论文资料-铁钴镍基二元合金论文：铁钴镍基二元合金微纳米结构的控制合成、磁学.doc

薅蚆肄膂芄蒈羀膁莇蚄袆膀葿蒇螂艿腿蚂蚈芈芁蒅羇芇莃蚀羃芇薆蒃衿芆芅蝿螅芅莇薂肃芄蒀螇罿芃薂薀袅莂节螅螁罿莄薈蚇羈蒆螄肆羇芆薆羂羆莈袂袈羅蒁蚅螄羅薃蒈肃羄芃蚃罿肃莅蒆袄肂蒇蚁螀肁膇蒄蚆肀荿蚀肅聿蒂薂羁聿薄螈袇肈芃薁螃肇莆螆虿膆蒈蕿羈膅膈螄袄膄芀薇螀膃蒂螃螆膃薅蚆肄膂芄蒈羀膁莇蚄袆膀葿蒇螂艿腿蚂蚈芈芁蒅羇芇莃蚀羃芇薆蒃衿芆芅蝿螅芅莇薂肃芄蒀螇罿芃薂薀袅莂节螅螁罿莄薈蚇羈蒆螄肆羇芆薆羂羆莈袂袈羅蒁蚅螄羅薃蒈肃羄芃蚃罿肃莅蒆袄肂蒇蚁螀肁膇蒄蚆肀荿蚀肅聿蒂薂羁聿薄螈袇肈芃薁螃肇莆螆虿膆蒈蕿羈膅膈螄袄膄芀薇螀膃蒂螃螆膃薅蚆肄膂芄蒈羀膁莇蚄袆膀葿蒇螂艿腿蚂蚈芈芁蒅羇芇莃蚀羃芇薆蒃衿芆芅蝿螅芅莇薂肃芄蒀螇罿芃薂薀袅莂节螅螁罿莄薈蚇羈蒆螄肆羇芆薆羂羆莈袂袈羅蒁蚅螄羅薃蒈肃羄芃蚃罿肃莅蒆袄肂蒇蚁螀肁膇蒄蚆肀荿蚀肅聿蒂薂羁聿薄螈袇肈芃薁螃肇莆螆虿膆蒈蕿羈膅膈螄袄膄芀薇螀膃蒂螃螆膃薅蚆肄膂芄蒈羀膁莇蚄袆膀葿蒇螂艿腿蚂蚈芈芁蒅羇芇莃蚀羃芇薆蒃衿芆芅蝿螅芅莇薂肃芄蒀螇罿芃薂薀袅莂节螅螁罿莄薈蚇羈蒆螄肆羇芆薆羂羆莈袂袈羅蒁蚅螄羅薃蒈肃羄芃蚃罿肃莅蒆袄肂蒇蚁螀肁膇蒄蚆肀荿蚀肅聿蒂薂羁聿薄螈袇肈芃薁螃肇莆螆虿膆蒈蕿羈 铁钴镍基二元合金论文：铁钴镍基二元合金微纳米结构的控制合成、磁学及催化性能【中文摘要】磁性合金材料作为一类重要的功能材料,引起了科学家的广泛关注,并在很多领域得到广泛的应用,如:磁流体、催化、生物科技和生物医药、磁共振成像、数据存储、环境治理等领域。而纳米材料的性能常常受其尺寸、形貌和组成的影响,因此,可控制合成磁性微纳米材料与性能研究成为了化学和材料学研究的重要领域之一。本论文旨在发展不同的合成方法制备具有不同形貌、尺寸和组成的铁钴镍基二元合金微纳米材料,同时,对其形成机理、相关磁学性能和在对硝基苯酚【英文摘要】Magnetic alloys materials are very important functional materials, which have attracted extensive attention because of their special physical, chemical properties and their potential applications in ferrofluids, magnetic resonance imaging, biotechnology, biomedicine, data storage, catalytsis, and environmental remediation, etc., and which strongly depended on their size, morphology, composition, and structure etc. In this thesis, we focused on developing different methods to synthesize magnetic binary alloys micro-/nanostructures based on Fe, Co and Ni with different morphologies, sizes, and compositions. At the same time, their formation mechanism, magnetic properties, and catalytic applications in reduction of 4-Nitrophenol were studied. The main contents and major results are given as follows:1. Uniform-sized, monodisperse, and single crystalline 3-dimensional NiCo2 dendritic microstructures were successfully synthesized in high yield by a simple and facile solution phase route in presence of CTAB. By adjusting the experimental parameters NiCo alloys nanostructures with different morphologies, sizes, and compositions were controllable synthesized, at the same time, the formation mechanism was investigated. While NiCo2 alloys micro-structure with shapes of sphere-like and flower-like were prepared by hydrothermal and solvothermal methods, respectively. Magnetic measurements revealed that all of the NiCo2 alloys obtained are ferromagnetic at room temperature. The saturation magnetization value of the Ni33.8Co66.2 dendrites （163.55 emu/g） is lower than that of the Ni32.3Co67.7 spheres （212.29 emu/g） and Ni33.4Co66.6 flower-likes （195.79 emu/g）, but the Ni33.8Co66.2 dendritic structures exhibit an enhanced coercivity value. NiCo2 alloys with different shapes (Ni33.8Co66.2 dendrites, Ni33.4Co66.6 flower-likes and Ni32.3Co67.7 spheres) have been used as reusable heterogeneous catalysts to reduce 4-nitrophenol （4-NP） into 4-aminophenol （4-AP） by NaBH4. From the average reaction rate constants at three different temperatures, we determined the activation energy, the entropy of activation, and the pre-exponential factor for each shape of NiCo2 alloys. The kinetic data indicate that Ni33.8Co66.2 dendrites are catalytically more active than that of both the Ni33.4Co66.6 flower-likes and Ni32.3Co67.7 spheres probably due to its largest surface-to-volume ratio and surface areas.2. The Ni-based metals, such as Ni, and FeNi alloy nanostructures with different shapes were synthesized by solvothermal method in polyol system. The reaction parameters such as reaction time, the concentration of NaOH, temperature, solvent, and the initial concentration of metals ions that affected the morphology of FeNi alloys were investigated systematically. When we changed the type of solvents, the Ni nanostructures with chain-like were obtained, and the possible formation mechanism was also discussed. Magnetic data show that all of the Ni and FeNi2 alloys obtained are ferromagnetic at room temperature. The saturation magnetization value of the Fe34.8Ni65.2 spheres with size of ca. 300 nm （174.62 emu/g） is higher than that of the Fe34.1Ni65.9 spheres with size of ca. 230 nm （166.71 emu/g） and Fe33.5Ni66.5 spheres with size of ca. 170 nm （160.05 emu/g）, but the Fe33.5Ni66.5 spheres （ca. 170 nm） exhibit an enhanced coercivity value. The saturation magnetization value of the chain-like Ni nanostructures （68.3 emu/g） is lower than that of flower-like Ni nanostreutures （84.9 emu/g）, but all higher than that of the bulk nickel （55 emu/g）. Especially, the flower-like Ni nanostructures exhibit an enhanced coercivity value （ca. 204.81 Oe）. At last, the FeNi2 alloys with three different sizes were applied to reduce the 4-Nitrophenol to 4-Aminophenol by NaBH4 in aqueous solution, and the reaction rate constants were obtained. The kinetic data indicate that Fe33.5Ni66.5 nanospheres （ca. 170 nm） are catalytically more active than that of both the Fe34.1Ni65.9 nanospheres （ca. 230 nm） and Fe34.8Ni65.2 nanospheres （ca. 300 nm） probably attribute to its smallest size, which induces the largest surface-to-volume ratio and surface areas. The BET3. Crystalline FeCo alloys （Fe59Co41, Fe37Co63） nanoparticles in diameter of 6?12 nm were synthesized by reduction of FeCl3 with hydrazine under ultrasonic wave, which is a simple, low-cost, surfactant-free route, and may stimulate technological interests. The reaction parameters such as temperature, the total concentration of Fe3+ + Co2+, and the initial ratio of Fe3+/Co2+ that affected the FeCo sizes and morphologies were investigated systematically. As-synthesized Fe59Co41 nanocrystallite shows excellent soft magnetic behaviour with high saturation magnetization