本文選題：溶液燃燒合成 + 納米材料��； 參考：《北京科技大學》2017年博士論文

【摘要】：納米鐵基材料具有獨特的電、磁、光、熱、化學等性能,在能源存儲與轉換、水處理、環(huán)境修復、高效催化、磁性介質等領域有著廣泛的應用前景�，F(xiàn)有納米鐵基材料的制備方法存在著工藝復雜、成本高、產率低等問題。溶液燃燒合成是近年來快速發(fā)展的一種制備納米材料的新型濕化學方法,具有簡便、快捷、成本低、產率高等諸多優(yōu)點。本論文將溶液燃燒合成應用于納米鐵基材料的制備,研究內容主要包括以下幾方面:(1)以硝酸鐵為鐵源和氧化劑、甘氨酸為燃料、葡萄糖為添加劑,采用一種基于溶液燃燒合成的新方法成功制備出網(wǎng)狀多孔α-F2O3納米片。該方法包含溶液燃燒合成、煅燒和熱處理三個簡單步驟。首先,溶液燃燒合成片狀前驅體,在前驅體中均勻分布著無定形氧化鐵和無定形碳;接著,在氬氣氣氛中將前驅體在500℃下煅燒0.5h,在煅燒產物中,尺寸為5～10nm的過渡相Fe3C納米顆粒形成,并且均勻地鑲嵌在片狀碳支持體上;隨后,在空氣氣氛中將鍛燒產物在500℃下熱處理0.5h,獲得網(wǎng)狀多孔α-Fe2O3納米片。在納米片中,光滑致密的骨架間均勻分布著大量～40nm的圓形單孔以及少量通孔,該網(wǎng)狀多孔α-Fe2O3納米片的比表面積達到71m2/g。提出了熱處理過程中該多孔納米片的形成機制即在熱處理過程中多孔納米片的形成過程主要包括目標相α-Fe2O3納米顆粒的生成、聚集以及燒結三個階段。(2)選取甘氨酸-硝酸鐵和葡萄糖-甘氨酸-硝酸鐵兩種燃燒體系合成氧化鐵前驅體,隨后在氫氣氣氛中將其還原,獲得不同顆粒尺寸的納米鐵粉。深入研究了燃氧比(φ)對溶液燃燒溫度、前驅體物相、比表面積和微觀形貌的影響以及還原溫度對還原產物物相、顆粒尺寸和磁性能的影響。在甘氨酸-硝酸鐵燃燒體系中,溶液(φ=1)燃燒溫度為574℃,前期體(φ=1)為α-Fe2O3和γ-Fe2O3的混合物,具有高的比表面積(50.8m2/g)和高的孔隙率,其完全還原溫度為400℃。該前驅體在400℃還原2h獲得的納米鐵粉的顆粒尺寸為～60nm,飽和磁化強度為201.7emu/g,矯頑力為380.6Oe。在葡萄糖-甘氨酸-硝酸鐵燃燒體系中,葡萄的加入改變了燃燒反應條件,使反應變得溫和可控。該體系的溶液燃燒溫度為383℃,合成的前驅體為α-Fe2O3,具有更高的比表面積(75m2/g)和更高的反應活性,其完全還原溫度為275℃。在275℃下還原2h獲得的納米鐵粉顆粒的尺寸為20～50nm,飽和磁化強度為196.3emu/g,矯頑力為611.4Oe。(3)以硝酸鐵為鐵源和氧化劑、甘氨酸為燃料、葡萄糖為碳源,采用一種基于溶液燃燒合成的新方法成功制備出片狀納米鐵碳復合材料。該方法包含溶液燃燒合成、氫還原兩個簡單步驟。首先,溶液燃燒合成片狀前驅體,在前驅體中均勻分布著無定形氧化鐵和無定形碳;隨后,在氫氣氣氛中將前驅體在400℃還原,獲得片狀納米鐵碳復合材料。該復合材料由納米鐵顆粒和無定形碳組成,并且納米鐵顆粒均勻地鑲嵌于片狀碳支持體上。400℃還原2h得到鐵碳復合材料的納米鐵顆粒尺寸為～20nm,碳含量為23.2wt.%,比表面積為274.9m2/g,飽和磁化強度為145.7emu/g,矯頑力428.1Oe。(4)采用常壓燒結和SPS燒結兩種方法實現(xiàn)甘氨酸-硝酸鐵燃燒體系所制備納米鐵粉的致密化。深入研究了燒結溫度對燒結純鐵的致密度、顯微組織、力學性能以及磁性能的影響規(guī)律。納米鐵粉具有高的燒結活性,800℃常壓燒結純鐵的致密度達到97.3%。900～1300℃常壓燒結純鐵具有高的磁飽和強度、高的硬度和抗拉強度。600℃SPS燒結純鐵的致密度達到96.1%,并且具有高的硬度(HRC44.5)。
[Abstract]:Nanometer iron-based materials with unique electrical, magnetic, optical, thermal, chemical and other properties, in the energy storage and conversion, water treatment, environmental remediation, efficient catalysis, magnetic media and other fields have a wide application prospect. The traditional preparation method of nano iron material has complex process, high cost and low yield. Solution combustion synthesis is developing rapidly in recent years, the preparation of a new nano material wet chemical method is simple, fast, low cost, high yield and many other advantages. This paper will be applied to nano solution combustion synthesis of iron-based materials preparation, the main research contents include the following aspects: (1) the iron nitrate iron source and oxidant, glycine as a fuel additive, glucose, using a solution combustion method for synthesis of prepared porous reticular alpha -F2O3 nanosheets. Based on this method contains the solution combustion synthesis, calcination and heat treatment three Simple steps. Firstly, solution combustion synthesis of lamellar precursor in precursor dispersed amorphous iron oxide and amorphous carbon; then, in argon atmosphere, calcination precursor body at a temperature below 500 DEG 0.5h in the calcined products, the formation of size 5 ~ 10nm phase transition of Fe3C nanoparticles, and uniformly dispersed in the sheet carbon support; then, in the atmosphere, calcination product at 500 DEG C for heat treatment of 0.5h, obtaining reticulated porous -Fe2O3 nanosheets. Alpha in nano film, smooth and compact framework of uniformly distributed circular single hole large ~ 40nm and a small hole, the reticulated porous alpha -Fe2O3 nanosheets the specific surface area reached 71m2/g. proposed the formation