction peaks corresponding to -Al 2O 3and weak peaks of -Al 2O 3have been found for samples calcined at 1000 C for 2h indicating - -Al 2O 3transformation.The difference in the crystallization temperature of -Al 2O 3as observed in DTA and XRD could be because of the difference in heating schedule for the two samples.While XRD pattern was recorded on samples which were held for 2h at 1000 C,the DTA was done without any isothermal hold.Thus the isothermal hold at 1000 C has accelerated the transformation to -Al 2O 3at lower temperature.With the increase of calcinations,temperature to 1100 C -Al 2O 3disappears;only -Al 2O 3with low intensity peaks is found indicating complete transformation to -Al 2O 3.A typical XRD pattern of the resultant -Al 2O 3powders after calcinations at 1200 C (2h)are shown in Fig. 4.The crystalline size of the calcined powders (1200 C)atFigure 2.—TGA curve of alumina precursor ramped at 10 C/min in air.D o w n l o a d e d b y [C o l d a n d A r i d R e g i o n sE n v i r o n m e n t a l a n d E n g i n e e r i n g R e s e a r c h I n s t i t u t e ] a t 00:59 01 A p r i l 2014496J.CHANDRADASS AND D.-S.BAEFigure 3.—XRD patterns of the alumina nanoparticles synthesized at R =4and calcined at different temperatures (a)1000 C;(b)1100 C;(c)1200 C (•- -Al 2O 3; - -Al 2O 3 .different value of R has been obtained from X-ray line broadening studies using the Scherer equation [24].Table 1shows that water/surfactant molar ratio R inﬂuenced crystallite size.The crystallite size of the alumina nanoparticles increased with increase in R -value from 4to 8.An increase in the domain size of aqueous droplets,duetoFigure 4.—XRD patterns of the as-synthesized alumina nanoparticles calcined at 1200 C and as a function of R (a)R =4;(b)R =6;(c)R =8.Table 1.—The crystallite size of -Al 2O 3at 1200 C.R =[water]/[surfactant]Crystallite size (nm)481684896Figure 5.—TEM micrographs of as-synthesized alumina nanoparticles calcined at 1200 C and as a function of R (a)R =4;(b)R =6;(c)R =8.D o w n l o a d e d b y [C o l d a n d A r i d R e g i o n sE n v i r o n m e n t a l a n d E n g i n e e r i n g R e s e a r c h I n s t i t u t e ] a t 00:59 01 A p r i l 2014SYNTHESIS AND CHARACTERIZATION OF ALUMINA NANOPARTICLES497Figure 6.—SEM micrographs of as-synthesized alumina nanoparticles calcined at 1200 C and as a function of R (a)R =4;(b)R =6;(c)R =8.an increase in aqueous content in the microemulsion,will lead to an apparent increase in the size of the particle [19].The nucleation and growth of the alumina nanoparticles is likely to be a diffusion-controlled process through interaction between micelles,but it can be inﬂuenced by many other factors such as phase behavior and solubility,average occupancy of reacting species in the aqueous pool and the dynamic behavior of the microemulsion [25].The degree of agglomeration is evident in the TEM micrograph (Fig.5)showing average particle size increase from 135to 200nm as the R -value increases from 4to 8.This is also in agreement with the particle size range as observed from SEM (Fig.6).TEM micrographs (Fig.5)also show the alumina solid bridging (necking)links powder particles together between neighbouring particles.The particle size as observed from TEM is larger than that calculated from the Scherer formula.This is because the nanosized precursor particles derived from micro-emulsions have very high surface areas;thus they tend to aggregate together to form particle agglomerates in the calcined ceramic powders [26].ConclusionNanosized -Al 2O 3powders have been prepared via reverse micelle and sol-gel processing.The XRD analysis showed that the complete transformation from -Al 2O 3to -Al 2O 3was observed at 1100 C.The resulting alumina nanopowder exhibits particle agglomerates of 135–200nm in average diameter occur when they calcined at 1200 C.The average particle size was found to increase with increase in water to surfactant R molar ratio.AcknowledgmentThis study was supported by Korean Research Foundation through project no.KRF-2004-005-D0009.References1.Janbey,A.;Pati,R.K.;Tahir,S.;Pramanik,P.A new chemical route for the synthesis of -Al 2O 3.J.European Ceramic Society 2001,21,2285–2289.2.Pathak,L.C.;Singh,T.B.;Das,S.;Verma, A.K.;Ramachandrarao,P.Effect of pH on the combustion synthesis of nano-crystalline alumina powder.Materials Letter 2002,57,380–385.3.Kiminami,R.H.G.A.;Morelli,M.R.;Folz,D.Z.;Clark,D.C.;Clark,D.E.Microwave synthesis of alumina