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wjh522996

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自蔓延燃烧合成镍锌铁氧体及其机理研究
摘要
本文采用自蔓延高温合成(SHS)与自蔓延低温合成(LCS)方法对NiZn铁氧体进行了系统的研究。对采用自蔓延高温合成方法合成NiZn铁氧体中的热力学进行了理论分析;实验研究了ZnO含量、铁粉和NaClO4含量、压坯密度对SHS镍锌铁氧体样品性能的影响;初次采用Ni粉、NiCO3作为镍源SHS镍锌铁氧体。首次在SHS反应的坯料中添加各类氧化物,系统地对镍锌铁氧体的掺杂进行了研究。率先在我国开展磁场下自蔓延高温合成铁氧体的技术工作,对外加磁场条件下合成镍锌铁氧体进行了实验研究,主要针对磁场强度、磁场方向和燃烧波传播方向关系、以及不同燃烧阶段施加磁场对燃烧温度、样品性能的影响进行了系列研究。应纳米镍锌铁氧体发展趋势,对自蔓延低温合成镍锌铁氧体进行了研究,对柠檬酸与金属离子的摩尔配比、溶胶pH、引燃温度、烧结温度和燃料种类等影响因素进行了分析讨论。用红外测温仪测试了燃烧温度,应用XRD、EDS、SEM、VSM等对镍锌铁氧体的物相组成、显微结构及磁性能进行了表征,利用Jade软件对样品晶格常数、颗粒尺寸进行了分析。具体研究内容与研究结果如下:
首先应用热力学相关理论对SHS镍锌铁氧体反应过程的热力学进行了计算,得到不同配比下燃烧体系的绝热温度,根据合成可能发生反应的焓变和温度的关系推导出自蔓延高温合成镍锌铁氧体的合成途径,提出了自蔓延高温合成镍锌铁氧体的反应机制。
通过研究初始反应物中的ZnO含量对SHS镍锌铁氧体样品磁性能的影响,确定了具有较低的矫顽力、较高的比饱和磁化强度的Ni0.35Zn0.65Fe2O4作为自蔓延燃烧合成的目标产物,最佳合成工艺条件为:压坯密度为2.2g/cm3,Fe与Fe2O3比例为3:1,NaClO4含量为23.2%,合成得到Ni0.35Zn0.65Fe2O4的样品的矫顽力Hc为17Oe,比饱和磁化强度Ms最大可达68.1emu/g,初始磁导率为23.3;同时研究发现镍源对Ni0.35Zn0.65Fe2O4的性能有直接影响,采用Ni粉作为镍源也可以制备出与采用NiO性能相当的镍锌铁氧体样品。
在Ni0.35Zn0.65Fe2O4掺杂Bi2O3、Co2O3、PbO、MoO3和纳米SiO2的实验研究中,发现随着Bi2O3和PbO添加含量的增加,镍锌铁氧体晶体尺寸有长大的趋势;另外 PbO、MoO3和SiO2能有效提高镍锌铁氧体样品的烧结密度,磁导率也有所提高;添加纳米SiO2可达到晶粒细化的目的,铁氧体颗粒尺寸在1-2μm之间;当添加3%的SiO2时,初始磁导率提高10%。当添加1%的MoO3时,初始磁导率提高74.4%。
对外加电磁场下自蔓延高温合成Ni0.35Zn0.65Fe2O4研究结果表明:(1)磁场下燃烧合成镍锌铁氧体可以达到提高样品比饱和磁化强度的目的,本实验条件下约在在0.5T和1.1T附近样品的比饱和磁化强度普遍得到提高。在1.12T下合成Ni0.35Zn0.65Fe2O4的饱和磁化强度最大可达71.8emu/g,相比无磁场条件制备的样品提高5.4%。磁场强度使样品晶体长大,在场强为1.1T时,铁氧体由类球形变为多面体形状。1.12T反向磁场下自蔓延合成样品的初始磁导率达到32.2,比无磁场时提高38%。(2)通过在燃烧合成的不同阶段施加1.3T外磁场合成Ni0.35Zn0.65Fe2O4样品性能的研究表明:不同阶段下外加磁场使镍锌铁氧体的矫顽力都有所提高,比饱和磁化强度变化无明显趋势,磁场对自蔓延高温合成影响主要表现在自蔓延燃烧过程和燃烧产物冷却等两个阶段。初步建立了磁场下自蔓延燃烧合成过程中热传导的数学模型。
低温燃烧合成Ni0.35Zn0.65Fe2O4的最佳工艺条件为:在前躯体溶液pH值为7的条件下,取柠檬酸与金属阳离子的配比R为2:1,预烧温度400℃,烧结温度为1180℃时可以制备出性能优越的Ni0.35Zn0.65Fe2O4样品,矫顽力Hc为51.6Oe,比饱和磁化强度达70.2emu/g。除柠檬酸外,采用甘氨酸和尿素同样能制备出单相的Ni0.35Zn0.65Fe2O4样品。
Research on Synthesis and mechanism of NiZn Ferrite by
Self-Propagating Combustion Technology
Abstract
NiZn ferrite was synthesized with two different approaches respectively, namely self-propagating high-temperature synthesis (SHS) and self-propagating low temperature synthesis (LCS). In terms of SHS, thermodynamics of combustion synthesis are calculated. the influence of ZnO content,the iron content, green density, the Nickel source, as well as doped Bi2O3,Co2O3,PbO,SiO2 and MoO3 were investigated systematically NiZn ferrite were produced by SHS in a Magnetic field, which is one of the novelties of the study. The effects of magnetic field strength, change of magnetic direction, applied to the stage of combustion synthesis on the performance of sample were studied individual. In terms of LCS, molar ratio of citric acid to metal ions, sol pH, the influence of sintering temperature as well as preheating temperature were investigated, respectively. Reactions temperatures were obtained by and infrared radiation thermometer, The NiZn ferrite phase composition, microstructure and magnetic properties were also characterized with the help of XRD, EDS, SEM, VSM. The lattice parameter and the size of crystal were analysised by Jade5.0. These concrete works are the following:
