CN108585852A - 一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷、制备方法及其应用 - Google Patents
一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷、制备方法及其应用 Download PDFInfo
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- CN108585852A CN108585852A CN201810443144.2A CN201810443144A CN108585852A CN 108585852 A CN108585852 A CN 108585852A CN 201810443144 A CN201810443144 A CN 201810443144A CN 108585852 A CN108585852 A CN 108585852A
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- luminous
- zirconate
- piezoelectric ceramic
- temperature
- magnesium titanate
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- 239000000919 ceramic Substances 0.000 title claims abstract description 65
- 229910052777 Praseodymium Inorganic materials 0.000 title claims abstract description 60
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- GWDVJOAGOYAKRO-UHFFFAOYSA-N [Mg].[In].[Nb] Chemical compound [Mg].[In].[Nb] GWDVJOAGOYAKRO-UHFFFAOYSA-N 0.000 title claims description 49
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910002637 Pr6O11 Inorganic materials 0.000 claims abstract description 12
- 230000010287 polarization Effects 0.000 claims abstract description 9
- 229910019653 Mg1/3Nb2/3 Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000010955 niobium Substances 0.000 claims abstract description 8
- 230000033228 biological regulation Effects 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- AUVAKDFLPHLTIX-UHFFFAOYSA-N [Pb].[Mg].[In].[Nb] Chemical compound [Pb].[Mg].[In].[Nb] AUVAKDFLPHLTIX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 60
- 238000000498 ball milling Methods 0.000 claims description 51
- 238000001035 drying Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 17
- 229910052791 calcium Inorganic materials 0.000 claims description 17
- 239000011575 calcium Substances 0.000 claims description 17
- 239000004570 mortar (masonry) Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 12
- 230000005684 electric field Effects 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 8
- 230000001070 adhesive effect Effects 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims description 3
- 238000005424 photoluminescence Methods 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 2
- 239000002981 blocking agent Substances 0.000 claims 1
- 239000007767 bonding agent Substances 0.000 claims 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 229910052573 porcelain Inorganic materials 0.000 claims 1
- 239000002243 precursor Substances 0.000 claims 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 8