powders.American Ceramic Society Bulletin 2000,79,63–67.4.Wu,Y.Q.;Zhang,Y.F.;Huang,X.X.;Guo,J.K.Preparation of plate like nano alpha alumina particles.Ceramic International 2001,27,265–268.5.Karasev,V.V.;Onishchuk,A.A.;Lotov,O.G.;Baklanov,A.M.;Zarko,V.E.;Panﬁlov,V.N.Charges and fractal properties of nanoparticles—Combustion products of aluminum bustion Explosion and Shock Wave 2001,37,734–736.6.Ichinose,N.Superﬁne Particle Technology ;Springer-Verlag:London,U.K.,1993.7.Uyeda,R.Studies of ultra ﬁne particles in Japan:crystallography,methods of preparation,and technological applications.Progress in Materials Science 1991,35,1–96.D o w n l o a d e d b y [C o l d a n d A r i d R e g i o n sE n v i r o n m e n t a l a n d E n g i n e e r i n g R e s e a r c h I n s t i t u t e ] a t 00:59 01 A p r i l 2014498J.CHANDRADASS AND D.-S.BAE8.Wefers,K.;Misra,C.Oxides and Hydroxides of Aluminium ,Technical Paper No.19;Alcoa,Pittsburg,PA,1987.9.Panchula,M.L.;Ying,J.Y.;Mechanical synthesis of nanocrystalline -Al 2O 3seeds for enhanced transformation kinectics.Nanostructured Materials 1997,9,161–164.10.Varma,H.K.;Mani,T.V.;Damodaran,A.D.Characteristics ofalumina powders prepared by spray drying of boehmite sol.Journal of American Ceramic Society 1994,77,1597–1600.11.Li,J.G.;Sun,X.D.Synthesis and sintering behavior of ananocrystalline -Al 2O 3powder.Acta Materialia 2000,48,3103–3112.12.Zeng,W.M.;Gao,L.;Guo,J.K.A new sol-gel routeusing inorganic salt for synthesizing Al 2O 3nanopowders.Nanostructured Materials 1998,10,543–550.13.Faneli,A.J.;Burlew,J.V.Preparation of ﬁne alumina powderin alcohol.Journal of American Ceramic Society 1986,69,C174–C175.14.Bhaduri,S.;Zhou,E.;Bhaduri,S.B.Auto ignition processingof nanocrystalline -Al 2O 3.Nanostructured Materials 1997,13,605–610.15.Sugimoto,T.;Kimijima,K.New approach to the formationmechanism of AgCl nanoparticle in a reverse miscelle system.Journal of Physical Chemistry B 2003,107,10753–10759.16.McLeod,M.C.;McHenry,R.S.;Beckman,E.J.;Roberts,C.B.Synthesis and stabilization of silver metallic nanoparticles and premetallic intermediates in perﬂuoropolyether/CO 2reverse micelle system.Journal of Physical Chemistry B 2003,107,2693–2700.17.Sun,W.;Xu,L.;Chu,Y.;Shi,W.Controllable synthesis andCatalytic properties of WO 3/ZrO 2mixed oxide nanoparticles.Journal of Colloid and Interface Science 2003,266,99–106.18.Boutonnet,M.;Kizling,J.;Stenius,P.;Maire,G.The preparationof monodisperse colloidal metal particles from microemulsion.Colloids Surfaces 1982,5,209–225.19.Fang,J.;Wang,J.;Ng,S.-C.;Chew, C.-H.;Gan,L.M.Ultraﬁne zirconia powders via microemulsion processing route.Nanostructured Materials 1997,8,499–505.20.Bae,D.S.;Kim,B.K.;Han,K.S.Fabrication and microstructureof ZnO-TiO 2composite membrane by a reverse micelle and sol-gel processing.Materials Science Forum 2006,510–511,786–789.21.Bae,D.S.;Han,K.S.;Adair,J.H.Synthesis of platinum/silicananocomposite particle by reverse micelle and sol-gel processing.Journal of American Ceramic Society 2002,85,1321–1323.22.Son,J.H.;Park,H.Y.;Kang, D.P.;Bae, D.S.Synthesis andcharacterization of Ag/Pd doped SiO 2nanoparticles by a reverse micelle and sol-gel processing.Colloids and Surfaces A:Physicochemical and Engineering Aspects 2008,313–314,105–107.23.Monnoyer,Ph.;Fonseca,A.;Nagy,J.B.Preparation of colloidalAgBr particles from microemulsions.Colloids and Surfaces A:Physicochemical and Engineering Aspects 1995,100,233–243.24.Klug,M.P.;Alexander,L.E.X-ray Diffraction Procedure forPolycrystalline and Amorphous Materials ;Wiley:New York,1974;634pp.25.Osseo-Asare,K.Handbook of Microemulsion Science andTechnology ;Marcel Dekker,Inc.,Basel:New York,1999;549pp.26.Chow,G.M.;Markowitz,M.A.;Rayne,R.;Dunn,D.N.;Singh,A.Phospholipid mediated synthesis and characterization of gold nanoparticles.Journal of Colloidal Interface Science 1996,183,135–142.D o w n l o a d e d b y [C o l d a n d A r i d R e g i o n sE n v i r o n m e n t a l a n d E n g i n e e r i n g R e s e a r c h I n s t i t u t e ] a t 00:59 01 A p r i l 2014。

Synthesis and characterization of ATO SiO2 nanocomposite coating obtained by sol–gel method

