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1.
基于(1E,2E)-N1,N2-双((8-丁氧基喹啉-2-)亚甲基)乙烷-1,2-二胺的双核银配合物被合成,用1H NMR,单晶衍射表征其结构.该配合物I是一个三斜晶体,空间群为P-1,其余参数是:a=13.489(5)?,b=13.550(5)?,和c=19.836(8)?,α=70.077(6)°,β=75.145(9)°,γ=82.430(6)°,V=3291(2)?3,Z=2,C60H68Ag2F12N8O5P2, Mr=1486.90,Dx=1.500 g/cm3,T=296(2)K.晶体结构显示8-羟基喹啉衍射物是一个四齿配体,链接两个银离子.在室温下,用乙腈作为溶剂,浓度为1×10 -6mol· L-1,8-羟基喹啉衍射物与配合物I有相似的荧光光谱.  相似文献   

2.
水热条件对合成WO3纳米棒形貌和光吸收特性的影响   总被引:1,自引:1,他引:0       下载免费PDF全文
以钨酸钠为原料,硫酸钾为辅助盐,在强酸性反应体系通过水热法合成了WO3纳米棒.利用XRD,SEM,TEM和SAED等对产物进行了表征,结果表明:在水热体系中合成WO3纳米棒时,增加pH值、升高反应温度和延长反应时间,都有利于合成WO3纳米棒.在pH值为1.5、反应温度为240℃和反应时间72h下合成直径小于100nm的WO3纳米棒,此WO3米棒直径分布较均匀.对不同条件下合成的WO3进行紫外-可见光的吸收光谱分析可知,随着pH值的增加、反应温度的升高和反应时间的延长,获得的WO3样品的光吸收能力逐渐增加.  相似文献   

3.
在甲醇中用三氯化铋或三氯化锑分别与L-色氨酸(Htrp)和8-羟基喹啉(8-Hhq)合成了三元配合物M(trp)_2(8-hq) [M=Sb(Ⅲ),Bi(Ⅲ)].用元素分析、X射线粉末衍射和红外光谱对三元配合物进行了表征,研究了其热性质和电化学性质.对XRD数据进行了指标化,结果表明:2种三元配合物均属于单斜晶系, Sb(trp)_2(8-hq)的晶胞参数为:a=1.9322 nm,b=2.3938 nm,c=1.8736 nm,β=99.981°;Bi(trp)_2(8-hq)的晶胞参数:a=1.8938 nm,b=1.6168 nm,c=1.0482 nm,β=95.020°.  相似文献   

4.
以CaCO3和CaHPO4·2H2O为前驱体,采用水热法制备了羟基磷灰石(HAP)晶体,利用X射线衍射(XRD)、扫描电镜(SEM)及X射线能谱分析仪(EDS)系统研究了pH值、水热温度、反应时间、Ca2+浓度等条件对合成HAP晶体微结构及晶体生长的影响,同时对其生长机理进行了探讨.结果表明:随着水热合成温度的升高、时间的延长、Ca2浓度的增加,晶体发育越完整,HAP晶体的长径比呈增大趋势;体系的pH值对HAP晶体的生长有较大的影响,随着pH值的增加HAP晶粒的大小、长径比减小趋势明显;在水热温度为200℃,pH值=10,时间8h的条件下,可得到结晶度高、晶形完整清晰,端面尺寸在50~ 70 nm,生长极性明显的六方柱状的一维n-HAP晶体.EDS分析结果证实合成的HAP平均钙磷比约为1.70左右,同理论值比较相符.点分析研究表明晶体端面的钙磷比比平均的略高,钙磷比约为1.75,从而证明了Ca2+的浓度直接影响着HAP晶体的极性生长.  相似文献   

5.
以氧化钇、硝酸和硝酸铁为原料,氢氧化钾为矿化剂,采用水热合成法制备了钙钛矿结构铁酸钇正铁氧体(YFeO3)微晶.研究了水热反应时间、温度和溶液pH值对产物的物相组成、粒径大小和磁性能的影响,研究结果表明,在实验条件所在区间内,随着反应时间的增加和反应温度的升高,产物纯度逐渐变高.合成纯相YFeO3需要在一定的溶液pH值范围内.随溶液pH值的降低,产物颗粒的粒径变小,粒径分布变窄,并且晶粒的磁化强度增大.最佳的合成条件是pH值为9.5,温度为260℃,反应时间为60h.  相似文献   

