空心微珠复合吸波材料的研究
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摘要
吸波材料在军用及民用领域有着广泛的应用,已经成为各国军事装备隐身和民用防电磁辐射等技术领域研究的热点。在众多的吸波材料中,铁氧体和金属粉末吸收剂由于具有较好的性能和较低的成本往往是其中的主要吸波成分。但是铁氧体和金属粉末都有一个致命的缺点就是密度太大,不利于制备出质量轻的吸波材料。为解决这一难题,本文在前人研究的基础上设计出以火电厂粉煤灰空心微珠为基核,用化学镀和溶胶凝胶法制备空心微珠复合涂层颗粒吸收剂,并对化学镀和溶胶-凝胶法制备空心微珠涂层颗粒的制备工艺进行系统研究。
首次以AgNO3代替昂贵的PdCl2作催化剂并简化前处理步骤在空心微珠表面化学镀Ni-P和Ni-Co-P合金镀层,并对该工艺过程进行系统研究,确定了最佳制备工艺。
研究了溶胶-凝胶法制备钡铁氧体超细粉末、稀土(钇、钕、铕等)搀杂钡铁氧体超细粉末的各种工艺条件(溶胶组成、溶液浓度、络合剂配比、热处理制度及稀土搀杂量等)对铁氧体粉末物相结构、形貌及电磁性能影响的规律性。
首次用溶胶-凝胶法在空心微珠表面制备钡铁氧体包覆层,并用差热-热重分析(DTA-TG)、X射线衍射仪(XRD)、能谱仪(EDX)、扫描电镜(SEM)、X射线光电子能谱仪(XPS)、振动样品磁强计(VSM)和矢量网络分析仪对其进行了分析表征。
本文研究的成果和结论如下:
(1)将粉体化学镀的前处理步骤进行简化,省掉敏化步骤,并利用相对价廉的AgNO3代替贵金属PdCl2做催化剂,将催化剂的还原与化学镀中Ni2+的还原步骤合并为一步,在空心微珠表面化学镀Ni-P,Ni-Co-P合金镀层。VSM分析表明镍磷镀层的比饱和磁化强度为2.96emu/g,矫顽力为1807.2A/m;镍钴磷非晶态合金层的比饱和磁化强度达27.36emu/g,矫顽力为2059.5A/m,经400℃热处理后镀层结晶化,其比饱和磁化强度下降到2.08emu/g,矫顽力提高到15620.8A/m。空心微珠表面化学镀的机理为:通过碱洗步骤强化了空心微珠表面羟基化,从而提高了微珠表面吸附Ag(NH3)2+络离子的能力;Ag(NH3)2+离子通过氢键与微珠表面Al2O3和SiO2相结合,然后在镀液中被H2PO2-还原成金属银,为后续的化学镀提供催化活性中心。
(2)空心微珠表面化学镀Ni-P镀层过程中镀液的组成及试镀工艺条件对化学镀过程有较大影响。镀液中初始Ni2+浓度增加,反应速度并不随Ni2+浓度增大而加快,反应后剩余Ni2+浓度随初始Ni2+浓度增加而增大;还原剂次亚磷酸钠的浓度越大,反
应速度越快,反应后剩余金属离子浓度随次亚磷酸钠浓度增大而呈下降趋势;[Ni2+]/[柠檬酸根离子]的摩尔比越大亦即柠檬酸根离子浓度越低,反应速度越慢,反应后剩余金属离子浓度降低;用氨水调PH值时,当PH值少于9时,随着pH值增大,反应速度加快,当PH值大于9时,随pH值增大反应速度减慢;用氢氧化钠调节pH值,反应速度基本随pH值增加而增大,即pH值越大,反应速度越快;温度升高,反应速度加快;装载量越大,反应速度越快。
(3)空心微珠表面化学镀Ni-Co-P过程中,主盐中 Ni2+ 浓度增大,反应速度加快,突变时间缩短,总反应时间也缩短。当/(+)摩尔比大于0.4时,反应速度变化不大;次亚磷酸钠浓度的增大反应速度加快,当次亚磷酸钠的浓度大于0.3mol/l 时,反应突变时间已经变化不大,说明当次亚磷酸钠浓度与主盐的浓度比大于2:1时,反应速度达到最大,再增加次亚磷酸钠的浓度对镀速影响很小;缓冲剂硼酸对反应速度的影响较小,但存在最佳值0.5mol/l;采用柠檬酸钠和酒石酸钾钠复合作络合剂,在总浓度不变的情况下(络合剂总浓度为0.2mol/l),络合剂柠檬酸钠浓度越大,反应速度越快。但当柠檬酸钠浓度大于0.05mol/l时,增加柠檬酸钠浓度反应速度变化不大;用氨水调pH值时,当pH值小于8.5时,随着pH值增大,反应速度加快。当pH值大于9.5时,随pH值增大,反应速度急剧变缓,这主要由于氨水中的NH3对金属离子的络合作用降低了金属离子的浓度。用氢氧化钠调pH值,反应速度明显快于用氨水调pH值,并且随pH值增大,反应速度有加快的趋势。但是当pH值增大到10.5时,反应速度又有变缓的趋势,这可能是由于pH值过高,镀液中[OH-]浓度过大,[OH-]对金属离子进行络合的结果。装载量越大,反应速度越快。温度越高,反应速度越快。
(4)溶胶凝胶法制备的BaFe12O19铁氧体的生成条件是450℃预热处理1h后经850℃热处理3h。850℃保温时间太短,钡铁氧体没有完全晶化;保温时间太长,容易引起晶粒的长大。在溶胶凝胶法制备钡铁氧体的过程中,预热处理是一个关键的步骤,经过预热处理可以保证前驱物能够完全转化为γ-Fe2O3避免生成α-Fe2O3中间产物,从而降低钡铁氧体的完全晶化温度。初始溶液的pH值为7时才能得到均匀稳定的溶胶, 经热处理后生成单一、均匀的M型钡铁氧体。Fe与Ba之比从10到12之间都能够形成单一、均匀的M型钡铁氧体。原料中柠檬酸与硝酸盐之比为1时,自燃烧过程最剧烈;柠檬酸比例越高,所得粉体的颗粒越小;溶胶初期加入聚乙二醇可以降低所得超细粉末的颗粒粒径。
