CN111908915A - 一种锆钛酸镧铅基压电陶瓷及其制备方法与应用 - Google Patents
一种锆钛酸镧铅基压电陶瓷及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种锆钛酸镧铅基压电陶瓷及其制备方法与应用。所述锆钛酸镧铅基压电陶瓷的组成为:Pb1‑xLax(ZryTi1‑y)1‑x/4O3+a Pb(Yb0.5Nb0.5)O3+b N,其中,N为Sb2O5或Sb2O3,x=0.055~0.070,y=0.55~0.61,以Pb1‑xLax(ZryTi1‑y)1‑x/4O3总重为百分比,a为0.8~1.2%,b为0.8~1.2%。以Pb3O4、La2O3、ZrO2、TiO2、Yb2O3、Nb2O5以及Sb2O5或Sb2O3为原料;球磨混合均匀后煅烧;然后进行二次球磨,造粒压制成坯体;经排胶烧结后得到锆钛酸镧铅基压电陶瓷。
Description
技术领域
本发明属于压电陶瓷材料技术领域,具体涉及一种锆钛酸镧铅基压电陶瓷及其制备方法与应用。
背景技术
压电材料是能将机械能和电能相互转换的功能材料。随着科学的进步,电子整机的不断小型化,驱动电压的不断降低,使得人们对压电材料性能的要求越来越高。比如:在同样的力(或电场)作用下要获得较大的电信号(或应变),需要提高压电电荷系数d33。这类具有较大压电常数的压电材料在电声器件、传感器、制动器和医用超声成像换能器等方面都有广泛的应用需求。
压电性与结构和相不稳定性形成平滑自由能曲线密切相关,因而提高压电性可以通过软性添加改性、寻找准同型相界、引入弛豫结构等方法实现。目前高压电电荷系数铁电陶瓷的研究主要集中于具有钙钛矿结构铅基弛豫铁电体。钙钛矿结构驰豫铁电体可以分成两类:B位驰豫铁电体和A位驰豫铁电体。目前广泛研究的是B位驰豫铁电体,如铌镁酸铅-钛酸铅(PMN-PT)和铌锌酸铅-钛酸铅(PZT-PT),最大压电电荷系数d33可达1500pC/N。然而,A位驰豫铁电体的压电电荷系数d33却不高,如锆钛酸镧铅(PLZT)最大的报道值不超过500pC/N。近年来,本课题组对PLZT进行了研究(Temperature dependence of the ferroelectricproperties of PLZT 6/58/42ceramics with Sb2O5 addition,Ferroelectrics,488:1-5,2015;High piezoelectricity of PLZT ceramics with strong frequency dielectricdispersion below depolarization temperature,Journal of Alloys and Compounds,727:925-930,2017),通过引入Sb2O5或Sb2O3使压电电荷系数d33达到821pC/N,但相比PMN-PT基压电陶瓷d33还是较低。
发明内容
为解决现有技术的缺点和不足之处,本发明的首要目的在于提供一种锆钛酸镧铅基压电陶瓷,该压电陶瓷进一步提升了PLZT基压电陶瓷的压电电荷系数。
本发明的另一目的在于提供上述一种锆钛酸镧铅基压电陶瓷的制备方法。
本发明的再一目的在于提供上述锆钛酸镧铅基压电陶瓷的应用。
本发明目的通过以下技术方案实现:
一种锆钛酸镧铅基压电陶瓷,其组成为:Pb1-xLax(ZryTi1-y)1-x/4O3+a Pb(Yb0.5Nb0.5)O3+b N,其中,N为Sb2O5或Sb2O3,x=0.055~0.070,y=0.55~0.61,以Pb1-xLax(ZryTi1-y)1-x/ 4O3总重为百分比,a为0.8~1.2%,b为0.8~1.2%。
上述一种锆钛酸镧铅基压电陶瓷的制备方法,包括以下步骤:
(1)将Pb3O4、Yb2O3、Nb2O5按化学计量比Pb(Yb0.5Nb0.5)O3配料,球磨混合均匀,烘干,过筛,煅烧,得到Pb(Yb0.5Nb0.5)O3粉体;
(2)将Pb3O4、La2O3、ZrO2和TiO2按照化学计量比Pb1-xLax(ZryTi1-y)1-x/4O3配料,再加入0.8~1.2wt%Pb(Yb0.5Nb0.5)O3以及0.8~1.2wt%Sb2O5或Sb2O3,球磨混合均匀,烘干,过筛,煅烧,得到粉体;
