CN102320666B - 氟替代铁酸铋晶格中氧的制备方法 - Google Patents
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Abstract
氟替代铁酸铋晶格中氧的制备方法,步骤1:采用耐腐蚀材料做成的器皿为容器,采用稀酸为溶剂,称量化学计量比的Bi的氮化物和Fe的氮化物加入溶剂中,摩尔比为1∶1,配制适量的含氟盐,最后在溶液中加入柠檬酸。步骤2:将配置好的溶液在水浴中初步反应,反应时间为2.5±0.5h,反应过程中均匀搅拌。然后在烘箱中烘干得到粉末;步骤3:把得到的粉末放置于高温下进行分解反应,高温条件为780±15℃,反应时间为30±3min;除去杂质;将分解后的粉末进行压片,在高温下烧结,其烧结温度为810±15℃,烧结时间为10±2min;得到F-1有效地进入BFO晶格的样品。氟有效进入铁酸铋晶格并取代氧的样品既具有铁电性,又具有铁磁性,为实现多功能电子器件的发展提供另一条通途。
Description
一、技术领域
本发明所属领域为新型功能材料,尤其是氟替代铁酸铋晶格中氧的制备方法。
二、背景技术
随着科学技术的日新月异,人们对器件的多功能性和小型化的要求越来越高,这就需要发展同时具有两种或两种以上功能的新材料,以研制能同时实现多种功能的新型器件。多铁性材料是近年来功能材料的研究热点之一。多铁性材料是指在一定温度范围内同时存在铁磁序、铁电序及铁弹序的体系。由于各种物理效应同处一个体系,它们之间不可避免地将发生互相作用,从而实现不同功能间的互相调控,为发展新的多功能器件提供机会。由于铁磁性和铁电性在现代科技中有着广泛地应用,人们自然而然地想到能否将铁磁性和铁电性结合在一起,获得同时具有铁磁性和铁电性的材料。
有关铁磁性和铁电性功能间的互相调控,国际国内学者取得了较大的进展,发表的文献主要有:1)Science 309(2005)391-392;2)Nature Materials 6(2007)296-302;3)Science 312(2006)1481-1482;4)Nature Materials 7(2008)425-426;5)Physical Review Letters 98(2007)257602;6)Nature 442(2006)759-765.多铁性材料在磁介质存储方面有着极其重要的应用前景,是国际国内科研工作者研究的热点之一。
BiFeO3是到目前为止唯一同时在室温以上表现出铁电性和磁性的材料.其结构为典型的单钙钛矿ABO3结构型化合物。室温下BiFeO3具有棱形畸变钙钛矿结构,空间群为R3c,晶格常数为a=b=c=5.633和α=β=γ=59.4°,其铁电相变发生在TC≈1110K,反铁磁奈尔温度TN≈640K,这一高的相变温度也预示其很大的自发极化,理论预测室温下其饱和电极化可达100μC/cm2,有着潜在巨大的应用价值。
BiFeO3自发现以来就受到广泛的关注,科研工作者对其成相条件、微结构、铁电性起源、自旋排列进行了广泛而深入的研究。对其进行了丰富的阳离子掺杂,近年来发表的国际文献有:1)Current Applied Physics 11(2011)508-512;2)J MaterSci:Mater Electron(2011)22:323-327;3)Applied Physics Letters 98(2011)072901;4)Physical Review B 83(2011)054406.虽然阳离子掺杂取得了丰硕的成果,但阴离子掺杂的工作在国际国内范围内还无人进行,这主要是由于阴离子掺杂的制备工艺不够完善,阴离子未能有效地进入晶格导致的。阴离子有效地进入BiFeO3晶格对其微结构,铁电性及铁磁性有重要影响。科研工作者一直寻求一种能有效地将阴离子掺入BiFeO3晶格的方法。本发明介绍一种切实可行的F有效进入BiFeO3晶格的制备方法。该技术不但能有效地使氟进入铁酸铋晶格,占据氧位,而且制备出的材料颗粒均匀。
三、发明内容