By thermodynamic calculation based on thermodynamic principle, the adiabatic temperature of combustion synthesis Ni0.35Zn0.65Fe2O4 has been calculated when different mixture of iron, iron oxides, Zinc oxide, Niekel oxide and sodium perchlorate powders. The synthesis pathways of NiZn ferrite were induced according to the relationship of free enthalpies of reaction products vs temperature, and a mechanics corresponding to the self –propagating high temperature combustion mechanism of form Ni - Zn ferrite powders were proposed.
In the process of self-propagating high temperature synthesis of NiZn ferrite in normal air atmosphere,Ni0.35Zn0.65Fe2O4 were selected as the main prescriptions, with the low coercivity and high specific saturated magnetization. Ni0.35Zn0.65Fe2O4 reached the optimal performance when Fe:Fe2O3=3:1, odium perchlorate content was 23.1%, in which condition the saturated magnetization (Ms) was 68.1emu/g, coercivity was 17Oe, The initial permeability was 23.3. Ni0.35Zn0.65Fe2O4 synthesized by  Ni and NiO have better magnetic properties.
The effects of Bi2O3, Co2O3, PbO, MoO3 and SiO2-doping respectively on the microstructures and electromagnetic properties of Ni0.35Zn0.65Fe2O4 were investigated. The results show that Bi2O3 and PbO addition can promote the grain growth, MoO3 and SiO2 addition can increase the density of sintered product and the initial permeability of NiZn ferrites. the grain of Ni0.35Zn0.65Fe2O4 can decrease after SiO2 were doped, the size are about 1-2μm. the initial permeability of NiZn ferrites can increase 10% and 74.4% corresponding individually doped 1% SiO2 and MoO3.
This paper also systematically explores the effect of the electromagnetic field on ferrite by combustion synthesis. The high saturation magnetization Nickel-zinc ferrite can be improved by combustion synthesis in the optimum magnetic field strength of 0.5T or 1.1T. The specific saturation magnetization of products increased of 5.4% in a field of 1.12T compared those of 0T. The initial permeability of sample increased of 38% prepared in the field of 1.12T than those of 0T. When the magnetization is 1.1T, NiZn ferrite became polygonal crystal pronounced, which is due to the crystal growth. (2) The magnetic field of 1.3T applied to different stages of combustion process were studied, Hc of sample were increased when the applied magnetic field; the specific saturation magnetization were not change obviously trend. The magnetic field influence on the property of NiZn ferrite is mainly determined by the property of combustion pro and the cooling process of the product after combustion. The model of heat and mass transfer process during SHS under external magnetic field had been built.
Ni0.35Zn0.65Fe2O4 was synthesized by sol-gel self-propagating synthesis router. The best optimum technological conditions are the body solution pH=7.00, citric acid and metal ions of the material in a ration of 2:1, ignition temperature at 400℃ and sintering temperature at 1180℃, in which condition the specific saturated magnetization (Ms) was 70.2 emu/g, coercivity was 51.6Oe. Ni0.35Zn0.65Fe2O4 was synthesized by means of sol-gel auto-combustion synthesis method using other fule, such as glycine and urea.