(3)将粉体再次球磨混合均匀,干燥,然后加入粘结剂研磨造粒,过筛,压片,得到坯体;
(4)将坯体排胶处理,然后在1250~1290℃保温2~2.5h,烧结成陶瓷片,涂覆银浆,烧银,极化,得到锆钛酸镧铅基压电陶瓷。
优选的,步骤(1)~(3)所述球磨混合均匀均指湿法球磨。
优选的,步骤(1)所述球磨混合均匀的条件为:以去离子水为溶剂,锆球为球磨介质,其中锆球、去离子水和粉体的质量比为2:1:1,300~350r/min下球磨1.5~3.0h。
优选的,步骤(1)所述烘干的条件为:100~150℃下保温8~12h。
优选的,步骤(1)所述过筛指过60~100目筛。
优选的,步骤(1)所述煅烧的条件为:在850~950℃煅烧3.5~4.5h。
优选的,步骤(2)所述球磨混合均匀的条件为:以去离子水为溶剂,锆球为球磨介质,其中锆球、去离子水和粉体的质量比为2:1:1,300~350r/min下球磨1.5~3.0h。
优选的,步骤(2)所述烘干的条件为:100~150℃下保温8~12h。
优选的,步骤(2)所述过筛指过60~100目筛。
优选的,步骤(2)所述煅烧的条件为:在850~950℃煅烧3.5~4.5h。
优选的,步骤(3)所述球磨混合均匀的条件为:以去离子水为溶剂,锆球为球磨介质,其中锆球、去离子水和粉体的质量比为2:1:1,300~350r/min下球磨1.5~3.0h。
优选的,步骤(3)所述烘干的条件为:100~150℃下保温8~12h。
优选的,步骤(3)所述粘结剂为聚乙烯醇(PVA),所述粘结剂的加入量占粉体质量的1.0~1.5%。
优选的,步骤(3)所述过筛指过60~80目筛。
优选的,步骤(3)所述压片的条件为:24~26MPa下保压20~30s。
优选的,步骤(3)所述胚体为直径为25mm,厚度为1.1~1.7mm的圆片。
优选的,步骤(4)所述排胶处理为:依次在120~150℃、250~300℃,450~500℃和750~800℃保温1~1.5h。
优选的,步骤(4)所述烧银的条件为:600~800℃下烧结15~30min。
优选的,步骤(4)所述极化指在常温硅油中于2~3kV/mm的电场下极化10~30min。
上述一种锆钛酸镧铅基压电陶瓷的应用。
优选在换能器电子器件领域中的应用。
与现有技术相比,本发明具有以下优点及有益效果:
本发明提供一种锆钛酸镧铅基压电陶瓷的制备方法,使用固相反应法,通过成分设计引入Pb(Yb0.5Nb0.5)O3,由于Pb(Yb0.5Nb0.5)O3的加入,其加入量的增加使得矫顽场降低,电畴运动容易,进一步提升了压电电荷系数d33,最高可达930pC/N。本发明方法简单,可重复性好,所得材料压电性能优异,可能成为超声换能器等领域一个有希望的替代体系。
附图说明
图1为实施例1-3和对比例1中制备陶瓷的X射线衍射图谱。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。
本发明实施例中未注明具体条件者,按照常规条件或者制造商建议的条件进行。所用未注明生产厂商者的原料、试剂等,均为可以通过市售购买获得的常规产品。
本申请实施例和对比例中所加入Pb(Yb0.5Nb0.5)O3和Sb2O5的质量百分比均以Pb1- xLax(ZryTi1-y)1-x/4O3总重为百分比算,即占Pb1-xLax(ZryTi1-y)1-x/4O3总重的质量百分比。
对比例1
步骤1,将Pb3O4、La2O3、ZrO2和TiO2按照化学计量比为Pb0.935La0.065(Zr0.59Ti0.41)0.98375O3称量,再加入0.3wt%的Pb3O4(补偿铅在高温环境的挥发)和1.0wt%的Sb2O5,以去离子水为溶剂,锆球为球磨介质进行行星球磨,其中锆球、去离子水和粉料的质量比为2:1:1,转速为300r/min,球磨时间为1.5h,取出浆料在130℃下干燥10h后研磨过80目筛,然后在900℃下煅烧4h。
步骤2,以去离子水为溶剂,锆球为球磨介质,将步骤1煅烧后的粉体进行二次球磨,其中锆球、去离子水和粉料的质量比为2:1:1,转速为300r/min,球磨时间为1.5h,取出在130℃下干燥10h浆料,然后加入10wt%的聚乙烯醇(PVA)溶液(水为溶剂,质量溶度为10%)研磨造粒,经60目筛网过筛后,在粉末压片机中,加压至24MPa,并保压20s制备成直径为25mm,厚度为1.7mm的圆片。