Synthesis and characterization of ATO/SiO 2nanocompositecoating obtained by sol–gel methodXiaoChuan Chen *The Key Laboratory of Materials Physics,Institute of Solid State Physics,Chinese Academy of Sciences,Hefei 230031,People’s Republic of ChinaReceived 19June 2004;accepted 20December 2004Available online 11January 2005AbstractA new sol–gel route was developed for synthesizing homogeneous nanocomposite thin film that was composed of Sb-SnO 2(ATO)nanoparticles and silica matrix.TEM studies show that as-prepared composite thin film contains the amorphous silica matrix and ATO nanocrystalline particles that were dispersed homogeneously in silica matrix.The oxalic acid is an excellent dispersant for colloidal stability of ATO aqueous sol at pH b 5.The result of Zeta potential measurement shows that dispersion mechanism comes from the chemisorption of oxalic acid on the surface of ATO nanoparticles.The thermal treatment in reducing atmosphere considerably promotes grain growth of ATO nanoparticles and changes the optical property of ATO/SiO 2nanocomposite thin film.D 2005Elsevier B.V .All rights reserved.Keywords:Sol–gel preparation;Thin films;Nanocomposites;Sb-doped SnO 21.IntroductionTin oxide is a wide band gap nonstoichiometric semi-conductor with a low n-type resistivity [1–3].The resistance can be reduced further by doping Sb,F elements [4,5].F-doped SnO 2(FTO),Sb-doped SnO 2(ATO)conducting thin films not only have high transparency in the visible region but also are good infrared reflecting materials [6,7].ATO thin films have been used in many fields such as heat shielding coating on low-emissivity window for energy saving [8].Fabrication techniques used to deposit ATO thin film include dip coating based on sol–gel method;sputtering and spray pyrolysis.The sol–gel route has several advantages over the other method.It is a low cost and simple process and makes the precise control of doping concentration easier [9,10].In order to improve the scratching abrasive resistance of ATO thin film prepared by sol–gel route [11,12]a novel sol–gel route has been proposed.In this technological process an organic–inorganic hybrid silica sol was used as the pre-cursor of protecting matrix.The ATO functional componentwas homogeneously distributed in a transparent silica matrix.The mixed structure is of benefit to preventing the crack of thin film in drying and annealing process [13].When a composite material containing two oxides with different pho-to index hopes to keep high transmittance in visible light re-gion the second phase component must be dispersed homogeneously into the amorphous matrix at a level of nanometer.In this work a transparent nanocomposite thin film com-posed of ATO and silica was synthesized by the sol–gel route.The sol–gel method includes (a)the synthesis of ATO sol and hybrid organic–inorganic silica sol;(b)mixing of two nanoparticulate sols.A TEM investigation of phase structure in ATO–silica composite gel is reported.The optical proper-ties and crystallizability of composite thin film is discussed.2.Experimental2.1.Preparation of ATO aqueous solAll the chemical reagents used in the synthesis experi-ment were obtained from commercial sources without0167-577X/$-see front matter D 2005Elsevier B.V .All rights reserved.doi:10.1016/j.matlet.2004.12.033*Tel.:+865515591477;fax:+865515591434.E-mail address:chenxiaochuan126@.Materials Letters 59(2005)1239–1242/locate/matletfurther purification.The aqueous ATO sol were prepared by a co-precipitation process from hydrolysis of SnCl4d5H2O and SbCl3,and followed by the peptization of the precipitate. The reaction was performed at room temperature.In the co-precipitation procedure aqueous NH4OH solution was added directly to the mixture solution of SnCl4d5H2O and SbCl3 until the pH of the mixture reach6–8,where pale yellow ATO hydroxide precipitate were produced.Peptization of ATO hydroxide with the aqueous solution containing oxalic acid gives a yellowish transparent sol.Finally ATO sol was heated and refluxed at608C for4h.2.2.Synthesis of hybrid organic–inorganic silica solThe hybrid organic–inorganic silica-based sols were synthesized as follows:First a mixture solution of tetrae-thoxysilane(TEOS),3-glycidoxypropyltrimethoxysilane (GPTS),isopropyl and alcohol in weight ratio1:1:2.5:3.5 was prepared.Then a suitable amount of deionized water (pH=1,by HCl addition)was added to the mixture solution. The mole ratio of TEOS and H2O is about1:6to1:8.The mixed solution was stirred and heated under reflux at808C for16h.The synthesized transparent hybrid silica sol was used as protecting component of nanocomposite thin film.2.3.Preparation of ATO/SiO2nanocomposite thin filmsA transparent functional gelled film was deposited from the mixture sol comprising the hybrid organic–inorganic silica sol and the ATO sol.Deposition was performed on the glass substrate at room temperature by a simple dip coating process.After being dried at room temperature the nano-composite gelled thin film was thermally densified at a temperature up to4008C in a reducing atmosphere containing N2and vapor of alcohol.2.4.InstrumentationThe Zeta potential measurement of the0.5wt.