- 150000002910 rare earth metals Chemical class 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 26
- 230000008878 coupling Effects 0.000 description 6
- 238000010168 coupling process Methods 0.000 description 6
- 238000005859 coupling reaction Methods 0.000 description 6
- 230000000994 depressogenic effect Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- RZVJAVOTAADABK-UHFFFAOYSA-N [Nb].[In] Chemical compound [Nb].[In] RZVJAVOTAADABK-UHFFFAOYSA-N 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005662 electromechanics Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- WCWKKSOQLQEJTE-UHFFFAOYSA-N praseodymium(3+) Chemical compound [Pr+3] WCWKKSOQLQEJTE-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
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- 238000005303 weighing Methods 0.000 description 1
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Abstract
一种镨掺杂铌铟镁酸铅‑钛酸铅发光压电陶瓷、制备方法及其应用,本发明属于功能陶瓷材料领域,具体涉及一种镨掺杂铌铟镁酸铅‑钛酸铅发光压电陶瓷、制备方法及其应用。本发明要解决现有稀土元素掺杂压电陶瓷机电性能偏低的问题。压电陶瓷的化学式为0.24Pb(In1/2Nb1/2)O3‑0.42Pb(Mg1/3Nb2/3)O3‑0.34PbTiO3:xPr3+,其中x为摩尔分数,0<x≤0.02。制备方法为先合成InNbO4和MgNb2O6前驱体,然后以InNbO4、MgNb2O6、PbO、TiO2和Pr6O11为原料制备,再镀金电极及极化处理,即得到压电陶瓷。本发明用于高灵敏度温度传感和电光调控。
Description
技术领域
本发明属于功能陶瓷材料领域,具体涉及一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷、制备方法及其应用。
背景技术
稀土元素是化学元素周期表中具有丰富物理化学性质的一类元素。稀土发光材料一般是由稀土元素和材料主体化合物组成的,用以发光的稀土元素通常被称为发光中心或者激活剂,材料主体化合物被称为基质。稀土元素掺杂的多功能材料具备显著的可调制发光特性,而稀土元素镨掺杂的氧化物被证明具有高效的发光效率,在发光器件、光学传感器件方面表现出巨大应用潜力,引起了科学界与工业界的广泛关注。研究表明,对于具有机电耦合效应的压电基质材料,镨的发光强度强烈依赖于掺杂浓度、温度和晶场等环境因素,因而使得镨掺杂压电陶瓷发光材料在温度传感、电场传感等传感器领域有着广阔的应用。
但是,目前作为镨掺杂氧化物基质的压电材料的压电系数和机电耦合因子普遍偏低。例如,镨掺杂钛酸钡基压电陶瓷的压电系数d33为200-300pC/N,机电耦合因子kp约为50%,而镨掺杂钛酸铋钠基压电陶瓷的压电系数d33仅为80-100pC/N。基质材料较低的压电性能限制了镨掺杂氧化物在高灵敏度温度传感、电场传感领域的进一步应用。因此,制备具有高压电性能和机电耦合因子的新型镨掺杂发光压电陶瓷材料,进而通过镨离子各能级相关的荧光发射强度比值随温度变化的关系,实现高灵敏度的温度测量,具有重要的实际意义。
发明内容
本发明是要解决现有稀土元素掺杂压电陶瓷机电性能偏低的问题,而提供一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷、制备方法及其应用。
一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的化学通式为0.24Pb(In1/2Nb1/2)O3-0.42Pb(Mg1/3Nb2/3)O3-0.34PbTiO3:xPr3+,其中x为摩尔分数,0<x≤0.02。
一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法是按以下步骤完成的:
一、采用固相反应法合成纯相的InNbO4前驱体粉体;
二、采用固相反应法合成纯相的MgNb2O6前驱体粉体;
三、以PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体为原料,采用固相反应法合成具有钙钦矿结构的预烧粉体;
四、将具有钙钦矿结构的预烧粉体放入研钵中研磨,然后转移至球磨罐中,以无水乙醇作为球磨介质在转速为120~200r/min的条件下球磨8~12h,得到球磨后的湿料,将球磨后的湿料置于温度为60~120℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料与粘合剂混合在10~50MPa压强下保压2~3min压成圆片,再次放入研钵中研磨,80~200目过筛后,在4~10MPa的压强下保压2~3min压成圆片,得到成型圆片;
五、将成型圆片置于坩埚中,采用具有钙钦矿结构的预烧粉体进行掩埋,以2~4℃/min的升温速率将坩埚由室温升温至500~650℃,在温度为500~650℃的条件下保温2h~4h,然后以2~4℃/min的升温速率将温度从500~650℃升温至1000~1300℃,在温度为1000~1300℃的条件下烧结5~7h,得到烧结后的陶瓷片;