步骤3,将步骤2制得的坯体进行排胶处理,依次在120℃,250℃,450℃,750℃保温1h,然后在1290℃密闭刚玉坩埚中保温2h,烧结成陶瓷片,对陶瓷片进行打磨并用无水乙醇洗涤,在其表面涂覆银浆,在750℃下烧银15min,然后在室温硅油中于2kV/mm的电场下极化30min,得到锆钛酸镧铅基压电陶瓷。
图1(a)是Pb0.935La0.065(Zr0.59Ti0.41)0.98375O3+1.0wt%Sb2O5陶瓷块体的X射线衍射图谱,样品呈单一的钙钛矿相,无第二相出现。
对比例2
步骤1,将Pb3O4、La2O3、ZrO2、TiO2、Yb2O3和Nb2O5按照化学计量比为0.04Pb(Yb0.5Nb0.5)O3-0.96Pb0.935La0.065(Zr0.59Ti0.41)0.98375O3称量,再加入0.3wt%的Pb3O4(补偿铅在高温环境的挥发)和1.0wt%的Sb2O5,以去离子水为溶剂,锆球为球磨介质进行行星球磨,其中锆球、去离子水和粉料的质量比为2:1:1,转速为300r/min,球磨时间为1.5h,取出浆料在130℃下干燥10h后研磨过80目筛,然后在900℃下煅烧4h。
步骤2,以去离子水为溶剂,锆球为球磨介质,将步骤1煅烧后的粉体进行二次球磨,其中锆球、去离子水和粉料的质量比为2:1:1,转速为300r/min,球磨时间为1.5h,取出在130℃下干燥10h,然后加入10wt%的聚乙烯醇(PVA)溶液(水为溶剂,质量溶度为10%)研磨造粒,经60目筛网过筛后,在粉末压片机中,加压至24MPa,并保压20s制备成直径为25mm,厚度为1.7mm的圆片。
步骤3,将步骤2制得的坯体进行排胶处理,依次在120℃,250℃,450℃,750℃保温1h,然后在1290℃密闭刚玉坩埚中保温2h,烧结成陶瓷片,对陶瓷片进行打磨并用无水乙醇洗涤,在其表面涂覆银浆,在750℃下烧银15min,然后在室温硅油中于2kV/mm的电场下极化30min,得到锆钛酸镧铅基压电陶瓷。
实施例1
步骤1,Pb3O4、Yb2O3、Nb2O5为原料,按化学计量比Pb(Yb0.5Nb0.5)O3配料,以去离子水为溶剂,锆球为球磨介质进行行星球磨,其中锆球、去离子水和粉料的质量比为2:1:1,转速为300r/min,球磨时间为1.5h,取出浆料在130℃下干燥10h后研磨过80目筛,然后在900℃下煅烧4h得到Pb(Yb0.5Nb0.5)O3粉体。
步骤2,将Pb3O4、La2O3、ZrO2和TiO2按照化学计量比为Pb0.935La0.065(Zr0.59Ti0.41)0.98375O3称量,再加入0.3wt%的Pb3O4(补偿铅在高温环境的挥发),0.8wt%的Pb(Yb0.5Nb0.5)O3,1.0wt%的Sb2O5,以去离子水为溶剂,锆球为球磨介质进行行星球磨,其中锆球、去离子水和粉料的质量比为2:1:1,转速为300r/min,球磨时间为1.5h,取出浆料在130℃下干燥10h后研磨过80目筛,然后在900℃下煅烧4h。
步骤3,将步骤2煅烧后的粉体进行二次球磨,以去离子水为溶剂,锆球为球磨介质,其中锆球、去离子水和粉料的质量比为2:1:1,转速为300r/min,球磨时间为1.5h,取出并在130℃下干燥10h,然后加入10wt%的聚乙烯醇(PVA)溶液(水为溶剂,质量溶度为10%)研磨造粒,经60目筛网过筛后,在粉末压片机中,加压至24MPa,并保压20s制备成直径为25mm,厚度为1.7mm的圆片。
步骤4,将步骤3制得的坯体进行排胶处理,依次在120℃,250℃,450℃,750℃保温1h,然后在1290℃密闭刚玉坩埚中保温2h,烧结成陶瓷片,对陶瓷片进行打磨并用无水乙醇洗涤,在其表面涂覆银浆,在750℃下烧银15min,然后在室温硅油中于2kV/mm的电场下极化30min,得到锆钛酸镧铅基压电陶瓷。
图1(b)是Pb0.935La0.065(Zr0.59Ti0.41)0.98375O3+0.8wt%Pb(Yb0.5Nb0.5)O3+1.0wt%Sb2O5陶瓷块体的X射线衍射图谱,样品呈单一的钙钛矿相,无第二相出现。
实施例2
实施例2与实施例1的区别仅在于:Pb(Yb0.5Nb0.5)O3加入量为1.0wt%。