(5)随着Y、Eu、Nd等稀土元素RE搀杂量的增大,主晶相为六角晶系磁铅石型钡铁氧体相结构的钡铁氧体逐渐出现比较明显的REFeO3的衍射峰,并伴随着REFeO3
的出现,也出现了很少量的α-Fe2O3。Y、Eu、Nd等稀土元素RE对钡铁氧体的搀杂使样品的比饱和磁化强度下降,比剩余磁化强度?
Microwave absorbing materials have been widely in stealth technology and in electro-magnetic compatibility (EMC) technology, and they are researching hotspot in these technology field. In most of absorbers, the ferrite and metal powder are the main components because of good performance and low cost. But the defect of high density is not benefit for the preparation of light absorber. In response to the need for high performance absorber, in this paper, the composite-coating absorbers with hollow cenosphere as nuclear are prepared by sol-gel and electroless plating technology.
The Electroless Ni-P and Ni-Co-P-coating processes is modified by replacing the conventional sensitization and activation steps with only using activation step with AgNO3 activator, and the optimal forming conditions is made certain.
The BaFe12O19 and BaRexFe12-xO19 (RE denote Y、Nd and Eu) ultrafine powders with M-type structure are synthesized by sol-gel technique. The effects of the composition of the gel, strength of solution, the amount of complexing agent, the different kinds of anions, the adding of dispersant, and the condition in heat treatment of the gel on crystal phase, morphology and magnetic properties of The BaFe12O19 and BaRexFe12-xO19 were investigated systematically to clarify the optimum forming conditions.
Thin films of Barium hexaferrite are prepared on fly ash cenpsphere particles by sol-gel using Fe(NO3)3·9H2O、Ba(NO3)2 and citric acid as raw materials. The prepared films are characterized by differential and thermogravimetric analysis (DTA-TG), X-ray diffraction analysis (XRD), scanning electron microscope (SEM), energy dispersive spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and vibrating sample magnetometer(VSM) and Vector Network Analyzer.