%ATO aqueous sol was carried out with a ZETASIZER3000HS A measuring system(MALVERN).0.1N HNO3was used to adjust the pH of reference ATO sol that does not contain oxalic acid.The X-ray diffractometer(XRD)was used for the structural characterization of the as-dried and thermally densified ATO–SiO2nanocomposite material.The micro-structure feature of nanocomposite gel film and annealed film were observed with a transmission electron microscope (TEM)(type JEM-2010).The sample for TEM study was prepared as follows:A droplet of mixed sol consisting of ATO colloidal sol and hybrid silica sol was dropped on a copper grid covered with organic film,and after solvents were vaporized a nanocomposite thin film was deposited on the copper grid.The chemical composition of annealed nanocomposite thin film was measured using an energy dispersive X-ray analysis system(EDS)equipped with a scanning electron microscope.Optical transmission was determined using a Varian Cary5E spectrophotometer in the wavelength range of300–2500nm.3.Results and discussion3.1.Surface adsorption studiesWhen oxalic acid was added to the ATO suspension the pH of suspension was adjust to2by the ionization of oxalic acid.Peptization with oxalic acid turns slowly the initial turbid ATO suspension into transparent stable sol.If without addition of oxalic acid ATO nanoparticles in the suspension will show aggregating behavior and begin precipitating at pH b5.The experimental result tells us that colloidal stability of ATO sol comes from addition of oxalic acid.Oxalic acid molecule acts as a surface-modifying agent and prevents aggregation of ATO particles.Fig.1shows the result of Zeta potential measurement at different pH level.The date shows that surface of ATO nanoparticles in aqueous sol is positively charged at pH\5without the addition of oxalic acid.The addition of oxalic acid decreases the Zeta potential of surface and changes the surface to a negative charge in the pH range2–4.According to the dissociation constant of oxalic acid the neutral molecules and negatively charged HO–(CO)2–OÀ1ions are predominant components in aqueous solution at2b pH b3.In initial suspension surface of ATO nanoparticles has a charge especially opposing the oxalic acid ions.The electrostatic force generated by the opposing charges will facilitate the ions transport stage of adsorption reaction.Now we assume that markedinteraction Fig.1.Zeta potential of ATO aqueous sol as a function of pH;0.5wt.% ATO content was used.X.C.Chen/Materials Letters59(2005)1239–1242 1240exist between oxalic acid ions and positive surface hydroxylgroups Q Sn–OH 2+or neutral surface hydroxyl groups Q Sn–OH.The oxalic acid ions can be preferentially adsorbed to the surface of ATO nanoparticles by hydrogen bond or Q Sn–O–C bond.The adsorbed ions neutralize surface positive charges and ultimately reverse the surface to a negative Zeta potential.Fig.1shows that the magnitude of negative Zeta potential is not large enough to stabilize the ATO nanoparticle electrostatically in sol.After oxalic acid was added to the suspension the transparent sol is found to remain stable almost infinitely at pH b 4.The only possible explanation is that effective dispersion mechanism comes from a combination of electrostatic and steric repulsion between oxalic acid ions that were adsorbed on surface of different ATO particles.3.2.XRD and EDS studiesFig.2shows XRD spectra of the ATO–silica nano-composite sample.The pattern (a)relates to the nano-composite gel obtained as dried at room temperature and the pattern (a)shows the presence of a very broad diffraction peak attributable only to cassiterite structure.The XRD patterns of nanocomposite samples show little difference between as-dried and thermally densified samples.Theresult indicates that ATO colloidal particles have developed a nanocrystal structure of cassiterite during sol preparation which contains a hydrothermal process at 608C.TheFig.2.XRD pattern of ATO–SiO 2composite gel:(a)as-dried at room temperature;(b)heat-treated at 5008C in air for 1h.Table 1Elemental