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yjhorn

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★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★
wjh522996(金币+5,VIP+0):谢谢 11-14 10:12
wjh522996(金币+10,VIP+0):就这么多金币,大家分了,谢谢 11-14 10:24
修改了一下:Abstract
NiZn ferrite was synthesized with(换成BY) two different approaches respectively, namely(换成OR) self-propagating high-temperature synthesis (SHS) and self-propagating low temperature synthesis (LCS). In terms of SHS, thermodynamics of combustion synthesis are calculated. the influence of ZnO content,the iron content, green density, the Nickel source, as well as doped Bi2O3,Co2O3,PbO,SiO2 and MoO3 were(换成was) investigated systematically NiZn ferrite were produced by SHS in a Magnetic field, which is one of the novelties of the study. The effects of magnetic field strength, change of magnetic direction, applied to the stage of combustion synthesis on the performance of sample were studied individual(ly).
认识大家是缘分啊!
3楼2009-11-07 20:58:37
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phyweiw

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★ ★ ★ ★ ★
wjh522996(金币+5,VIP+0):谢谢,很感谢你的意见 11-7 20:07
太长了,没有时间看,
你的标题,建议用Study, 不用research
technology建议改成technique
2楼2009-11-07 20:05:20
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phyweiw

铁杆木虫 (著名写手)

楼主还给我金币了,谢谢,谢谢,不过就看了个标题,拿5个金币不好意思了。
干脆在看两句,这样就心安理得了,呵呵。

第一句话为什么不用更简洁的语言呢?你是摘要啊。
NiZn ferrite was synthesized using self-propagating high-temperature synthesis (SHS) and self-propagating low temperature synthesis (LCS), respectively.

第二句:Theoretical analyses of combustion synthesis were performed in terms of SHS.

不要再给我金币了,我比你多。
4楼2009-11-07 21:10:24
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goodtimega

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★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ...
wjh522996(金币+50,VIP+0):谢谢,给我的帮助 11-14 10:23
zap65535(金币+10,VIP+0):补发 12-22 01:33
Synthesis and Mechanism of NiZn Ferrite by Self-Propagating Combustion