六、对烧结后的陶瓷片进行表面磨平处理,然后采用小型金属溅射镀膜机对烧结后的陶瓷片镀金20~30min,得到镀金后的陶瓷片,再采用直流高压电源在温度为100~150℃、电场强度为15~20kV/cm的条件下对镀金后的陶瓷片极化处理30~60min,极化完成后,即得到镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷。
一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷用于高灵敏度温度传感和电光调控。
本发明有益效果:本发明制备的镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷具有良好的机电性能和发光性能,矫顽场Ec为11kv/cm~7kv/cm,机械品质因数Qm为90~70,压电应变系数d33为550pC/N~450pC/N,机电耦合系数kp为68%~50%。本发明利用镨掺杂铌铟镁酸铅-钛酸铅压电陶瓷的1D2-3H4和3P0-3H4荧光强度比值与温度的关系实现了高灵敏度的温度传感,同时实现陶瓷的电光调控。
附图说明
图1为实施例一得到的镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的XRD谱图;
图2为实施例一得到的镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的表面SEM图;
图3为实施例一得到的镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的室温电滞回线;其中1表示40kV/cm,2表示30kV/cm,3表示20kV/cm,4表示10kV/cm;
图4为实施例一得到的镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的变温发光光谱图;其中按箭头方向从上到下依次为308K、318K、328K、338K、348K、358K、368K、378K和388K不同温度的曲线;
图5为实施例一得到的镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷温度传感拟合曲线;
图6为实施例一得到的镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷在不同直流电压下的PL光谱图;其中按箭头方向从上到下依次为0.00kV/cm、0.63kV/cm、1.25kV/cm、1.88kV/cm和2.50kV/cm不同电场强度的曲线。
具体实施方式
本发明技术方案不限于以下所列举的具体实施方式,还包括各具体实施方式之间的任意组合。
具体实施方式一:本实施方式一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的化学通式为0.24Pb(In1/2Nb1/2)O3-0.42Pb(Mg1/3Nb2/3)O3-0.34PbTiO3:xPr3+,其中x为摩尔分数,0<x≤0.02。
具体实施方式二:本实施方式一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法是按以下步骤完成的:
一、采用固相反应法合成纯相的InNbO4前驱体粉体;
二、采用固相反应法合成纯相的MgNb2O6前驱体粉体;
三、以PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体为原料,采用固相反应法合成具有钙钦矿结构的预烧粉体;
四、将具有钙钦矿结构的预烧粉体放入研钵中研磨,然后转移至球磨罐中,以无水乙醇作为球磨介质在转速为120~200r/min的条件下球磨8~12h,得到球磨后的湿料,将球磨后的湿料置于温度为60~120℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料与粘合剂混合在10~50MPa压强下保压2~3min压成圆片,再次放入研钵中研磨,80~200目过筛后,在4~10MPa的压强下保压2~3min压成圆片,得到成型圆片;
五、将成型圆片置于坩埚中,采用具有钙钦矿结构的预烧粉体进行掩埋,以2~4℃/min的升温速率将坩埚由室温升温至500~650℃,在温度为500~650℃的条件下保温2~4h,然后以2~4℃/min的升温速率将温度从500~650℃升温至1000~1300℃,在温度为1000~1300℃的条件下烧结5~7h,得到烧结后的陶瓷片;
六、对烧结后的陶瓷片进行表面磨平处理,然后采用小型金属溅射镀膜机对烧结后的陶瓷片镀金20~30min,得到镀金后的陶瓷片,再采用直流高压电源在温度为100~150℃、电场强度为15~20kV/cm的条件下对镀金后的陶瓷片极化处理30~60min,极化完成后,即得到镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷。
本实施方式步骤五中以2~4℃/min的升温速率将坩埚由室温升温至500~650℃,在温度为500~650℃的条件下保温2~4h的目的是排除粘合剂。
具体实施方式三:本实施方式与具体实施方式二不同的是:步骤一中采用固相反应法合成纯相的InNbO4前驱体粉体具体是按以下步骤进行的:
将In2O3和Nb2O5按照摩尔比1:1进行称取,将称取的In2O3和Nb2O5混合并置于球磨罐中,以无水乙醇作为球磨介质在转速为200~260r/min的条件下球磨40~50h,得到球磨后的湿料,将球磨后的湿料置于温度为80~120℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料在20~30MPa压强下压成直径为30mm的圆片,将直径为30mm的圆片置于坩埚中,以2~4℃/min的升温速率将坩埚由室温升温至1000~1200℃,在温度为1000~1200℃的条件下烧结4~7h,烧结后放入研钵中研磨成粉末,得到纯相的InNbO4前驱体粉体。其他与具体实施方式二相同。