concentration of ATO/SiO 2nanocomposite thin film Sample Atomic concentration,%V olume ratio,SiO 2/ATO O Si Sn Sb As-dried69.6917.2510.722.351.5Fig.3.Diffraction pattern and TEM image of ATO–SiO 2nanocomposite thin film as-dried at room temperature:(a)ED pattern;(b)TEMimage.Fig.4.Diffraction pattern and TEM image of ATO–SiO 2composite thin film thermal-treated at 3008C in reducing atmosphere for 2h:(a)ED pattern;(b)TEM image.X.C.Chen /Materials Letters 59(2005)1239–12421241hydrothermal process under atmosphere is also an effective method for promoting the crystallization of ATO nano-particles in the aqueous solution [14,15].The element contents in ATO–SiO 2film are shown in Table 1.Measured Si/Sn+Sb atom ratio of sample is about 1.3:1.The SiO 2/ATO volume ratio in the nanocomposite is calculated from the atom ratio and theory density.3.3.TEM and UV–Vis–Nir spectra studiesThe TEM image of as-dried ATO–SiO 2nanocomposite thin film is shown in Fig.3(b).We can observe that ATO nanoparticles are homogeneously dispersed in SiO 2-based amorphous matrix without any evidence of aggregation.ATO grains are found to have a size range of 3–5nm in diameter.Fig.3(a)shows a typical electron diffraction pattern of ATO nanocrystalline grain.Four electron dif-fraction (ED)rings can be indexed to the pattern of ATO with cassiterite structure.The result is in good agreement with XRD analysis.The structural change induced by thermal treatment of ATO thin film has been investigated.Fig.4shows the ED pattern and TEM image taken from ATO–SiO 2nanocomposite thin film which was annealed at 3008C in reducing atmosphere.The contrast morphology in this image shows some large crystal grains with diameter range from 20nm to 25nm.The ED pattern taken from the same sample contains some sharp spots resulting from thelarge crystallites.The observed results indicate that thermal treatment in reducing atmosphere can accelerate grain growth of ATO nanoparticles.The growth of crystal grain was accompanied by the disappearance of grain boundary and increased electrical conductivity and Nir-light reflec-tance of ATO film [1].The optical transmission spectra of ATO thin film deposited on the glass substrate of 1mm thick are shown in Fig.5.A high transmission of 85%is observed in the visible region.The reduction of transmission in the Nir wavelength arises from improved conductivity of nanocrystalline ATO particles that were heat-treated in the reducing atmosphere.4.ConclusionsThe transparent ATO–SiO 2nanocomposite thin films have been prepared successfully by the sol–gel method.The transmission of thin film is rather high in the visible region,range between 85%and 90%as well as the transmission in Nir region has been decreased to 41%.The thermal treatment in reducing atmosphere is an effective method for promoting crystalline grain growth of ATO nanoparticles.The oxalic acid is an excellent dispers-ing agent for ATO nanoparticle in the aqueous solution in pH range 2–4.References[1]G.Frank,E.Kauer,H.Kostlin,Thin Solid Films 77(1981)107.[2]M.S.Castro,C.M.Aldao,J.Eur.Ceram.Soc.20(2000)303.[3]O.Safonova,I.Bezverkhy,P.Fabrichnyi,M.Rumyantseva, A.Gaskov,J.Mater.Chem.7(1997)997.[4]S.Shanthi,C.Subramanian,P.Ramasamy,Cryst.Res.Technol.34(1998)1037.[5]A.E.Rakhshani,Y .Makdisi,H.A.Ramazaniyan,J.Appl.Phys.83(2)(1998)1049.[6]C.Goebbert,R.Nonninger,M.A.Aegerter,H.Schmidt,Thin SolidFilms 351(1999)79.[7]C.Terrier,J.P.Chatelon,J.A.Roger,Thin Solid Films 295(1997)95.[8]H.Ohsaki,Y .Kokubu,Thin Solid Films 351(1999)1.[9]M.A.Aegerter,N.Al-Dahoudi,J.Sol–Gel Sci.Technol.27(2003)81.[10]A.N.Banerjee,S.Kundoo,P.Saha,K.K.Chattopadhyay,J.Sol–GelSci.Technol.28(2003)105.[11]S.W.Kim,Y .W.Shin,D.S.Bae,J.H.Lee,J.Kim,H.W.Lee,ThinSolid Films 437(2003)242.[12]K.Abe,Y .Sanada,T.Morimoto,J.Sol–Gel Sci.Technol.26(2003)709.[13]J.Gallardo,A.Duran,I.Garcia,J.P.Celis,M.A.Arenas,A.Conde,J.Sol–Gel Sci.Technol.27(2003)175.[14]D.Y .Zhang,D.Z.Wang,G.M.Wang,Y .H.Wu,Z.Wang,Mater.Sci.Eng.,B,Solid-State Mater.Adv.Technol.8(1991)189.[15]S.J.Kim,S.D.Park,Y .H.Jeong,S.Park,J.Am.Ceram.Soc.82(1999)927.Fig.5.UV–Vis–Nir transmission spectra:(a)550nm thick ATO–SiO 2thin film which was coated on glass substrate;(b)glass substrate.X.C.Chen /Materials Letters 59(2005)1239–12421242。

一种α,β不饱和羧酸亚胺酯的合成、表征与晶体结构