up to 216.2 emu/g that is comparable with that of bulk Fe and Fe60Co40 alloy, and could have applications in catalysis, biotechnology, and magnetic storage devices.4. The metals/r-graphene and alloys/r-graphene hybrid materials, such as Ni/r-graphene, Co/r-graphene, Cu/r-graphene, NiCo/r-graphene, FeCo/r-graphene, FeNi/r-graphene, CoCu/r-graphene and NiCu/r-graphene hybrid materials were successfully synthesized by a fiacle two steps method used hydrazine as reduction reagent. The samples were characterizated by SEM, TEM, HRTEM, XRD, EDX, and ICP, respectively, the results shown that the nanoparticles were uniform dispersed on the surface of the graphene sheets. The reaction parameters such as reaction time, the concentration of metals ions, the modified of graphene, and the added sequence of the materials that affected the formation of hybrid materials were investigated systematically, based on which possible formation mechanism for the hybrid materials was proposed. The room temperature magnetic properties were characterizated by SQUID （MPMS XL-7）, the metal or alloy/r-graphene hybrid materials exhibited an enhanced saturation magnetization or coercivity. At last, the reduction of 4-NP to 4-AP were carried out used five different materials as catalysts. The rate constants of the five catalysts is 5.8210-3 S-1（S1, Ni/r-graphene）, 4.6310-3 S-1（S2, Ni/r-graphene）, 4.9510-3 S-1（S3, Ni/r-graphene）, 2.6010-3 S-1（r-graphene）, 3.5010-3 S-1（Ni nanoparticles）, 4.1510-3 S-1（the mixture of Ni nanoparticles and r-graphene）, respectively. Here, the r-graphene shows a good catalytic property for this reduction reaction, which was needed further investigation.【关键词】铁钴镍基二元合金 微纳米结构 磁性材料 控制合成 催化应用 复合材料 石墨烯【英文关键词】Fe, Co and Ni-based binary alloy Micro-/Nanostructure Magnetic materials Controlled-synthesis Catalytic application Composite materials Graphene【目录】铁钴镍基二元合金微纳米结构的控制合成、磁学及催化性能摘要5-8Abstract8-10第一章 绪言13-261.1 引言13-171.1.1 液相还原法14-151.1.2 水热/溶剂热法15-161.1.3 超声化学合成法16-171.2 论文选题意义及论文设想17-181.2.1 论文选题目的及意义171.2.2 论文研究内容17-18参考文献18-26第二章 镍钴合金磁性微纳米合金材料的制备及其催化应用研究26-572.1 引言26-272.2 实验部分27-282.2.1 试剂与仪器272.2.2 样品制备27-282.2.3 样品表征282.3 结果与讨论28-412.3.1 NiCo_2枝茎样品的形貌和结构分析28-382.3.2 花状Ni_(33.4)Co_(66.6)合金结构的分析38-392.3.3 球状Ni_(32.3)Co_(67.7)合金结构的分析39-402.3.4 不同形貌的NiCo_2合金微结构的磁学性能40-412.4 不同形貌的镍钴合金在对硝基苯酚催化中的应用41-452.4.1 催化实验412.4.2 催化可行性分析以及催化过程的跟踪41-422.4.3 催化结果与讨论42-452.5 本章小结45-46参考文献46-57第三章 高饱和磁化强度的镍基金属材料的溶剂热合成及其催化性能研究57-813.1 引言57-583.2 实验部分58-593.2.1 试剂和仪器583.2.2 镍基金属的制备583.2.3 样品的表征58-593.2.4 催化性能593.3 结果与讨论59-723.3.1 FeNi 合金纳米结构的控制合成59-663.3.2 镍纳米结构的表征66-673.3.3 Fe-Ni 和Ni 纳米材料的磁学性能67-703.3.4 不同尺寸的Fe-Ni 合金的催化性能70-723.4 本章小结72-73参考文献73-81第四章 超声法合成高饱和磁化强度的铁钴合金纳米晶81-954.1 引言814.2 实验部分81-824.2.1 试剂和仪器81-824.2.2 Fe-Co 合金的制备824.2.3 样品的表征824.3 结果与讨论