Some important results are concluded as follows:
(1) The Electroless Ni-P and Ni-Co-P-coated cenospheres is preparated by replacing the conventional sensitization and activation steps with only using activation step with AgNO3 activator. The magnetic properties of Ni-P coated cenospheres are δs (27.3emu/g) and Hc (1807.2A/m) , while those of Ni-Co-P coated cenospheres are δs (27.36emu/g) and Hc (2059.5A/m), and those of Ni-P coated cenospheres after heat treatment are δs (2.08
emu/g) and Hc (15620.8A/m). The electroless mechanism is following: the ability of absorbing Ag(NH3)2+ is improved by hydroxy on cenosphere surface after alkali solution liquid rinsing. Then in the coating bath, [Ag(NH3)2]+ are reduced to Ag by H2PO2- . The catalytic action of Ag act as a nucleation sites for subsequent Ni-P or Ni-Co-P deposition.
(2) In the process of Ni-P electroless plating, the velocity of reaction is not augmented, while the residual Ni2+ after reaction is increased with the increased concentration of Ni2+. The velocity of reaction is increased, while the residual Ni2+ after reaction is declined with the increased concentration of H2PO2-. The velocity of reaction is fell, while the residual Ni2+ after reaction is declined with the increased mol ratio of Ni2+/[C6H5O7]3-. When the pH is adjusted by NH3.H2O the velocity of reaction is increased with the increase of pH (pH<9.0) and the velocity of reaction is fell with the increase of pH (pH>9.0). But when the pH is adjusted by NaOH the velocity of reaction is increased with the increase of pH. And the velocity of reaction is increased with the increasing temperature and the increasing loading.
(3) In the process of Ni-Co-P electroless plating, the velocity of reaction is augmented with the increased concentration of Ni2+. While the mol ratio of /(+) is more then 0.4, the velocity of reaction only change a little with the increased concentration of Ni2+. The velocity of reaction is increased with the increased concentration of H2PO2-. But when the concentration of H2PO2- is more than 0.3mol/l, the velocity of reaction only change a little. There is a little effect of the concentration of H3BO3 on the velocity of reaction, 0.5mol/l is the optimal concentration. The velocity of reaction is increased with the
