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氧化鐵基納米棒(顆粒)的可控合成與磁性能研究

發(fā)布時(shí)間:2018-05-17 16:42

  本文選題:磁性材料 + 氧化鐵。 參考:《哈爾濱工業(yè)大學(xué)》2017年碩士論文


【摘要】:磁性納米材料作為功能納米材料的一個(gè)重要分支,由于其在納米級(jí)有趣的磁學(xué)性質(zhì)和潛在的應(yīng)用而受到了廣泛的關(guān)注和研究。根據(jù)矯頑力的大小,磁性材料可以分為硬磁材料和軟磁材料。磁性納米粒子具有許多不同于體相材料的特殊磁性質(zhì),例如,高矯頑力、超順磁性、低居里溫度等,這些性質(zhì)主要是由表面效應(yīng)和小尺寸效應(yīng)決定的。此外,磁性納米粒子的矯頑力和飽和磁化強(qiáng)度,不僅和納米粒子本身的晶體結(jié)構(gòu)有關(guān),還和它的尺寸,形貌,化學(xué)組成和分散性有關(guān)。納米氧化鐵是一種非常有前景的無(wú)機(jī)非金屬功能材料,具有無(wú)毒,抗腐蝕性能強(qiáng),儲(chǔ)存量豐富,多價(jià)態(tài)等特點(diǎn),并且由于其可接受的磁學(xué)性能和高度的穩(wěn)定性,能夠廣泛應(yīng)用于磁存儲(chǔ),磁記錄,電磁吸收,生物醫(yī)學(xué),超級(jí)電容器負(fù)極材料,傳感器,能源催化等領(lǐng)域。本論文中,我們首先以氯化鐵為前驅(qū)體,十六烷基三甲基溴化銨(CTAB)為表面活性劑,在120oC用水熱法合成了α-Fe_2O_3納米粒子和β-FeOOH納米粒子。借助場(chǎng)發(fā)射掃描電子顯微鏡(FESEM),電子衍射能譜(EDS),X射線衍射(XRD),震動(dòng)樣品磁強(qiáng)計(jì)(VSM)等表征手段,研究α-Fe_2O_3納米粒子和β-FeOOH納米粒子的形貌,結(jié)構(gòu)和磁性能。晶體的形貌和尺寸可以通過(guò)改變前驅(qū)體的濃度來(lái)控制,當(dāng)氯化鐵濃度比較低時(shí),合成出了菱形、球形和立方體的α-Fe_2O_3納米粒子;當(dāng)氯化鐵濃度較高時(shí),得到了不同縱橫比的β-FeOOH納米棒。將β-FeOOH納米棒在不同溫度下煅燒,得到了不同尺寸的α-Fe_2O_3納米棒,并對(duì)其磁性進(jìn)行表征,探索了煅燒溫度對(duì)相轉(zhuǎn)變的影響。最后,將得到的α-Fe_2O_3納米棒在不同溫度下用H_2還原,得到了Fe,Fe_3O_4和Fe_2O_3@Fe_3O_4復(fù)合物。其次,以氯化鐵和氯化鈷為前驅(qū)體,以CTAB為表面活性劑,以尿素為絡(luò)合劑,合成出了具有高飽和磁化強(qiáng)度和高矯頑力的CoFe_2O_4球形納米粒子,研究了絡(luò)合劑,前驅(qū)體濃度,反應(yīng)溫度,反應(yīng)時(shí)間,超聲,外加磁場(chǎng)等條件對(duì)納米粒子尺寸形貌和磁性能的影響,通過(guò)SEM,EDS,XRD,VSM對(duì)產(chǎn)物進(jìn)行表征。最終,我們得出,在氯化鐵濃度0.04 M,氯化鈷濃度為0.02 M,尿素濃度為0.6 M,反應(yīng)溫度為150oC,反應(yīng)時(shí)間為12 h,超聲時(shí)間為0.5 h的最優(yōu)條件下,得到了粒徑尺寸為60 nm的球形CoFe_2O_4納米粒子,其矯頑力為3.57 kOe,飽和磁化強(qiáng)度34.743 emu·g-1。
[Abstract]:As an important branch of functional nanomaterials, magnetic nanomaterials have received extensive attention and research due to their interesting magnetic properties and potential applications. According to the size of coercivity, magnetic materials can be divided into hard magnetic materials and soft magnetic materials. Magnetic nanoparticles have many special magnetic properties, such as high coercivity, superparamagnetism and low Curie temperature, which are mainly determined by surface effect and small size effect. In addition, the coercivity and saturation magnetization of magnetic nanoparticles are not only related to their crystal structure, but also to their size, morphology, chemical composition and dispersion. Nanocrystalline iron oxide is a promising inorganic nonmetallic functional material with the advantages of non-toxic, strong corrosion resistance, abundant storage, multivalent state, etc., and due to its acceptable magnetic properties and high stability, Can be widely used in magnetic storage, magnetic recording, electromagnetic absorption, biomedical, supercapacitor anode materials, sensors, energy catalysis and other fields. In this thesis, 偽 -Fe _ 2O _ 3 nanoparticles and 尾 -FeOOH nanoparticles were synthesized by hydrothermal method using ferric chloride as precursor and cetyltrimethylammonium bromide (CTAB) as surfactant in 120oC. The morphology, structure and magnetic properties of 偽 -Fe _ 2O _ 3 nanoparticles and 尾 -FeOOH nanoparticles were studied by means of field emission scanning electron microscopy (SEM), electron diffraction spectrum (EDS), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). The morphology and size of the crystal can be controlled by changing the concentration of the precursor. When the concentration of ferric chloride is low, the rhombic, spherical and cubic 偽 -Fe _ 2O _ 3 nanoparticles are synthesized; when the concentration of ferric chloride is high, the 偽 -Fe _ 2O _ 3 nanoparticles are synthesized. 尾 -FeOOH nanorods with different aspect ratios were obtained. 偽 -Fe2O3 nanorods with different sizes were obtained by calcining 尾 -FeOOH nanorods at different temperatures. The magnetic properties of 偽 -Fe2O3 nanorods were characterized, and the effect of calcination temperature on phase transition was explored. Finally, the 偽 -Fe2O3 nanorods were reduced by H _ 2 at different temperatures, and the Fe-Fe _ 3O _ 4 and Fe_2O_3@Fe_3O_4 complexes were obtained. Secondly, CoFe_2O_4 spherical nanoparticles with high saturation magnetization and high coercivity were synthesized by using ferric chloride and cobalt chloride as precursors, CTAB as surfactant and urea as complexing agent. The effects of reaction temperature, reaction time, ultrasonic and applied magnetic field on the size, morphology and magnetic properties of the nanoparticles were investigated. Finally, under the optimum conditions of ferric chloride 0.04 M, cobalt chloride 0.02 M, urea 0.6 M, reaction temperature 150oC, reaction time 12 h, ultrasonic time 0.5 h, the spherical CoFe_2O_4 nanoparticles with particle size of 60 nm were obtained. The coercivity is 3.57 KOe and the saturation magnetization is 34.743 emu g-1.
【學(xué)位授予單位】:哈爾濱工業(yè)大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:TB34;TB383.1

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