具体实施方式四:本实施方式与具体实施方式二或三不同的是:步骤二中采用固相反应法合成纯相的MgNb2O6前驱体粉体具体是按以下步骤进行的:
将MgO和Nb2O5按照摩尔比1:1进行称取,将称取的MgO和Nb2O5混合并置于球磨罐中,以无水乙醇作为球磨介质在转速为200~260r/min的条件下球磨40~50h,得到球磨后的湿料,将球磨后的湿料置于温度为80~120℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料在20~30MPa压强下压成直径为30mm的圆片,将直径为30mm的圆片置于坩埚中,以2~5℃/min的升温速率将坩埚由室温升温至900~1200℃,在温度为900~1200℃的条件下烧结5~7h,烧结后放入研钵中研磨成粉末,得到纯相的MgNb2O6前驱体粉体。其他与具体实施方式二或三相同。
具体实施方式五:本实施方式与具体实施方式二至四之一不同的是:步骤三中以PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体为原料,采用固相反应法合成具有钙钦矿结构的预烧粉体具体是按以下步骤进行的:
按化学通式为0.24Pb(In1/2Nb1/2)O3-0.42Pb(Mg1/3Nb2/3)O3-0.34PbTiO3:xPr3+配比称取PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体,其中x为摩尔分数,0<x≤0.02,然后将称取的PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体混合,得到混合料,将混合料置于球磨罐中,以无水乙醇作为球磨介质在转速为130~200r/min的条件下球磨40~50h,得到球磨后的湿料,将球磨后的湿料置于温度为80~120℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料用研钵进行研磨得到混合粉末,在20~30MPa压强下压成直径为30mm的圆片,将直径为30mm的圆片置于坩埚中,以1~3℃/min的升温速率将坩埚由室温升温至700~900℃,在温度为700~900℃的条件下煅烧3~5h,得到具有钙钦矿结构的预烧粉体;所述混合料与无水乙醇的质量比为1:(1.2~1.5)。其他与具体实施方式二至四之一相同。
具体实施方式六:本实施方式与具体实施方式二至五之一不同的是:步骤四得到的成型圆片的直径为13mm。其他与具体实施方式二至五之一相同。
具体实施方式七:本实施方式与具体实施方式二至六之一不同的是:步骤四中所述粘合剂为PVA,粘合剂的添加量为干燥块料质量的3~5%。其他与具体实施方式二至六之一相同。
具体实施方式八:本实施方式一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷用于高灵敏度温度传感和电光调控。
具体实施方式九:本实施方式与具体实施方式八不同的是:镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷用于高灵敏度温度传感按以下步骤进行:在加热温度为300K~450K的范围下,采用300nm~400nm激发光对铌铟镁酸铅-钛酸铅压电陶瓷的光致发光特性进行测量,得到峰位中心分别位于492nm蓝光和603nm红光发光峰。其他与具体实施方式八相同。
具体实施方式十:本实施方式与具体实施方式八或九不同的是:镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷用于电光调控的极化电场为0.5kV/cm~3.5kV/cm。其他与具体实施方式八或九相同。
采用下述实施例验证本发明的有益效果:
实施例一:一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法是按以下步骤完成的:
一、将In2O3和Nb2O5按照摩尔比1:1进行称取,将称取的In2O3和Nb2O5混合并置于球磨罐中,以无水乙醇作为球磨介质在转速为220r/min的条件下球磨48h,得到球磨后的湿料,将球磨后的湿料置于温度为80℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料在20MPa压强下压成直径为30mm的圆片,将直径为30mm的圆片置于坩埚中,以2℃/min的升温速率将坩埚由室温升温至1100℃,在温度为1100℃的条件下烧结7h,烧结后放入研钵中研磨成粉末,得到纯相的InNbO4前驱体粉体;
二、将MgO和Nb2O5按照摩尔比1:1进行称取,将称取的MgO和Nb2O5混合并置于球磨罐中,以无水乙醇作为球磨介质在转速为220r/min的条件下球磨48h,得到球磨后的湿料,将球磨后的湿料置于温度为80℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料在20MPa压强下压成直径为30mm的圆片,将直径为30mm的圆片置于坩埚中,以3℃/min的升温速率将坩埚由室温升温至1000℃,在温度为1000℃的条件下烧结7h,烧结后放入研钵中研磨成粉末,得到纯相的MgNb2O6前驱体粉体;
三、按化学通式为0.24Pb(In1/2Nb1/2)O3-0.42Pb(Mg1/3Nb2/3)O3-0.34PbTiO3:xPr3+配比称取PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体,其中x为摩尔分数,x=0.005,然后将称取的PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体混合,得到混合料,将混合料置于球磨罐中,以无水乙醇作为球磨介质在转速为150r/min的条件下球磨48h,得到球磨后的湿料,将球磨后的湿料置于温度为80℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料用研钵进行研磨得到混合粉末,在20MPa压强下压成直径为30mm的圆片,将直径为30mm的圆片置于坩埚中,以2℃/min的升温速率将坩埚由室温升温至800℃,在温度为800℃的条件下煅烧4h,得到具有钙钦矿结构的预烧粉体;所述混合料与无水乙醇的质量比为1:1.3;