本发明的目的是使氟有效进入铁酸铋晶格,占据氧位,从而制备出具有铁磁性和铁电性的铁磁共同体,以实现磁电耦合,便于制备各种多功能的器件。
本发明的技术方案是:氟替代铁酸铋晶格中氧的制备方法,即阴离子F-1有效进入BiFeO3(BFO)晶格并取代氧的制备方法。
步骤1:采用耐腐蚀材料做成的器皿为容器,采用稀酸为溶剂,称量化学计量比的Bi的氮化物(Bi(NO3)3·5H2O)和Fe的氮化物(Fe(NO3)3·9H2O)加入溶剂中,两者之间的摩尔比为1∶1,然后配制适量的含氟盐(HF),最后在溶液中加入柠檬酸。
步骤2:将配置好的溶液在水浴中初步反应,水浴温度为80±5℃,反应时间为2.5±0.5h,反应过程中均匀搅拌。然后在烘箱中烘干得到粉末,烘烤温度为260±10℃,在烘烤过程中初步反应;
步骤3:把得到的粉末放置于高温下进行分解反应,高温条件为780±15℃,反应时间为30±3min;除去杂质;将分解后的粉末进行压片,在高温下烧结,其烧结温度为810±15℃,烧结时间为10±2min;得到F-1有效地进入BFO晶格的样品。即BiFeO3-XFX;x=0.1-0.25。
本发明有益效果是:本发明氟替代铁酸铋晶格中氧的制备方法制备出的样品,其铁磁性显著增强。掺F的铁酸铋样品既具有铁电性,又具有铁磁性,这使多功能电子器件的发展得到保证。具有铁磁性和铁电性的铁磁共同体,以实现磁电耦合。
四、附图说明
图1是制备流程示意图。
图2是氟的掺杂量分别为0.1、0.15、0.2、0.25的样品BiFeO2.9F0.1、BiFeO2.85F0.15、BiFeO2.8F0.2、BiFeO2.75F0.25的X射线衍射图谱。
图3是氟的掺杂量为0.25的样品BiFeO2.75F0.25的X射线光电子能谱。
图4是氟的掺杂量为0.25的样品BiFeO2.75F0.25的SEM图。
图5是氟的掺杂量分别为0、0.1、0.15、0.2、0.25的系列样品BiFeO3、BiFeO2.9F0.1、BiFeO2.85F0.15、BiFeO2.8F0.2、BiFeO2.75F0.25的磁滞回线示意图,内插图是剩余极化强度与掺杂量的关系。F的掺杂使BFO的磁性明显增强。
五、具体实施方式
实施例1:合成F的含量为0.25(结构式)的样品
采用附图1所示的制备流程,合成F含量为0.25的BiFeO2.75F0.25样品。其合成步骤为:
a)采用耐腐蚀材料做成的器皿为容器,首先配制一种稀酸溶液,取200ml的烧杯一个,量取稀酸溶液100ml。称取摩尔质量比为1∶1的Bi盐(Bi(NO3)3·5H2O)和Fe盐(Fe(NO3)3·9H2O)加入该稀酸溶液中,充分搅拌,使其完全溶解,并混合均匀。
b)烧杯一个,滴灌一只,AL104Mettler Toledo电子天平一台。称量化学计量比含F盐(HF),加入到a)配制好的溶液中,充分搅拌,使其混合均匀。
c)称取适量柠檬酸加入b)配置好的溶液中,充分搅拌,使其完全溶解,并混合均匀。
d)将c)配制好的溶液放在水浴锅内,使其混合均匀,并初步反应。
e)将在水浴锅内充分混合搅拌后的溶液放在烘箱内烘干成粉。
f)将e)所得粉末放置于高温下进行分解反应。
g)将f)所得到的粉末进行研磨、压片。
h)将g)压片后得到的样品在高温下烧结。
至此,样品的制备已经完成,为检测样品的质量,我们做了X射线衍射(X-raydiffraction,XRD)分析,其XRD图谱如附图2中的x=0.25所示。XRD结果说明样品的成相度很好。X射线光电子能谱分析(X-ray photo electron spectroscopy,XPS)如附图3所示。XRD和XPS的实验结果说明氟有效地进入了铁酸铋晶格。附图4是F含量为0.25样品的扫描电子显微镜照片,其颗粒尺寸为纳米级,与固相反应法制备出的微米级的颗粒相比,其尺寸明显减小。为检测F有效地进入铁酸铋晶格后,其性能是否显著增强,测量了其室温下的磁滞回线,如附图5中的X=0.25所示。结果表明:氟有效进入铋铁氧晶格的样品表现出了明显的铁磁性。未掺杂的铋铁氧样品由于自旋螺旋排列,并不显示宏观铁磁性,但氟进入铋铁氧晶格后,其铁磁性显著增强。掺F的铋铁氧样品既具有铁电性,又具有铁磁性,这使多功能电子器件的发展看到了曙光。