Abstract
NiZn ferrite was synthesized with two different approaches, namely self-propagating high-temperature synthesis (SHS) and self-propagating low temperature synthesis (LCS), respectively. In terms of SHS, thermodynamics of combustion synthesis is calculated. The influence of ZnO content,the iron content, green density, the nickel source, as well as doped Bi2O3,Co2O3,PbO,SiO2 and MoO3 were investigated systematically. NiZn ferrite was produced by SHS under magnetic field, which is one of the novelties of the study. The effects of magnetic field strength, change of magnetic direction, application to the stage of combustion synthesis on the performance of sample were studied individual. In terms of LCS, molar ratio of citric acid to metal ions, sol pH, the influence of sintering temperature as well as preheating temperature were investigated. Reactions temperatures were obtained by and infrared radiation thermometer, The NiZn ferrite phase composition, microstructure and magnetic properties were also characterized with the help of XRD, EDS, SEM, VSM. The lattice parameter and the size of crystal were analyzed by Jade5.0. The concrete works are the following: By thermodynamic calculation based on thermodynamic principle, the adiabatic temperature of combustion synthesis Ni0.35Zn0.65Fe2O4 has been calculated when different mixture of iron, iron oxides, zinc oxide, niekel oxide and sodium perchlorate powders. The synthesis pathways of NiZn ferrite were induced according to the relationship of free enthalpies of reaction products vs. temperature, and a mechanics corresponding to the self–propagating high temperature combustion mechanism of form Ni - Zn ferrite powders was proposed.
In the process of self-propagating high temperature synthesis of NiZn ferrite in normal air atmosphere,Ni0.35Zn0.65Fe2O4 was selected as the main prescriptions, with the low coactivity and high specific saturated magnetization. Ni0.35Zn0.65Fe2O4 reached the optimal performance when Fe:Fe2O3=3:1, odium perchlorate content was 23.1%, in which condition the saturated magnetization (Ms) was 68.1emu/g, coercivity was 17Oe, The initial permeability was 23.3. Ni0.35Zn0.65Fe2O4 synthesized by  Ni and NiO has improved magnetic properties.
The effects of Bi2O3, Co2O3, PbO, MoO3 and SiO2-doping respectively on the microstructures and electromagnetic properties of Ni0.35Zn0.65Fe2O4 were investigated. The results show that Bi2O3 and PbO addition can promote the grain growth, MoO3 and SiO2 addition can increase the density of sintered product and the initial permeability of NiZn ferrites. The grain of Ni0.35Zn0.65Fe2O4 can decrease after SiO2 were doped, the size are about 1-2μm. The initial permeability of NiZn ferrites can increase by 10% and 74.4% corresponding individually doped 1% SiO2 and MoO3.
This paper also systematically explores the effect of the electromagnetic field on ferrite by combustion synthesis. The high saturation magnetization nickel-zinc ferrite can be improved by combustion synthesis in the optimum magnetic field strength of 0.5T or 1.1T. The specific saturation magnetization of products increased of 5.4% in a field of 1.12T compared those of 0T. The initial permeability of sample increased of 38% prepared in the field of 1.12T than those of 0T. When the magnetization is 1.1T, NiZn ferrite becomes polygonal crystal pronounced, which is due to the crystal growth. (2) The effect of magnetic field of 1.3T applied to different stages of combustion process was studied. While the Hc of sample was increased with the applied magnetic field, the specific saturation magnetization was not changed noticeably trend. The magnetic field influence on the property of NiZn ferrite is mainly determined by the property of combustion pro and the cooling process of the product after combustion. The model of heat and mass transfer process during SHS under external magnetic field had been built.
Ni0.35Zn0.65Fe2O4 was synthesized by sol-gel self-propagating synthesis router. The optimal technological conditions refer to a body solution pH=7.00, citric acid and metal ions of the material in a ratio of 2:1, ignition temperature at 400℃ and sintering temperature at 1180℃, in which condition the specific saturated magnetization (Ms) is 70.2 emu/g, coercivity is 51.6Oe. Ni0.35Zn0.65Fe2O4 was synthesized by means of sol-gel auto-combustion synthesis method using other fule, such as glycine and urea.
5楼2009-11-07 21:43:06
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