四、将具有钙钦矿结构的预烧粉体放入研钵中研磨,然后转移至球磨罐中,以无水乙醇作为球磨介质在转速为150r/min的条件下球磨8h,得到球磨后的湿料,将球磨后的湿料置于温度为60℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料与PVA混合在20MPa压强下保压3min压成圆片,再次放入研钵中研磨,80~200目过筛后,在6MPa的压强下保压3min压成圆片,得到成型圆片;成型圆片的直径为13mm;所述粘合剂的添加量为干燥块料质量的3~5%;
五、将成型圆片置于坩埚中,采用具有钙钦矿结构的预烧粉体进行掩埋,以2℃/min的升温速率将坩埚由室温升温至550℃,在温度为550℃的条件下保温3h,然后以2℃/min的升温速率将温度从550℃升温至1150℃,在温度为1150℃的条件下烧结6h,得到烧结后的陶瓷片;
六、对烧结后的陶瓷片进行表面磨平处理,然后采用小型金属溅射镀膜机对烧结后的陶瓷片镀金20min,得到镀金后的陶瓷片,再采用直流高压电源在温度为150℃、电场强度为20kV/cm的条件下对镀金后的陶瓷片极化处理60min,极化完成后,即得到镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷,其化学式为0.24Pb(In1/2Nb1/2)O3-0.42Pb(Mg1/3Nb2/3)O3-0.34PbTiO3:0.005Pr3+。
对实施例一得到的镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷进行结构和性能测试:
步骤一:将陶瓷样品研碎磨细成粉体用于X射线粉末衍射,具体测试条件为室温下,测量角度范围为10度~90度,采用的步长为0.01度,每分钟2度。根据所得X射线粉末衍射谱图,如图1所示,表明室温下镨掺杂铌铟镁酸铅-钛酸铅压电陶瓷具有纯钙钦矿结构。
步骤二:将得到的陶瓷样品,在表面进行喷金后,用德国卡尔蔡司公司SIGMA-300扫描电镜观察陶瓷表面的形貌,如图2所示,表明陶瓷片中晶粒大小分布均匀,致密性良好。
步骤三:将所得到的镨掺杂铌铟镁酸铅-钛酸铅压电陶瓷样品两面抛光后喷金,用于电滞回线的测试。测量不同电场下的电滞回线。在±40kv/cm的直流电压下,出现饱和现象。确定矫顽场Ec为8kv/cm~7kv/cm,如图3所示。
步骤四:测试镨掺杂铌铟镁酸铅-钛酸铅压电陶瓷的压电性能。利用准静态d33测试仪测得的压电常数d33为500pC/N~450pC/N。
步骤五:测试镨掺杂铌铟镁酸铅-钛酸铅压电陶瓷的其他电学参数。利用HP4294测试仪可以得到压电陶瓷在室温下的机电耦合系数、机械品质因素。机电耦合系数kp为60%~50%,机械品质因素Qm为80~70,镨掺杂铌铟镁酸铅-钛酸铅压电陶瓷表现出了非常优异的压电、介电性能。
将实施例一得到的镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷进行温度传感和电光调控应用。
步骤一:将所得到的镨掺杂铌铟镁酸铅-钛酸铅压电陶瓷样品两面抛光后,用HORIBA,Fluoromax-4分光光谱仪对其发光特性进行测试。用360nm激发光对铌铟镁酸铅-钛酸铅压电陶瓷样品的光致发光特性进行测量,如图4所示,得到峰位中心分别位于的492nm蓝光发光峰和603nm红光发光峰。并进一步利用其1D2-3H4和3P0-3H4荧光强度比值与温度的关系实现了高灵敏度的温度传感。603nm处与492nm处的激发强度的比值随温度变化的拟合曲线如图5所示,并给出了拟合的公式。拟合结果表明,其传感灵敏度为9987.1/T2,拟合度达到0.999,实现了高灵敏度的温度传感应用。
步骤二:将所得到的镨掺杂铌铟镁酸铅-钛酸铅压电陶瓷样品两面抛光后,在0.5kv/mm~3.5kv/mm直流电场下,测量其光致发光谱,如图6所示,实现了镨掺杂铌铟镁酸铅-钛酸铅压电陶瓷的电光调控。
Claims (10)
1.一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷,其特征在于镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的化学通式为0.24Pb(In1/2Nb1/2)O3-0.42Pb(Mg1/3Nb2/3)O3-0.34PbTiO3:xPr3+,其中x为摩尔分数,0<x≤0.02。
2.如权利要求1所述的一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法,其特征在于镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法是按以下步骤完成的:
一、采用固相反应法合成纯相的InNbO4前驱体粉体;
二、采用固相反应法合成纯相的MgNb2O6前驱体粉体;
三、以PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体为原料,采用固相反应法合成具有钙钦矿结构的预烧粉体;
四、将具有钙钦矿结构的预烧粉体放入研钵中研磨,然后转移至球磨罐中,以无水乙醇作为球磨介质在转速为120~200r/min的条件下球磨8~12h,得到球磨后的湿料,将球磨后的湿料置于温度为60~120℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料与粘合剂混合在10~50MPa压强下保压2~3min压成圆片,再次放入研钵中研磨,80~200目过筛后,在4~10MPa的压强下保压2~3min压成圆片,得到成型圆片;