mechanism of the nano porous film in the heat treatment process of the porous heat treatment process in nano sheet forming process includes the goal of alpha phase -Fe2O3 nanoparticles, aggregation and sintering three Stage. (2) selection of glycine iron nitrate and glucose glycine nitrate combustion synthesis system of iron two iron oxide precursor, then the reduction in hydrogen atmosphere, different particle size of nanometer iron powder was studied. The burning oxygen ratio (PHI) solution of combustion temperature, precursor phase, influence the surface area and micro morphology and reduction temperature on the reduction phase of the product, the influence of size and magnetic properties of particles. In the glycine nitrate combustion system of iron in solution (=1) combustion temperature is 574 DEG C, the body (phi =1) is a mixture of alpha -Fe2O3 and gamma -Fe2O3, has high ratio the surface area (50.8m2/g) and high porosity, the reduction temperature of 400 DEG. The particle size of the precursor obtained by reduction of 2H nanometer iron powder at the temperature of 400 DEG C ~ 60NM, saturation magnetization is 201.7emu/g, coercivity of 380.6Oe. in glucose glycine nitrate combustion system of iron in Portugal Also changed with the addition of the combustion reaction conditions, the reaction is mild and controllable. The solution becomes the combustion temperature is 383 DEG C, the synthesized precursor is alpha -Fe2O3, has a higher surface area (75m2/g) and higher reactivity, the complete reduction of the temperature of 275 DEG. Reduction of nanometer iron powder particles 2H at 275 DEG C to the size of 20 ~ 50nm, saturation magnetization is 196.3emu/g, coercivity of 611.4Oe. (3) with iron nitrate as iron source and oxidant, glycine as fuel, glucose as carbon source, using a solution combustion method for synthesis of prepared nano iron carbon composite materials based on the method includes solution combustion synthesis, hydrogen reduction of two simple steps. Firstly, solution combustion synthesis of lamellar precursor in precursor dispersed amorphous iron oxide and amorphous carbon; then, the precursor reduction in hydrogen atmosphere in 400 DEG C, get Nano iron carbon composite materials. The composite material is composed of nano iron particles and amorphous carbon, and iron nano particles are uniformly embedded in the sheet carbon support.400 C 2H reduction iron particle size of nano iron carbon composite materials for ~ 20nm, the carbon content is 23.2wt.%, the specific surface area is 274.9m2/g, saturation magnetization the strength of 145.7emu/g, the coercivity of 428.1Oe. (4) by atmospheric pressure sintering and sintering of SPS two kinds of methods to achieve the glycine nitrate combustion system for densification of iron nano iron powder was studied. The sintering temperature on density of sintered iron, microstructure, mechanical properties and the influence of the magnetic properties of nanometer iron powder has. High sintering activity, 800 DEG C atmospheric density of sintered iron reaches to 1300 DEG 97.3%.900 atmospheric pressure sintered iron with high magnetic saturation strength, high hardness and tensile strength of.600 C SPS density of sintered iron To 96.1%, and have high hardness (HRC44.5).

【學位授予單位】：北京科技大學
【學位級別】：博士
【學位授予年份】：2017
【分類號】：TB383.1

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