6.
以正硅酸乙酯、镁盐和铝盐为原料,通过溶胶-凝胶法合成堇青石粉体,通过TGA-DSC、XRD等测试手段,讨论了反应体系pH值和烧结温度对产物晶相和性能的影响.结果表明:体系pH值为2的试样,在900℃时,出现尖晶石相和假蓝宝石相,升温到1000℃的时候,开始有μ-堇青石出现,在1250℃煅烧2h几乎全部转化为α-堇青石,体系pH为7的试样,在900℃时,有μ-堇青石形成,经1250℃煅烧后,β-堇青石相增多,μ-堇青石相和镁铝尖晶石相消失,合成粉体的平均晶粒尺寸随pH值增加呈先减小后增加的趋势,在不同温度煅烧下的压片试样,体系pH值为7的试样收缩最大.  相似文献   

7.
合成了一个新的锌配合物[Zn(8-ahsb)(N3)](1)(8-ahsb=8-氨基喹啉水杨醛席夫碱阴离子),并对其进行了元素分析、红外光谱和X-射线单晶衍射表征.配合物1属于单斜晶系,空间群为C2/c,a=0.6762(3)nm,b=2. 2842(9)nm,c=1.8162(8)nm,β=91.309(7)°,V=2.805(2)nm3,Z=8.中心离子Zn(II)为三角双锥配位构型,分别与四个N原子、一个氧原子配位,其中1个8-氨基喹啉席夫碱配体提供了2个N原子、一个氧原子,剩余两个N原子分别来自于两个N3-阴离子,且每个N-3桥联邻近的两个Zn2+形成一维无限链状结构.荧光光谱的分析表明该化合物具有强的绿色发光性能,且可作为荧光探针检测低浓度的铜离子.  相似文献   

8.
本文采用水热法,以SnCl4·5H2O为前驱物,在180℃,填充度为68;,反应时间8h,强酸环境条件下合成了SnO2纳米金红相晶体,直径约为5~10nm,长30~100nm.加入一定量的NaOH,调节溶液pH值为强碱性(pH=11),同样条件下也合成了SnO2金红相纳米柱晶体,长200nm、直径10~20nm.提高水热反应的温度为430℃,矿化剂为3mol/L NaOH,反应时间24h,合成了亚微米金红相SnO2晶体,最大线度为300nm.  相似文献   

9.
以喹啉-2-甲酸与醋酸镍为原料,采用水热法合成配合物2[NiL2(H2O)2]·DMF(L=喹啉-2-甲酸根离子,DMF=N,N-二甲基甲酰胺),并通过X-射线单晶衍射、X-射线粉末衍射、元素分析、红外光谱、热重分析、荧光光谱对其进行结构解析和性质表征.晶体结构解析表明:标题配合物晶体属于正交晶系,空间群为Pna21;其晶胞参数是:a=2.06753(6)nm,b=0.82571(3)nm,c=2.34776(7)nm,V=4.0081(2)nm3,Z=4,Mr=951.210,Dc=1.576 g/cm3.标题配合物为单核配合物,配位单元之间通过分子间氢键和π-π堆积作用,把配合物扩展为三维超分子结构.荧光光谱分析表明配体和标题配合物均有良好的荧光性,且配合物荧光性优于配体.  相似文献   

10.
李梦  赵欣  刘亚飞 《人工晶体学报》2016,45(6):1635-1638
采用化学液相沉淀工艺制备了过氧化银(AgO)粉体,研究了Na2S2O8用量、反应体系的pH值、反应时间等制备工艺参数对AgO产率的影响,并采用X射线衍射仪(XRD)及扫描电子显微镜(SEM)对制备的AgO粉体进行了表征.结果表明,优选的制备工艺是将AgNO3、Na2S2O8和SDBS的质量比定为1∶4.4∶1,然后在反应体系的温度达到60℃后通过滴加NaOH溶液调整反应体系的pH值为13.00,并维持反应时间30 min.随着AgNO3与SDBS的质量比从2.5升高到20.0,AgO粉末颗粒的形貌从近似的球形转变为球状和片状结构的混合物.  相似文献   