五、将成型圆片置于坩埚中,采用具有钙钦矿结构的预烧粉体进行掩埋,以2~4℃/min的升温速率将坩埚由室温升温至500~650℃,在温度为500~650℃的条件下保温2~4h,然后以2~4℃/min的升温速率将温度从500~650℃升温至1000~1300℃,在温度为1000~1300℃的条件下烧结5~7h,得到烧结后的陶瓷片;
六、对烧结后的陶瓷片进行表面磨平处理,然后采用小型金属溅射镀膜机对烧结后的陶瓷片镀金20~30min,得到镀金后的陶瓷片,再采用直流高压电源在温度为100~150℃、电场强度为15~20kV/cm的条件下对镀金后的陶瓷片极化处理30~60min,极化完成后,即得到镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷。
3.根据权利要求2所述的一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法,其特征在于步骤一中采用固相反应法合成纯相的InNbO4前驱体粉体具体是按以下步骤进行的:
将In2O3和Nb2O5按照摩尔比1:1进行称取,将称取的In2O3和Nb2O5混合并置于球磨罐中,以无水乙醇作为球磨介质在转速为200~260r/min的条件下球磨40~50h,得到球磨后的湿料,将球磨后的湿料置于温度为80~120℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料在20~30MPa压强下压成直径为30mm的圆片,将直径为30mm的圆片置于坩埚中,以2~4℃/min的升温速率将坩埚由室温升温至1000~1200℃,在温度为1000~1200℃的条件下烧结4~7h,烧结后放入研钵中研磨成粉末,得到纯相的InNbO4前驱体粉体。
4.根据权利要求2所述的一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法,其特征在于步骤二中采用固相反应法合成纯相的MgNb2O6前驱体粉体具体是按以下步骤进行的:
将MgO和Nb2O5按照摩尔比1:1进行称取,将称取的MgO和Nb2O5混合并置于球磨罐中,以无水乙醇作为球磨介质在转速为200~260r/min的条件下球磨40~50h,得到球磨后的湿料,将球磨后的湿料置于温度为80~120℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料在20~30MPa压强下压成直径为30mm的圆片,将直径为30mm的圆片置于坩埚中,以2~5℃/min的升温速率将坩埚由室温升温至900~1200℃,在温度为900~1200℃的条件下烧结5~7h,烧结后放入研钵中研磨成粉末,得到纯相的MgNb2O6前驱体粉体。
5.根据权利要求2所述的一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法,其特征在于步骤三中以PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体为原料,采用固相反应法合成具有钙钦矿结构的预烧粉体具体是按以下步骤进行的:
按化学通式为0.24Pb(In1/2Nb1/2)O3-0.42Pb(Mg1/3Nb2/3)O3-0.34PbTiO3:xPr3+配比称取PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体,其中x为摩尔分数,0<x≤0.02,然后将称取的PbO、TiO2、Pr6O11、纯相的InNbO4前驱体粉体和纯相的MgNb2O6前驱体粉体混合,得到混合料,将混合料置于球磨罐中,以无水乙醇作为球磨介质在转速为130~200r/min的条件下球磨40~50h,得到球磨后的湿料,将球磨后的湿料置于温度为80~120℃的电热鼓风干燥箱内烘干,得到干燥块料,将干燥块料用研钵进行研磨得到混合粉末,在20~30MPa压强下压成直径为30mm的圆片,将直径为30mm的圆片置于坩埚中,以1~3℃/min的升温速率将坩埚由室温升温至700~900℃,在温度为700~900℃的条件下煅烧3~5h,得到具有钙钦矿结构的预烧粉体;所述混合料与无水乙醇的质量比为1:(1.2~1.5)。
6.根据权利要求2所述的一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法,其特征在于步骤四得到的成型圆片的直径为13mm。
7.根据权利要求2所述的一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的制备方法,其特征在于步骤四中所述粘合剂为PVA,粘合剂的添加量为干燥块料质量的3~5%。
8.如权利要求1所述的一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的应用,其特征在于镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷用于高灵敏度温度传感和电光调控。
9.根据权利要求8所述的一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的应用,其特征在于镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷用于高灵敏度温度传感按以下步骤进行:在加热温度为300K~450K的范围下,采用300nm~400nm激发光对铌铟镁酸铅-钛酸铅压电陶瓷的光致发光特性进行测量,得到峰位中心分别位于492nm蓝光和603nm红光发光峰。
10.根据权利要求8所述的一种镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷的应用,其特征在于镨掺杂铌铟镁酸铅-钛酸铅发光压电陶瓷用于电光调控的极化电场为0.5kV/cm~3.5kV/cm。
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