第38卷第3期2019年9月中南民族大学学报(自然科学版)Journal of South-Central University for Nationalities(Natural Science Edition)Vol.38No.3Sep.2019一种a,卩不饱和竣酸亚胺酯的合成、表征与晶体结构吴滨，范誌，王吉庆，杨金明*(中南民族大学药学院，武汉430074)摘要报道了一种烯酮亚胺反应活性中间体的重排产物一a,卩不饱和竣酸亚胺酯化合物的合成，并通过核磁共振氢谱和X射线单晶衍射对其结构进行了表征.单晶X-衍射分析表明:该化合物三斜晶系,P-1空间群，晶胞参数a=7.9832(2)A,6=8.3409(2)A,c=14.5288(4)A,a=81.1650(10)°,0=74.4740(10)°,■/=63.9960(10)°,卩= 837.03(4)F.实验结果为烯酮亚胺的重排反应这一化学理论提供了有力的证据.关键词烯酮亚胺;重排反应;晶体结构中图分类号0621.3文献标识码A文章编号1672-4321(2019)03-0357-05DOI10.12130/znmdzk.20190307引用格式吴滨，范詰，王吉庆，等.一种a,0不饱和竣酸亚胺酯的合成、表征与晶体结构［J］.中南民族大学学报(自然科学版),2019,38(3)：357-361.WU Bin,FAN Zhe,WANG Jiqing,et al.Synthetic characterization and crystal structure of a ketenimine rearrangement products［J］.Journal of South-Central University for Nationalities(Natural Science Edition),2019,38(3)：357-361.Synthetic characterization and crystal structure of aketenimine rearrangement productsWU Bin,FAN Zhe,WANG Jiqing,YANG Jinming(School of Pharmaceutical Sciences,South-Central University for Nationalities,Wuhan430074,China)Abstract The synthesis of an a,P-unsaturated carboximidate via a rearrangement reaction of ketenimine was reported.The compound was characterized by1H NMR and single crystal X-ray diffraction.X-ray diffraction analysis of single crystal shows that the compound belongs to the triclinic crystal system and is crystallized in space group P-1,cell parameters:a=7.9832(2)A,6=8.3409(2)A,c=14.5288(4)A,a=81.1650(10)°,/3=74.4740(10)0,y=63.9960(10)°,7=837.03(4)A3.It provides strong evidence for the chemical theory of rearrangement chemistry of ketenimine.Keywords1,2,3-triazoles；ketenimines；rearrangement chemistry；crystal structureCuAAC(Copper-Catalyzed Azide-Alkyne Cycload dition)反应,是指在Cu⑴催化剂存在的条件下,叠氮化物与末端烘桂通过分步反应发生1,3-环加成反应生成1,4-二取代-1,2,3-三氮哩的反应⑴.该反应以其温和的反应条件、优异的收率和普适性引起了广泛的关注⑵.1,4-二取代-1,2,3-=氮哩因其独特的化学结构也成了金属有机化学家们的一个热点研究领域•通常，在过渡金属铐(II)的催化作用下, 1,4-二取代-1,2,3-三氮哩极易失去一分子氮生成a-亚胺基铐卡宾,从而有效地替代危险的重氮试剂.这种独特的反应模式使其成为一种非常稳定、安全的铐卡宾前体卩⑷.三氮哩产生a-亚胺基链卡宾后参与的反应非常丰富，多个课题组相继报道了该活性中间体与烯燈"句、块燈刀、醛和亚胺剧、a,0-不饱和醛⑼、联烯少］、异氤酸酯和异硫氤酸酯⑴］、以及1, 3-二烯①］的环加成反应，合成多种类型的杂环化合物•施敏小组报道了链(II)催化官能团化的1,2,3-三氮哩类底物合成氮桥苯并二氧环庚烷衍生物［闵，收稿日期2019-06-12*通信作者杨金明，研究方向:有机合成,E-mail：jmyang@作者简介吴滨(1973-)，男，教授，博士，研究方向:有机合成,E-mail：2015084@基金项目国家自然科学基金资助项目(21772236)；中央高校基本科研业务费专项资金资助项目(CZT18012)358中南民族大学学报（自然科学版）第38卷1,2-二氢异座咻和1-苗酮类化合物M ,3-亚甲基-2,3-二氢苯并咲喃和3-亚甲基-2,3-二氢阿嗥类化合物［⑸.几乎同时，利用相同的底物，仅仅改变反应条件，在体系中加入醇或者水作为亲核试剂,杨震课题组少］报道了二氢异苯并咲喃和苗酮类化合物的合成•最近,李传莹小组M 报道了铐（II ）催化1,2,3-三氮哩与乙烯基瞇化合物串联合成了系列哌腱衍生物.从简单化合物合成具有结构多样性的复杂分子一直是有机合成领域的一个挑战问题，围绕click 化学发展多组分串联反应为此问题提供了一个强有力的策略•近年发现,在一些烘烧化合物中,铜催化产生环加成中间过渡态后会脱去一分子氮生成烯酮亚胺的结构,烯酮亚胺中间体会进一步接受亲核试剂进攻,发生重排反应,得到a ,0-不饱和亚胺化合物.Punniyamurthy 小组购报道了一价铜催化烘醛，苯酚以及磺酰叠氮在温和条件下一步合成芳基甲基醵类香豆素衍生物，并提出了可能的机理.在一价铜的催化下,烘桂与磺酰叠氮发生［3 + 2］环加成生成中间体A, A 失去一份子氮并再生一价铜催化剂后产生烯酮亚胺中间体B ［19］，氧上的孤对电子进攻中间体B,可能通过四元环两性离子过渡态C 进行拟态周环的［1,3］-迁移重排⑵如，从而得到中间体D,再与苯氧基负离子发生1,4共辄加成反应和瓮醛缩合反应最终得到目标化合物（图1） •O『N 、ySC )2R + ArOHCu(l), base TBAIArOH baseTBAI图1 Pimniyamurthy 小组提出的烯酮亚胺重排可能机制Fig.l Possible mechanism of ketimide rearrangement proposed by Punniyamurthy groupD为了进一步验证并完善该反应机理,设计通过水杨酸甲酯la 为原料合成底物2a,再通过CuAAC 反应合成目标化合物3a.结果除了以21%的分离收率得到目标化合物3a 之外,还意外得到了 41%的主产物3b.核磁谱图及高分辨质谱对化合物3b 的结构进行了初步表征解析,并进一步通过X-射线单晶衍射确定了化合物3b 的结构（图2和3）.图2化合物2a 、3a 以及3b 的合成Fig.2 Synthesis of 2a,3a and 3bOMe3b, 41%yield第3期吴滨，等:一种a,卩不饱和竣酸亚胺酯的合成、表征与晶体结构3591实验部分1.1仪器与试剂'H NMR在Bruker AM-600上测定，氛代试剂为Cambrige生产,TMS作为内标物，化学位移单位为ppm.HRMS在Agilent6200Q-TOF上测定.X-射线单晶衍射通过BRUKER D8QUEST测定.水杨酸甲酯、烘丙基漠以及对甲苯磺酰叠氮等试剂从Alfa Aesar、韶远、安耐吉、阿拉丁、TCI、柏卡等公司购买.除甲苯进行了回流重蒸除水(Call?)，其他试剂使用前未经任何处理.1.2化合物2a的合成称取水杨酸甲酯(30mmol,3.9mL)和碳酸钾(60mmol,8.30g)于50mL圆底烧瓶中，加入20 mL N,N-二甲基甲酰胺(DMF)溶解，室温下搅拌，将烘丙基漠(36mmol,3.1mL)缓慢滴加进烧瓶中，搅拌过夜•加入200mL水溶液淬灭反应，加入乙酸乙酯萃取3次，然后合并有机相,用饱和食盐水水洗有机相,再用无水硫酸钠干燥有机相,减压浓缩,通过柱层析进行粗分离纯化(石油矽乙酸乙酯=10/1)得浅黄色油状液体2a6.1g.2a为已知化合物NMR数据与文献报道炉］的一致.1.3化合物3a,3b的合成与3b的表征在N?氛围下，将2a(5mmol,957mg)与CuTC (0.1mmol,19mg)加到50mL圆底烧瓶中,加入干燥的甲苯(15mL),随后边搅拌边缓慢滴加对甲苯磺酰叠氮(5mmol,1.1mL),室温下搅拌过夜.反应结束后，将溶液通过硅藻土过滤，乙酸乙酯冲洗，减压旋干浓缩，柱层析分离(石油醯/乙酸乙酯=5/ 1),得浅黄色固体442mg3a,产率23%,白色固体741mg3b,产率41%.化合物3a」H NMR(600MH z,CDC13)88.33 (s,lH),8.01(d,J=&4Hz,2H),7.85(dd,_7= 7.7,1.8Hz,lH),7.47(ddd,J=8.4,7.4,1.8Hz, lH),7.41-7.36(m,2H),7.08-7.02(m,2H),5.29 (s,2H),3.91(s,3H),2.45(s,3H).13C NMR(151 MHz,CDC13)8166.34,157.56,147.56,144.44,133.87,132.97,132.08,130.58,128.87,122.90, 121.55,120.71,114.16,63.23,52.22,21.98.化合物3b.iH NMR(600MH z,CDC13)87.97 (ddj=7.8,1.7Hz,lH),7.56(d,J=8.3Hz,2H), 7.53(td,J=7.9,1.7Hz,lH),7.35(q,lH),7.30 (tdJ=7.7,1.0Hz,lH),7.17(d J=&1Hz,2H), 7.10(ddj=&1,0.9Hz,lH),6.68(dd,J=17.0, 1.0Hz,lH),6.16(ddj=10.9,1.0Hz,lH),3.69 (s,3H),2.36(s,3H).13C NMR(151MH z,CDC13) 8166.18,164.79,151.07,143.35,138.42,134.02, 132.64,131.95,129.32,126.70,126.49,125.38, 123.46,123.20,52.39,21.63.HRMS calcd for[C18 H17NO5S]requires359.0827,found360.0892[M++ H]；382.0712[M++Na].