本文選題：氟化亞鐵 + 碳化鐵��； 參考：《浙江工業(yè)大學(xué)》2017年碩士論文

【摘要】：鐵基化合物納米材料因其獨(dú)特的磁性能、電化學(xué)性能和良好的生物相容性,被廣泛應(yīng)用于電極材料、藥物輸送、磁共振成像與生物分離等領(lǐng)域。其中,氟化亞鐵納米顆粒是常用的反鐵磁性材料,碳化鐵納米顆粒是一種典型的鐵磁性納米材料。制備這兩種納米材料并研究其各方面性能對(duì)于理解鐵基化合物納米材料具有重要作用。納米材料的物理化學(xué)性能與其顆粒的形貌、尺寸有著密切的關(guān)系。因此,可控制備具有特殊結(jié)構(gòu)的單分散鐵基化合物納米材料并研究其結(jié)構(gòu)依賴的性能成為近幾年的熱點(diǎn)。液相熱分解法能通過(guò)控制形核、生長(zhǎng)過(guò)程調(diào)控納米材料的形貌,是目前制備單分散納米材料常用手段之一。因此,本文采用液相熱分解法制備氟化亞鐵、碳化鐵兩種納米材料。本論文旨在通過(guò)合理的技術(shù)路線設(shè)計(jì),合成形貌結(jié)構(gòu)新穎的氟化亞鐵和碳化鐵納米材料,并研究其在磁共振成像與電池方面的應(yīng)用。懫用X射線衍射(XRD)、透射電子顯微鏡(TEM)、X射線光電子能譜(XPS)、能譜儀(EDS)、等離子體電感耦合-原子發(fā)射光譜(ICP-AES)、磁共振成像(MRI)、循環(huán)伏安(CV)、電化學(xué)阻抗(EIS)等測(cè)試手段對(duì)合成的材料的結(jié)構(gòu)、形貌、性能進(jìn)行研究。本文的具體研究?jī)?nèi)容如下:(1)采用液相熱分解法制備得到了尺寸形貌可控的FeF_2納米顆粒。以乙酰丙酮鐵為前驅(qū)體,氟化銨為反應(yīng)物,油胺同時(shí)作為溶劑、表面活性劑與還原劑,在惰性氣體保護(hù)下調(diào)節(jié)反應(yīng)時(shí)間與溫度,制備得到尺寸為100-200 nm的FeF_2納米立方團(tuán)簇。其中,氟離子在體系中充當(dāng)交聯(lián)劑。在反應(yīng)體系中加入適量油酸,可得到粒徑為十幾納米大小的FeF_2納米顆粒。作為T(mén)_1加權(quán)磁共振成像(MRI)造影劑,粒徑為100 nm的FeF_2納米顆粒表現(xiàn)出較好的成像效果,其縱向弛豫效能值為1.08 m M~(-1)s~(-1)。(2)研究了FeF_2納米團(tuán)簇作為鋰離子電池正極材料的性能,探討了碳材料的引入對(duì)其電池性能的影響。分別采用有機(jī)物混合燒結(jié)和石墨烯超聲物理吸附兩種手段對(duì)材料表面進(jìn)行碳層包覆。聚苯乙烯(PS)與FeF_2混合燒結(jié)成功在FeF_2表面形成碳層,提高了導(dǎo)電性和循環(huán)穩(wěn)定性,電荷轉(zhuǎn)移反應(yīng)電阻降為140Ω,并在30次循環(huán)后保有65%的初始放電容量。但由于高溫?zé)Y(jié)氧化鐵相的引入,FeF_2/C的初始放電容量降低為213 m Ah g~(-1),約為理論容量的37%(571 m Ah g~(-1))。超聲負(fù)載石墨烯使材料電荷轉(zhuǎn)移反應(yīng)電阻降為60Ω。FeF_2/G復(fù)合物的初始放電容量475 m Ah g~(-1),約為理論容量的83%。(3)采用鹵素離子誘導(dǎo)的液相熱分解法,以羰基鐵為前驅(qū)體,油胺為表面活性劑,十八胺為溶劑在合成bcc-Fe晶核的基礎(chǔ)上碳化,兩步法制備了Fe_2C(六方晶系、單斜晶系)和Fe_5C_2(單斜晶系)納米顆粒。鹵素離子的加入是碳化過(guò)程中調(diào)控Fe-C相的關(guān)鍵。Fe_2C可在碳化過(guò)程無(wú)鹵素參與下得到,其相轉(zhuǎn)化受熱力學(xué)控制,在260-300℃范圍內(nèi)得到的為六方晶系,310℃后轉(zhuǎn)化為單斜晶系。碳化過(guò)程中鹵素離子的引入使得Fe原子與C原子之間的結(jié)合力減小,故可得到Fe_5C_2。實(shí)驗(yàn)發(fā)現(xiàn),改變羰基鐵加入量、碳化時(shí)間、鹵素離子添加量對(duì)產(chǎn)物相結(jié)構(gòu)無(wú)顯著影響,但會(huì)部分改變產(chǎn)物形貌。對(duì)Fe_2C與Fe_5C_2兩種碳化鐵納米材料進(jìn)行T_2加權(quán)磁共振成像性能研究,發(fā)現(xiàn)其均表現(xiàn)出良好的成像效果,其橫向弛豫效能值分別為357 m M~(-1)s~(-1)和192 m M~(-1)s~(-1),均高于商用氧化鐵納米顆粒造影劑,是有前景的T_2磁共振成像造影劑。
[Abstract]:Iron based compound nanomaterials are widely used in the fields of electrode materials, drug delivery, magnetic resonance imaging and biological separation because of their unique magnetic properties, electrochemical properties and good biocompatibility. Among them, ferrous fluoride nanoparticles are commonly used antiferromagnetic materials, and iron carbide nanoparticles are a typical ferromagnetic nano material. It is important to prepare these two nanomaterials and study their properties for understanding the iron based compound nanomaterials. The physical and chemical properties of the nanomaterials are closely related to the morphology and size of the particles. Therefore, the mono dispersed iron based nanocomposites with special structures can be controlled and their structural dependence can be studied. Performance has become a hot spot in recent years. Liquid phase thermal decomposition (liquid-phase thermal decomposition) can control the morphology of nanomaterials by controlling the nucleation and growth process. Therefore, the liquid phase thermal decomposition method is used to prepare ferrous fluoride and two kinds of nanomaterials. The purpose of this paper is to establish a reasonable technical route. To synthesize the novel morphologies of ferrous fluoride and iron carbide nanomaterials, and to study their applications in magnetic resonance imaging and batteries. X ray diffraction (XRD), transmission electron microscopy (TEM), X ray photoelectron spectroscopy (XPS), energy dispersive spectroscopy (EDS), plasma inductively coupled atomic emission spectroscopy (ICP-AES), magnetic resonance imaging (MRI), and circulation Voltammetry (CV), electrochemical impedance (EIS) and other testing methods have been used to study the structure, morphology and properties of the synthesized materials. The specific contents of this paper are as follows: (1) the size and morphology controlled FeF_2 nanoparticles were prepared by the liquid phase thermal decomposition method. A FeF_2 nanocluster with a size of 100-200 nm was prepared by adjusting the reaction time and temperature under the protection of inert gas with the active agent and reducing agent. Among them, the fluorine ion acted as a crosslinker in the system. A suitable amount of oleic acid was added to the reaction system, and the size of FeF_2 nanoparticles with a size of more than ten nanometers was obtained. As a T_1 weighted magnetic resonance formation Like (MRI) contrast agent, FeF_2 nanoparticles with a particle size of 100 nm showed good imaging results, and their longitudinal relaxation efficiency was 1.08 m M~ (-1) s~ (-1). (2) the performance of FeF_2 nanoclusters as cathode materials for lithium ion batteries was studied. The effects of the introduction of carbon materials on their battery performance were investigated. Organic compound sintering and stone were used respectively. The surface of the material is coated with carbon layer by two means of ultrasonic physical adsorption. The mixed sintering of polystyrene (PS) and FeF_2 has successfully formed carbon layer on the surface of FeF_2. The conductivity and cyclic stability are improved, the charge transfer reaction resistance is reduced to 140 Omega, and the initial discharge capacity of 65% after 30 cycles is preserved. But due to the high temperature sintering of iron oxide phase The initial discharge capacity of FeF_2/C was reduced to 213 m Ah g~ (-1), about 37% of the theoretical capacity (571 m Ah g~ (-1)). The ultrasonic load graphene made the charge transfer reaction resistance of the material to the initial discharge capacity of 60 Omega.FeF_2/G compound 475 m Ah (3), about the theoretical capacity (3) using halogen induced liquid thermal decomposition method. Carbonyl iron is a precursor, oleamine is a surfactant, eighteen amine is used as a solvent to carbonization on the basis of the synthesis of bcc-Fe nucleation. Fe_2C (six square crystal system, monoclinic system) and Fe_5C_2 (monoclinic) nanoparticles are prepared by two step method. The addition of halogen ions is the key to the regulation of Fe-C phase in carbonization process, which can be obtained by the participation of halogen free process in carbonization process. When the phase transformation is controlled by thermodynamics, the six square crystal system is obtained in the range of 260-300 C and converted to monoclinic system at 310 C. The introduction of halogen ions in the carbonization process reduces the binding force between the Fe atom and the C atom. Therefore, the Fe_5C_2. experiment can be found to change the amount of carbonyl iron, the carbonization time, and the addition of halogen ions to the products. The phase structure has no significant influence, but the morphology of the product is partly changed. The T_2 weighted magnetic resonance imaging properties of two kinds of Fe_2C and Fe_5C_2 nano materials are studied. It is found that both of them exhibit good imaging results, and their transverse relaxation efficiency values are 357 m M~ (-1) s~ (-1) and 192 m M~ (-1) s~, respectively, which are higher than those of commercial iron oxide nanoparticles. The shadow agent is a promising T_2 magnetic resonance imaging contrast agent.
【學(xué)位授予單位】：浙江工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：TB383.1;TQ138.11

【參考文獻(xiàn)】

相關(guān)期刊論文 前1條

1 孫圣男;魏超;朱贊贊;侯仰龍;Subbu S Venkatraman;徐h醬，

本文編號(hào)：1921936