本文選題：硫酸鉍堿金屬復(fù)鹽　切入點：固相法　出處：《上海工程技術(shù)大學(xué)》2015年碩士論文

【摘要】：探索新晶體材料是晶體領(lǐng)域研究中非常重要的一部分,也是促進新能源研發(fā)和實踐工作的必然趨勢。在眾多晶體材料中,硫酸鹽晶體是非常重要的一族。本論文采用中熱固相法合成出了三種新型硫酸鉍堿金屬復(fù)鹽晶體:Na Bi(SO4)2、KBi(SO4)2和Rb Bi(SO4)2,另外,采用水熱合成法成功制得新型異雙金屬混合酸根復(fù)鹽晶體Bi Cu2(Te O3)(SO4)(OH)3。晶體衍射數(shù)據(jù)都是在Bruker APEX-II CCD X-射線單晶衍射儀上收集的,運用SHELX-2013軟件以直接法解析得到晶體結(jié)構(gòu)。采用循環(huán)伏安法、交流阻抗法、充放電法來測試硫酸鉍堿金屬復(fù)鹽的電化學(xué)性能,還采用了傅立葉紅外光譜儀、紫外可見近紅外光譜儀對它們的性質(zhì)進行了表征和分析。本論文的主要研究內(nèi)容如下:1.Na Bi(SO4)2晶體以單斜空間群P21/c結(jié)晶,晶胞參數(shù):a=9.4340(18)?,b=7.0536(13)?,c=9.4489(18)?,β=95.839(3)°,Z=4。沿著[100]方向其晶體結(jié)構(gòu)是由無數(shù)個SO4四面體和Bi O8雙帽三棱柱連接構(gòu)成的二維[Bi(SO4)2]-層狀結(jié)構(gòu),Na+位于層與層之間。其中,每一個SO4四面體周圍環(huán)繞著四個Bi O8雙帽三棱柱,SO42-中的一個O同時連接兩個Bi原子,其余三個O原子單獨各自連接一個Bi原子。2.KBi(SO4)2晶體以單斜空間群C2/c結(jié)晶,晶胞參數(shù):a=13.052(2)?,b=5.3577(10)?,c=9.4127(17)?,β=102.031(3)°,Z=4;Rb Bi(SO4)2晶體同樣以單斜空間群C2/c結(jié)晶,晶胞參數(shù):a=13.501(5)?,b=5.3688(19)?,c=9.467(3)?,β=102.697(6)°,Z=4。它們的結(jié)構(gòu)可以描述為:沿著[100]方向相鄰的Bi O8四方反棱柱通過兩個SO4四面體連接形成無限的一維[Bi(SO3)2]3+鏈,平行的鏈與鏈之間通過SO4中的O3連接,在[001]方向形成二維的[Bi(SO4)2]-層狀結(jié)構(gòu),層與層之間由K+或Rb+隔開。拉曼和紅外光譜很好的證實了晶體結(jié)構(gòu)中存在的S-O振動、O-Bi-O以及晶格振動。紫外可見漫反射光譜測得它們的禁帶寬度分別為4.46e V、4.18 e V、4.15 e V。3.Bi Cu2(Te O3)(SO4)(OH)3晶體以單斜空間群P21/n結(jié)晶,晶胞參數(shù):a=9.5513(15)?,b=6.3022(10)?,c=13.955(2)?,Z=4,其晶體結(jié)構(gòu)是由兩種Cu O6八面體形成的二維層狀結(jié)構(gòu)[Cu3O10]14-與扭曲Bi O帽三棱柱,Te O3三角錐,SO4四面體連接而形成的三維隧道框架結(jié)構(gòu)。拉曼和紅外光譜很好的證實了晶體結(jié)構(gòu)中存在的Te O32-、SO42-、OH-等基團。紫外可見漫反射光譜測得化合物的禁帶寬度為3.85 e V。4.論文首次嘗試把硫酸鉍堿金屬復(fù)鹽作為電極材料。高頻區(qū)的交流阻抗圖表明硫酸鉍堿金屬復(fù)鹽作為電極材料是合適的。在6 M KOH溶液中掃描速率為5 m V/s下,Na Bi(SO4)2,KBi(SO4)2,Rb Bi(SO4)2的比電容分別為260,338,231 F/g。
[Abstract]:Exploring new crystal materials is a very important part of the research in crystal field, and is also an inevitable trend to promote the development and practice of new energy. Sulfate crystals are very important. In this paper, three new bismuth sulfate base metal double salt crystals of bismuth sulfate have been synthesized by medium thermal solid state method. A new type of double salt crystal Bi Cu2(Te O _ 3O _ 3O _ 4 so _ 4 O _ H _ 3 was successfully synthesized by hydrothermal synthesis. The diffraction data were collected on Bruker APEX-II CCD X-ray single crystal diffractometer. The crystal structure was obtained by direct analysis with SHELX-2013 software. The electrochemical properties of bismuth sulfate base metal compound salt were measured by cyclic voltammetry, AC impedance method and charge-discharge method, and Fourier transform infrared spectroscopy (FTIR) was used. Their properties were characterized and analyzed by UV-Vis near infrared spectrometer. The main contents of this thesis are as follows: 1. The crystal of Na Bi(SO4)2 is crystallized in monoclinic space group P21 / c. BX 7.0536? 