单晶培养:取50mg3b溶解于少量二氯甲烷中，加入正己烷和正戊烷的混合溶剂后于室温下静置1 d,得到无色块状晶体.1.4晶体结构测定配合物的单晶结构数据在BRUKER D8 QUEST,BrukerShekTL软件包解析和优化该结构,多扫描方法(SADABS)对吸收效应进行数据校正,晶体结构用直接法求解,所有非氢原子使用全矩阵最小二乘法对F2进行各项异性修正,用理论加氢法对氢原子进行加和至理论位置.2结果与讨论2.1晶体结构鉴定和描述化合物3b(C18H17NO5S)的晶体数据和有关数据收集及结构精修数据列于表1,相关键长和键角数据列于表2.晶体编号:JM1-29-1.化合物3b的晶体结构如图3所示,是一种无色块状晶体，属三斜晶系,P-1空间群，相对分子量M=359.38,近似尺寸为0.160mm X0.337mmX0.410mm.X-ray晶体分析表明，晶胞参数a=7.9832(2)A,6=8.3409(2)k,c= 14.5288(4)A,a=81.1650(10)°,0=74.4740(10)°, y=63.9960(10)°,V=837.03(4)A3.360中南民族大学学报（自然科学版）第38卷表1化合物3b的晶体数据和结构精修数据Tab.l Crystal data and structure refinement for compound3b晶体参数晶体数据Chemical fbnnula C18H17NO5SFormula weight359.38g/molTemperature150(2)KWavelength 1.54178ACrystal size0.160x0.337x0.410mmCrystal habit light colourless BLOCKCrystal system triclinicSpace group P-1Unit cell dimensions a=7.9832(2)A a=81.1650(10)°Volume 几&3409(2)A j8=74.4740(10)°c=14.5288(4)A y=63.9960(10)°837.03(4)A3Z2Density(calculated) 1.426g/cm3Absorption coefficient 1.981mm-1F(000)376Theta range for data collection 3.16to79.24°Index ranges—10W h W10,-9W k W10,-18W I W18 Data/restraints/parameters3580/0/228Final R indices3543data；I>2cr(I)R1=0.0318,wR2=0.0859Weighting scheme Largest diff.peak and hole all data R1=0.0321,wR2=0.0862 w=l/[ct2(F qz)+(0.0455P)2+0.3479P] Where P=(F02+2F c2)/30.355and-0.471eA~3R.M.S.deviation from mean0.046eA~3表2是烯酮亚胺重排区域的相关键长键角.因为晶体结构C1-C2-C3-C4-C5-C12-C11,包括O4-S1-03区域是对甲苯磺酰基,C7-C16-C15-C14-C13-C8和05-C9-02-C10这部分对应水杨酸甲酯区域.根据晶体结构.C17-C18的碳碳双键与C6-N1的碳氮双键是处于反式共辄构型，因而能得到热力学稳定的3b.这为Punniyamurthy[6]小组提出的伪周环四元环状过渡态机理猜想提供了有力的证据，同时他们提出的机理中化合物D的画法是顺式共辄的构型，经过本实验的单晶验证,可以修正为反式共辄画法，这样更为严谨（图3）.表2配合物1的有关键角和键长数据Tab.2Selected bond lengths and angles for compound1图3化合物3b的晶体结构图Fig.3Molecular structure of compound3b 3结语键型键长/A键角类型键角/e O(l)-C(6) 1.3448(14)C(6)-O(l)-C(7)117.85(9) 0(l)-C(7) 1.4077(14)C(6)-N(1)-S1)126.83(9) N(l)-C(6) 1.2832(16)O(l)-C(6)-C(17)112.15(10) N(l)-S(l) 1.6366(10)N(l)-C(6)-O(l)117.78(10) C(6)-C(17) 1.4701(16)N(l)-C(6)-C(17)130.06(11) C(17)-C(18) 1.3144(19)C(6)-C(17)-C(18)122.10(12)使用CuAAC反应条件与设计的底物反应，意外合成出了化合物3b,通过中NMR、HRMS以及X-射线单晶衍射证实了化合物3b的确切结构.首次报道了烯酮亚胺发生迁移重排反应后的产物的单晶结构,为烯酮亚胺的重排化学提供了有力的证据,并为烯酮亚胺作为有机反应活性中间体发展更多有机合第3期吴滨，等:一种a,卩不饱和竣酸亚胺酯的合成、表征与晶体结构361成方法学提供了理论依据，基于烯酮亚胺为中间体的新型有机合成方法学的开发正在进一步探索中.参考文献[1]ROSTOVTSEV V V,GREEN L G,FOKIN V V,et al.Astepwise huisgen cycloaddition process:copper(I)catalyzedregioselective"ligation”of azides and tenrnnal alkynes[J].Angew Chem Int Ed,2002,41(14):2596-2599.[2]DAVIES H M L,ALFORD J S.Reactions of metallocarbenesderived from TV-sulfbnyl-1,2,3-triazoles[J].Chem Soc Rev,2014,43：5151-5162.[3]CHATTOPADHYAY B,GEVORGYAN V.Transition metalcatalyzed denitrogenative transannulation:Convertingtriazoles into other heterocyclic systems[J].Angew Chem IntEd,2012,51：862-872.[4]GULEVICH A V,GEVORGYAN V.Versatile reactivity ofrhodium-iminocarbenes derived from TV-sulfonyl triazoles[J].Angew Chem Int Ed,2013,52：1371-1373.[5]HOR1NEFF T,CHUPRAKOV S,CHERNYAK N,et al.Rhodium-catalyzed transannulation 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Synthesis and characterization of metal complexes

Synthesis and characterization ofmetal complexesIntroductionMetal complexes have been actively studied due to their potential applications in various fields such as catalysts, materials, and medicine. The synthesis and characterization of metal complexes are fundamental steps towards understanding their properties and behaviors. In this article, we will discuss some of the methods and techniques used for synthesizing and characterizing metal complexes, as well as their applications.Synthesis of metal complexesThe synthesis of metal complexes can be achieved through various methods such as salt metathesis, ligand exchange, and coordination polymerization. Salt metathesis involves replacing one metal ion in a salt with another metal ion. Ligand exchange involves replacing one ligand in a metal complex with another ligand. Coordination polymerization involves the combination of metal ions and organic ligands to form a three-dimensional network structure.One example of a metal complex synthesis method is ligand exchange. In this method, a metal complex with a specific ligand is reacted with a new ligand to form a different metal complex. For example, the reaction between copper(II) sulfate and sodium acetate results in the formation of copper(II) acetate.CuSO4 + 2NaOAc → Cu(OAc)2 + Na2SO4Another example is coordination polymerization. In this method, metal ions and organic ligands are combined in a solution to form a solid network structure. For example, the reaction between zinc(II) nitrate and 2,6-naphthalenedicarboxylic acid results in the formation of a porous coordination polymer called MOF-5.Zn(NO3)2 + H2bdc → Zn4O(H2bdc)3 + 2HNO3Characterization of metal complexesCharacterization of metal complexes is important in understanding their physical and chemical properties. Techniques such as X-ray crystallography, infrared spectroscopy, and nuclear magnetic resonance (NMR) spectroscopy can be used to identify the structure and composition of metal complexes.X-ray crystallography involves the analysis of crystals using X-rays to determine the positions of atoms in a molecule. It provides information on the three-dimensional structure of a metal complex. Infrared spectroscopy involves the measurement of the energy absorbed by a molecule due to vibrations of its chemical bonds. It provides information on the functional groups present in a metal complex. NMR spectroscopy involves the measurement of the absorption of energy by nuclei in an external magnetic field. It provides information on the electronic environment surrounding metal ions in a complex.Applications of metal complexesMetal complexes have a wide range of applications in various fields. They can act as catalysts in chemical reactions, for example, the use of palladium complexes as catalysts in Suzuki coupling reactions. They can also be used as materials in the form of coordination polymers for gas storage or catalysis. In medicine, metal complexes can be used as contrast agents in imaging techniques or as anticancer drugs.ConclusionIn summary, the synthesis and characterization of metal complexes are important for understanding their properties and behavior. Various methods and techniques can be used for synthesizing and characterizing metal complexes. Applications for metal complexes are diverse and extend to fields such as catalysis, materials, and medicine. With continued research and development, metal complexes are expected to play an increasingly important role in these fields.。

Cu_Co_Al类水滑石的合成_表征及吸附NO_x性能的研究

2005 年 4 月Journal of Chemical Engineering of Chinese Universities Apr. 2005 文章编号：1003-9015(2005)02-0223-05Cu-Co-Al类水滑石的合成、表征及吸附NO x性能的研究倪哲明1, 俞卫华2, 王力耕1, 郭志强1, 葛忠华1(1. 浙江工业大学化工学院, 浙江杭州 310032; 2. 浙江工业大学之江学院, 浙江杭州 310024)摘要：采用共沉淀法合成了铜钴铝不同摩尔投料比的碳酸根型水滑石(Cu/Co/Al摩尔比分别为111, 121,∶∶∶∶∶∶∶∶∶∶∶∶∶∶。

用X-射线粉末衍射、红外光谱、热重-差热分析对它们进行了表征，131,141,151,161,171)∶∶时测定了Cu-Co-Al类水滑石和活性炭对氮氧化物的吸附性能。

结果表明，Cu-Co-Al的摩尔比在111∶∶~171合成的复合金属氧化物都具有水滑石结构，Co的含量增加，水滑石层间高度略有增加。

红外光谱分析结果表明羟基和碳酸根被插入到水滑石层间结构。

热重-差热分析结果显示合成样品的分解均有两个过程, 且含Co量增加，热稳定性减弱。

二元的Co3Al-HTlc吸附NO x优于三元的CuCoAl-HTlcs和活性炭，CuCo3Al-HTlc对NO x吸附性能优于其它三元的CuCoAl-HTlcs。

Co3Al-HTlc和CuCo3Al-HTlc吸附容量分别为1781mg⋅g−1、12861mg⋅g−1。

关键词：铜钴铝类水滑石；制备；表征；吸附中图分类号：O643 文献标识码：ASynthesis, Characterization and NO x Absorption Capability ofCu-Co-Al Hydrotalcite-like CompoundsNI Zhe-ming1, YU Wei-hua2, WANG Li-geng1, GUO Zhi-giang GE Zhong-hua1(1. College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310032, China;2. College of Zhijiang, Zhejiang University of Technology, Hangzhou 310024, China) Abstract: Carbonate pillared hydrotalcite-like compounds ( CuCoAl-HTlcs ) with different Cu/Co/Al molar ratios were synthesized by coprecipitation and characterized by XRD, IR and TG-DTA. The NO x adsorption capabilities of the CuCoAl-HTlcs and activated carbon were also measured. The results show that the samples with Cu/Co/Al molar ratios of 1:1:1, 1:2:1, 1:3:1, 1:4:1, 1:5:1, 1:6:1 and 1:7:1 have hydrotalcite structures, and their interlayer spacings increase with the amount of Co in the samples. The IR results show that carbonation and hydroxyl are intercalated into the CuCoAl-HTlcs interlayer structures. The TG-DTA results show that the materials decompose in two stages, and their thermal stability decreases with the increase of Co content in the samples. The NO x adsorption ability of the Co3Al-HTlc is much better than that of CuCoAl-HTlcs and activated carbon, and that of CuCo3Al-HTlc is better than the other CuCoAl-HTlcs. The adsorption capacities of the Co3Al-HTlc and CuCo3Al-HTlc are 1781mg⋅g−1 and 1286 mg⋅g−1, respectively.Key words: Cu-Co-Al hydrotalcite-like compounds; preparation; characterization; adsorption1 前言水滑石(Hydrotalcites) 是一类具有层状微孔结构的双羟基金属复合氧化物。