首次以AgNO3代替昂贵的PdCl2作催化剂并简化前处理步骤在空心微珠表面化学镀Ni-P和Ni-Co-P合金镀层,并对该工艺过程进行系统研究,确定了最佳制备工艺。
研究了溶胶-凝胶法制备钡铁氧体超细粉末、稀土(钇、钕、铕等)搀杂钡铁氧体超细粉末的各种工艺条件(溶胶组成、溶液浓度、络合剂配比、热处理制度及稀土搀杂量等)对铁氧体粉末物相结构、形貌及电磁性能影响的规律性。
首次用溶胶-凝胶法在空心微珠表面制备钡铁氧体包覆层,并用差热-热重分析(DTA-TG)、X射线衍射仪(XRD)、能谱仪(EDX)、扫描电镜(SEM)、X射线光电子能谱仪(XPS)、振动样品磁强计(VSM)和矢量网络分析仪对其进行了分析表征。
本文研究的成果和结论如下:
(1)将粉体化学镀的前处理步骤进行简化,省掉敏化步骤,并利用相对价廉的AgNO3代替贵金属PdCl2做催化剂,将催化剂的还原与化学镀中Ni2+的还原步骤合并为一步,在空心微珠表面化学镀Ni-P,Ni-Co-P合金镀层。VSM分析表明镍磷镀层的比饱和磁化强度为2.96emu/g,矫顽力为1807.2A/m;镍钴磷非晶态合金层的比饱和磁化强度达27.36emu/g,矫顽力为2059.5A/m,经400℃热处理后镀层结晶化,其比饱和磁化强度下降到2.08emu/g,矫顽力提高到15620.8A/m。空心微珠表面化学镀的机理为:通过碱洗步骤强化了空心微珠表面羟基化,从而提高了微珠表面吸附Ag(NH3)2+络离子的能力;Ag(NH3)2+离子通过氢键与微珠表面Al2O3和SiO2相结合,然后在镀液中被H2PO2-还原成金属银,为后续的化学镀提供催化活性中心。
(2)空心微珠表面化学镀Ni-P镀层过程中镀液的组成及试镀工艺条件对化学镀过程有较大影响。镀液中初始Ni2+浓度增加,反应速度并不随Ni2+浓度增大而加快,反应后剩余Ni2+浓度随初始Ni2+浓度增加而增大;还原剂次亚磷酸钠的浓度越大,反
应速度越快,反应后剩余金属离子浓度随次亚磷酸钠浓度增大而呈下降趋势;[Ni2+]/[柠檬酸根离子]的摩尔比越大亦即柠檬酸根离子浓度越低,反应速度越慢,反应后剩余金属离子浓度降低;用氨水调PH值时,当PH值少于9时,随着pH值增大,反应速度加快,当PH值大于9时,随pH值增大反应速度减慢;用氢氧化钠调节pH值,反应速度基本随pH值增加而增大,即pH值越大,反应速度越快;温度升高,反应速度加快;装载量越大,反应速度越快。
(3)空心微珠表面化学镀Ni-Co-P过程中,主盐中 Ni2+ 浓度增大,反应速度加快,突变时间缩短,总反应时间也缩短。当/(+)摩尔比大于0.4时,反应速度变化不大;次亚磷酸钠浓度的增大反应速度加快,当次亚磷酸钠的浓度大于0.3mol/l 时,反应突变时间已经变化不大,说明当次亚磷酸钠浓度与主盐的浓度比大于2:1时,反应速度达到最大,再增加次亚磷酸钠的浓度对镀速影响很小;缓冲剂硼酸对反应速度的影响较小,但存在最佳值0.5mol/l;采用柠檬酸钠和酒石酸钾钠复合作络合剂,在总浓度不变的情况下(络合剂总浓度为0.2mol/l),络合剂柠檬酸钠浓度越大,反应速度越快。但当柠檬酸钠浓度大于0.05mol/l时,增加柠檬酸钠浓度反应速度变化不大;用氨水调pH值时,当pH值小于8.5时,随着pH值增大,反应速度加快。当pH值大于9.5时,随pH值增大,反应速度急剧变缓,这主要由于氨水中的NH3对金属离子的络合作用降低了金属离子的浓度。用氢氧化钠调pH值,反应速度明显快于用氨水调pH值,并且随pH值增大,反应速度有加快的趋势。但是当pH值增大到10.5时,反应速度又有变缓的趋势,这可能是由于pH值过高,镀液中[OH-]浓度过大,[OH-]对金属离子进行络合的结果。装载量越大,反应速度越快。温度越高,反应速度越快。
(4)溶胶凝胶法制备的BaFe12O19铁氧体的生成条件是450℃预热处理1h后经850℃热处理3h。850℃保温时间太短,钡铁氧体没有完全晶化;保温时间太长,容易引起晶粒的长大。在溶胶凝胶法制备钡铁氧体的过程中,预热处理是一个关键的步骤,经过预热处理可以保证前驱物能够完全转化为γ-Fe2O3避免生成α-Fe2O3中间产物,从而降低钡铁氧体的完全晶化温度。初始溶液的pH值为7时才能得到均匀稳定的溶胶, 经热处理后生成单一、均匀的M型钡铁氧体。Fe与Ba之比从10到12之间都能够形成单一、均匀的M型钡铁氧体。原料中柠檬酸与硝酸盐之比为1时,自燃烧过程最剧烈;柠檬酸比例越高,所得粉体的颗粒越小;溶胶初期加入聚乙二醇可以降低所得超细粉末的颗粒粒径。
(5)随着Y、Eu、Nd等稀土元素RE搀杂量的增大,主晶相为六角晶系磁铅石型钡铁氧体相结构的钡铁氧体逐渐出现比较明显的REFeO3的衍射峰,并伴随着REFeO3
的出现,也出现了很少量的α-Fe2O3。Y、Eu、Nd等稀土元素RE对钡铁氧体的搀杂使样品的比饱和磁化强度下降,比剩余磁化强度?