11.
The aim of this review is to emphasize solvent free or green synthesis, a most efficient utilization of starting materials to give maximum yield, and an alternative route to producing novel promising materials. In this regard the phase diagram study has shown applications in the determination of the precise composition of binary compounds of a specific nature and in the identification of the parameters that affect the crystal growth. To provide an overview worthy of phase diagram, physicochemical, thermal and structure investigations; studies of eleven systems, namely, urea–m-nitrobenzoic acid, urea–p-nitrophenol, urea–resorcinol, benzoin–o-phenylenediamine, pyrene–m-dinitrobenzene, vanillin–p-anisidine, resorcinol–p-dimethylaminobenzaldehyde, benzophenone–diphenylamine, anthracene–picric acid, 8-hydroxyquinoline–salicylic acid and 8-hydroxyqunoline–1,2,3-trihydroxybenzene forming organic complexes, have been reported. In addition, the original data of a newly synthesized complex of m-hydroxybenzaldehyde (HB) and p-chloroaniline (CA) is being reported for the first time. The phase diagram of HB–CA system also shows the formation of a complex in 1:1 M ratio, and two eutectics on either side of the complex. The complex's formation was studied using FTIR, NMR, DSC and powder X-ray diffraction techniques. The thermodynamic parameters such as heat of mixing, entropy of fusion, roughness parameter, interfacial energy and excess thermodynamic functions were calculated using the heat of fusion values. The single crystal growth and the atomic packing studies of some of the complexes have confirmed the formation of complexes. The optical transmittance efficiency and transparency of novel HB–CA complex crystal were found to be 70% and 399 nm, respectively.  相似文献   

12.
MAX相是一种兼具金属和陶瓷性能的新型三元层状过渡金属碳氮化物。传统合成MAX相的方法都有一定的局限性,如反应温度较高、合成时间过长、合成样品较少,且大部分无法直接一步制备所需MAX相。近些年来,采用熔盐法合成MAX相的报道越来越多,并且工艺持续改进。本文从传统熔盐法合成MAX相出发,分析并阐述了新熔盐法合成MAX相的研究进展。传统熔盐法利用较低熔点的熔盐作为反应溶剂,提高了反应效率;熔盐屏蔽法以熔盐作为反应溶剂的同时还可防止氧化,使得反应可以在空气中进行;路易斯酸盐法则是将熔盐作为反应原料来合成MAX新相;熔盐电化学法以电脱氧的方式,将合成原料由纯金属改为金属氧化物,降低了生产成本。熔盐法所合成MAX相产物较传统方法所合成产物的产量及纯度更高,所需要的温度、能耗以及成本更低。因此,熔盐合成法是未来大批量合成MAX相以及MAX新相合成的一个重要方法。  相似文献   

13.
The synthesis and physical properties of meta- and para-bis(metallocene) benzene complexes with M = Fe, Co, Ni are reported. The electrochemical properties suggest greater electronic interaction between metal centers in the para-M complexes. In addition, the magnetic properties suggest different degrees of spin exchange for the meta and para complexes, with the latter exhibiting more pronounced antiferromagnetic coupling. These molecular complexes are considered prototypes for extended metallocene polymers.  相似文献   

14.
In the present report, CuO, Cu2O and Cu have been successfully synthesized through a facile, one‐step hydrothermal method at a relative low temperature by controlling only the concentration of citric acid. Compared with other synthetic methods, the present method is mild, high‐efficient and nontoxic. The crystal structure and morphology of the as prepared samples were characterized by X‐ray diffraction and scanning electron microscopy, respectively. The mechanism for the crystal phase and morphological changes with different citric acid concentrations were discussed. The possible reaction process of the synthesis was also studied on the basis of the experimental results. We hope that this facile, one‐step hydrothermal method could be used in controlling synthesis of other metals and metal oxides under appropriate experimental conditions.  相似文献   

15.
In the current paper we designed a simple glucose reduction route for synthesis of sheet‐like Cu dendrites on a high yield, using CuSO4 as the starting material. The reaction was carried out at 180 °C for 18 h in the absence of any structure‐directing agent. The product was characterized by X‐ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and electron diffraction (ED). Some factors influencing the shapes of Cu microcrystals, including the reaction temperature, time, and the concentration of the starting CuSO4, were investigated. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)  相似文献   