实施例2:合成F的含量为0.2(结构式)的样品
采用附图1所示的制备流程,合成F的掺杂量为0.2的BiFeO2.8F0.2样品。其合成步骤同实施例1中的步骤。
样品制备完成后,为检测样品的质量,我们做了X射线衍射(X-ray diffraction,XRD)分析,其XRD图谱如附图2中的x=0.2所示。XRD结果说明样品的成相度很好。为检测F有效地进入铋铁氧晶格后,其性能是否显著增强,测量了其室温下的磁滞回线,如附图5中的X=0.2所示。结果表明:F有效地进入铋铁氧晶格后,表现出了明显的铁磁性。
实施例3:合成F的含量为0.15的样品
采用附图1所示的制备流程,合成F的含量为0.15的BiFeO2.85F0.15样品。其合成步骤同实施例1中的步骤。
样品制备完成后,为检测样品的质量,我们做了X射线衍射(X-ray diffraction,XRD)分析,其XRD图谱如附图2中的x=0.15所示。XRD结果说明样品的成相度很好。为检测F有效地进入铋铁氧晶格后,其性能是否显著增强,测量了其室温下的磁滞回线,如附图5中的X=0.15所示。结果表明:F有效地进入铋铁氧晶格后,表现出了明显的铁磁性。
实施例4:合成F的含量为0.1的样品
采用附图1所示的制备流程,合成F的含量为0.1的BiFeO2.9F0.1样品。其合成步骤同实施例1中的步骤。
样品制备完成后,为检测样品的质量,我们做了X射线衍射(X-ray diffraction,XRD)分析,其XRD图谱如附图2的x=0.1所示。XRD结果说明样品的成相度很好。其室温下的磁滞回线如附图5中的X=0.1所示。结果表明:F有效地进入铋铁氧晶格后,其磁性增强。
Claims (3)
1.氟替代铁酸铋晶格中氧的制备方法,其特征是
步骤1:采用耐腐蚀材料做成的器皿为容器,采用稀酸为溶剂,称量化学计量比的Bi(NO3)3·5H2O和Fe(NO3)3·9H2O加入溶剂中,两者之间的摩尔比为1:1,然后配制适量的含氟盐,最后在溶液中加入柠檬酸;
步骤2:将配置好的溶液在水浴中初步反应,水浴温度为80±5℃,反应时间为2.5±0.5h,反应过程中均匀搅拌;然后在烘箱中烘干得到粉末,烘烤温度为260±10℃,在烘烤过程中初步反应;
步骤3:把得到的粉末放置于高温下进行分解反应,高温条件为780±15℃,反应时间为30±3min;除去杂质;将分解后的粉末进行压片,在高温下烧结,其烧结温度为810±15℃,烧结时间为10±2min;得到F-1有效地进入BFO晶格的样品,且BiFeO3-XFX中,x=0.1-0.25。
2.如权利要求1所述的氟替代铁酸铋晶格中氧的制备方法,其特征是所述柠檬酸为C6H8O7·H2O,C6H8O7·H2O与Fe(NO3)3·9H2O的摩尔比是1:1。
3.如权利要求1所述的氟替代铁酸铋晶格中氧的制备方法,其特征是压片的压强为12-18MPa。
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Room temperature electrodeposition and characterization of bismuth ferric oxide (BFO) thin films from aqueous nitrate bath;T.P. Gujar et al.;《applied surface science》;20050624;第252卷;第3586页实验部分 * |
T.P. Gujar et al..Room temperature electrodeposition and characterization of bismuth ferric oxide (BFO) thin films from aqueous nitrate bath.《applied surface science》.2005,第252卷 |
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