Microwave absorbing materials have been widely in stealth technology and in electro-magnetic compatibility (EMC) technology, and they are researching hotspot in these technology field. In most of absorbers, the ferrite and metal powder are the main components because of good performance and low cost. But the defect of high density is not benefit for the preparation of light absorber. In response to the need for high performance absorber, in this paper, the composite-coating absorbers with hollow cenosphere as nuclear are prepared by sol-gel and electroless plating technology.
The Electroless Ni-P and Ni-Co-P-coating processes is modified by replacing the conventional sensitization and activation steps with only using activation step with AgNO3 activator, and the optimal forming conditions is made certain.
The BaFe12O19 and BaRexFe12-xO19 (RE denote Y、Nd and Eu) ultrafine powders with M-type structure are synthesized by sol-gel technique. The effects of the composition of the gel, strength of solution, the amount of complexing agent, the different kinds of anions, the adding of dispersant, and the condition in heat treatment of the gel on crystal phase, morphology and magnetic properties of The BaFe12O19 and BaRexFe12-xO19 were investigated systematically to clarify the optimum forming conditions.
Thin films of Barium hexaferrite are prepared on fly ash cenpsphere particles by sol-gel using Fe(NO3)3·9H2O、Ba(NO3)2 and citric acid as raw materials. The prepared films are characterized by differential and thermogravimetric analysis (DTA-TG), X-ray diffraction analysis (XRD), scanning electron microscope (SEM), energy dispersive spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and vibrating sample magnetometer(VSM) and Vector Network Analyzer.
Some important results are concluded as follows:
(1) The Electroless Ni-P and Ni-Co-P-coated cenospheres is preparated by replacing the conventional sensitization and activation steps with only using activation step with AgNO3 activator. The magnetic properties of Ni-P coated cenospheres are δs (27.3emu/g) and Hc (1807.2A/m) , while those of Ni-Co-P coated cenospheres are δs (27.36emu/g) and Hc (2059.5A/m), and those of Ni-P coated cenospheres after heat treatment are δs (2.08
emu/g) and Hc (15620.8A/m). The electroless mechanism is following: the ability of absorbing Ag(NH3)2+ is improved by hydroxy on cenosphere surface after alkali solution liquid rinsing. Then in the coating bath, [Ag(NH3)2]+ are reduced to Ag by H2PO2- . The catalytic action of Ag act as a nucleation sites for subsequent Ni-P or Ni-Co-P deposition.
(2) In the process of Ni-P electroless plating, the velocity of reaction is not augmented, while the residual Ni2+ after reaction is increased with the increased concentration of Ni2+. The velocity of reaction is increased, while the residual Ni2+ after reaction is declined with the increased concentration of H2PO2-. The velocity of reaction is fell, while the residual Ni2+ after reaction is declined with the increased mol ratio of Ni2+/[C6H5O7]3-. When the pH is adjusted by NH3.H2O the velocity of reaction is increased with the increase of pH (pH<9.0) and the velocity of reaction is fell with the increase of pH (pH>9.0). But when the pH is adjusted by NaOH the velocity of reaction is increased with the increase of pH. And the velocity of reaction is increased with the increasing temperature and the increasing loading.
(3) In the process of Ni-Co-P electroless plating, the velocity of reaction is augmented with the increased concentration of Ni2+. While the mol ratio of /(+) is more then 0.4, the velocity of reaction only change a little with the increased concentration of Ni2+. The velocity of reaction is increased with the increased concentration of H2PO2-. But when the concentration of H2PO2- is more than 0.3mol/l, the velocity of reaction only change a little. There is a little effect of the concentration of H3BO3 on the velocity of reaction, 0.5mol/l is the optimal concentration. The velocity of reaction is increased with the
引文
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