16.
以硝酸镧,氧化铕,硝酸锂,硝酸铋和偏钒酸铵为原料,采用简单的水热法合成了金属离子(Li~+,Bi~(3+))掺杂LaVO_4∶Eu~(3+)纳米荧光粉。通过XRD,SEM,FTIR,FL等手段进行表征。考察了金属离子(Li~+,Bi~(3+))摩尔掺杂浓度,反应温度,反应时间对LaVO_4∶Eu~(3+)荧光性能的影响,探讨合成Li~+,Bi~(3+)掺杂LaVO_4∶Eu~(3+)荧光粉的最佳条件。结果表明:所合成的产物以四方锆石结构(t-)LaVO_4纳米颗粒为主。Li~+,Bi~(3+)的掺杂,均能够提高荧光粉LaVO_4∶Eu~(3+)的发光强度;在180℃条件下反应24 h所得的LaVO_4∶5%Eu~(3+),4%Li~+,LaVO_4∶5%Eu~(3+),2%Bi~(3+)荧光粉荧光性能最佳。  相似文献   

17.
The precipitation of barium, zinc, lead, copper and silver chromates was studied in the presence of the chelating organic anions gluconate, tartrate, citrate, aspartate, glutamate and E.D.T. Aate. Generally, these chelators complex the metal cation and reduce the free metal cation and mean metal chromate concentrations in solution. The rates of nucleation with microcrystallite formation were then markedly reduced and the induction periods increased from below 1 sec to well above 100,000 sec with increasing chelator/cation concentration ratio; the experimental results were expressed by the relations; The coefficients F at any metal chromate concentration were related in turn to the stability constants of the metal-chelator complexes.  相似文献   

18.
王飞  田一光  张乔 《人工晶体学报》2017,(10):1992-1998
Sr_(0.975)Al_2Si_2O_8∶Eu_(0.025)~(2+)系列荧光粉利用高温固相法合成,系统研究了预烧温度、预烧时间、烧成温度和助溶剂硼酸的量对荧光体晶体结构和发光性能的影响;研究结果表明,各试样均为单斜晶系SrAl_2Si_2O_8,荧光体的X射线衍射强度、荧光体的晶粒尺寸及荧光体的发射强度,均随着预烧温度、预烧时间、烧成温度和助溶剂硼酸量的增加,呈先增加后减小的变化趋势。当预烧温度为1000℃,预烧时间为150 min,烧成温度为1250℃,助溶剂硼酸的量为6wt%,制得的荧光体Sr_(0.975)Al_2Si_2O_8∶Eu_(0.025)~(2+)的发光强度最强,优化了合成条件。  相似文献   

19.
The corrosion properties of several borosilicate nuclear waste glasses exposed to aqueous environments have been investigated using a combination of Rutherford backscattering (RBS) depth profiling and solution analysis. Using the technique of RBS, the concentration of individual elements in the glass can be quantitatively profiled within a 1–2 μm surface layer. All of the glass surfaces were corroded in distilled water at 90°C for times ranging from 0–28 days. The evolution and composition of the altered layer that formed on the glass surface was of particular interest, since this layer can be crucial in determining whether or not the remainder of the glass undergoes further rapid corrosion. Within the altered surface layer produced by the corrosion process, there was an enhancement in the concentrations of U, Ti, Sr, Nd, Gd, and Ca and a depletion of Na, Si, Cs, (and probably B) relative to the concentrations present in the bulk glass. The U concentration, for example, was often 3–4 times greater in the altered surface layer than in the bulk. The layer apparently forms due to a local reaction that results in the formation of insoluble complexes on the glass surface. A simple model of the corrosion process has been used to identify the most likely insoluble metal complex for each metal present in excess in the alteration layer. The mechanical and chemical stability of this layer are also discussed.  相似文献   

20.
Abstract

Four macrocyclic liquid crystalline ligands derived from 1,8 dihydroxy ethyl 1,3,6,8,10,13 hexa aza cyclotetradecane(DHAT) and trans-4-n-alkoxy cinnamoyl chloride have been synthesised and their metal complexes using Cu(II),Ni(II),Pb(II), V(V) and U(VI) metal ions have been isolated. The ligands and their metal complexes were characterised by elemental analysis, FTIR,NMR,X-Ray and DSC studies. Polarising microscope was used to identify mesomorphic textures of the ligands and the complexes.

The transition temperature and mesophase textures of the ligands and complexes have been compared. The effect of presence of different metal ions on mesomorphic properties has been discussed.  相似文献   

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