9. 4489? The crystal structure is composed of numerous SO4 tetrahedrons and Bi O 8 double cap triangulated prisms. The two dimensional [Bi(SO4)2] -layered structure Na is located between layers. Each SO4 tetrahedron is surrounded by one of the four BiO8 double cap triprism columns so 42- and one of the other three O atoms is connected with two Bi atoms at the same time. The other three O atoms are individually connected to one Bi atom. 2. The crystal is crystallized in a monoclinic space group C _ 2 / P _ c, and the cell parameter is: a ~ (13. 0522)? 5. 3577? 10? 9. 4127? The crystal of Rb Bi(SO4)2 is also crystallized in monoclinic space group C _ 2 / c, the unit cell parameter is 1: a ~ (13.501)? 5. 3688? 9. 467? Their structures can be described as follows: bi O 8 tetragonal antiprism in the direction of [100] is joined by two SO4 tetrahedrons to form an infinite one dimensional [Bi(SO3)2] 3 chain, and parallel chains and chains are connected by O 3 in SO4. Forming a two-dimensional [Bi(SO4)2] -layered structure in the [001] direction, The layers are separated by K or RB. Raman and infrared spectra well confirm the existence of S-O vibration, O-Bi-O and lattice vibration in crystal structure. The band gap is 4.46 e V ~ (4) ~ (18) e V ~ (15) e measured by UV-Vis diffuse reflectance spectroscopy, respectively. V.3.Bi Cu2(Te O3)(SO4)(OH)3 crystals are crystallized in monoclinic space group P21 / n, Unit cell parameter: 9. 5513? 6. 3022? 10? C. C. 13.955? Its crystal structure is a three-dimensional tunneling frame structure formed by two kinds of CuO6 octahedron [Cu3O10] 14- and the twisted Bi O cap triangulated cone so 4 tetrahedron. Raman and infrared spectra show that the structure is very good. TeO32-OSO42-OH- groups were found in the crystal structure. The band gap of the compound was 3.85 e V. 4 measured by UV-Vis diffuse reflectance spectroscopy. The bismuth sulfate base metal compound was first used as electrode material in this paper. Ac impedance diagram of high frequency region. It is suitable to use bismuth sulfate alkali metal double salt as electrode material. The specific capacitance of Na ~ (2 +) ~ (so _ (4)) _ (2) K _ (B) _ (so _ (4)) ~ (2) R _ (b) Bi(SO4)2 is 260338231 F / g at a scanning rate of 5 MV / s in 6 M KOH solution.
【學(xué)位授予單位】：上海工程技術(shù)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：TQ135.32

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