图1(c)是Pb0.935La0.065(Zr0.59Ti0.41)0.98375O3+1.0wt%Pb(Yb0.5Nb0.5)O3+1.0wt%Sb2O5陶瓷块体的X射线衍射图谱,样品呈单一的钙钛矿相,无第二相出现。
实施例3
实施例3与实施例1的区别仅在于:Pb(Yb0.5Nb0.5)O3加入量为1.2wt%
图1(d)是Pb0.935La0.065(Zr0.59Ti0.41)0.98375O3+1.2wt%Pb(Yb0.5Nb0.5)O3+1.0wt%Sb2O5陶瓷块体的X射线衍射图谱,样品呈单一的钙钛矿相,无第二相出现。
用Agilent E4981A电容仪在室温下测试陶瓷样品的电容C(1kHz)和介电损耗tanδ(1kHz),通过下式计算介电常数εr:
式中:C是电容(F),d是样品厚度(m),A是电极面积(m2),ε0=8.85*10-12F/m。
用Agilent 4294A阻抗分析仪在室温下测试陶瓷样品的径向谐振频率fr、反谐振频率fa、电容C0和谐振阻抗R,通过下式计算机械品质因数Qm:
式中C0是静态电容(F),R是径向谐振频率fr处的等效电阻(Ω)。
采用Radiant铁电特性测试仪观察电滞回线,以1Hz的双向三角波为测试信号。通过测试可得到样品的矫顽场Ec、剩余极化强度Pr等参数。
用ZJ-3型准静态压电系数测试仪测试样品的压电电荷系数d33,锆钛酸镧铅基压电陶瓷的性能测试结果见表1,表中kp分别为平面径向机电耦合系数。
当N为Sb2O5,x=0.065,y=0.59,a=1.0%,b=1.0%时,获得最大压电电荷系数d33(930pC/N)。
表1实施例1~3和对比例1~2所制备锆钛酸镧铅基压电陶瓷的性能参数
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (10)
1.一种锆钛酸镧铅基压电陶瓷,其特征在于,其组成为:Pb1-xLax(ZryTi1-y)1-x/4O3+a Pb(Yb0.5Nb0.5)O3+b N,其中,N为Sb2O5或Sb2O3,x=0.055~0.070,y=0.55~0.61,以Pb1-xLax(ZryTi1-y)1-x/4O3总重为百分比,a为0.8~1.2%,b为0.8~1.2%。
2.权利要求1所述一种锆钛酸镧铅基压电陶瓷的制备方法,其特征在于,包括以下步骤:
(1)将Pb3O4、Yb2O3、Nb2O5按化学计量比Pb(Yb0.5Nb0.5)O3配料,球磨混合均匀,烘干,过筛,煅烧,得到Pb(Yb0.5Nb0.5)O3粉体;
(2)将Pb3O4、La2O3、ZrO2和TiO2按照化学计量比Pb1-xLax(ZryTi1-y)1-x/4O3配料,再加入0.8~1.2wt%Pb(Yb0.5Nb0.5)O3以及0.8~1.2wt%Sb2O5或Sb2O3,球磨混合均匀,烘干,过筛,煅烧,得到粉体;
(3)将粉体再次球磨混合均匀,干燥,然后加入粘结剂研磨造粒,过筛,压片,得到坯体;
(4)将坯体排胶处理,然后在1250~1290℃保温2~2.5h,烧结成陶瓷片,涂覆银浆,烧银,极化,得到锆钛酸镧铅基压电陶瓷。
3.根据权利要求2所述一种锆钛酸镧铅基压电陶瓷的制备方法,其特征在于,步骤(1)和(2)所述煅烧的条件均为:在850~950℃煅烧3.5~4.5h。
4.根据权利要求2所述一种锆钛酸镧铅基压电陶瓷的制备方法,其特征在于,步骤(3)所述粘结剂为聚乙烯醇,所述粘结剂的加入量占粉体质量的1.0~1.5%。
5.根据权利要求2或3或4所述一种锆钛酸镧铅基压电陶瓷的制备方法,其特征在于,步骤(1)~(3)所述球磨混合均匀的条件均为:以去离子水为溶剂,锆球为球磨介质,其中锆球、去离子水和粉体的质量比为2:1:1,300~350r/min下球磨1.5~3h;
步骤(3)所述压片的条件为:24~26MPa下保压20~30s。
6.根据权利要求5所述一种锆钛酸镧铅基压电陶瓷的制备方法,其特征在于,步骤(1)和(2)所述过筛均指过60~100目筛;步骤(3)所述过筛指过60~80目筛。
7.根据权利要求5所述一种锆钛酸镧铅基压电陶瓷的制备方法,其特征在于,步骤(4)所述烧银的条件为:600~800℃下烧结15~30min;所述极化指在常温硅油中于2~3kV/mm的电场下极化10~30min。
8.根据权利要求5所述一种锆钛酸镧铅基压电陶瓷的制备方法,其特征在于,步骤(1)~(3)所述烘干的条件均为100~150℃下保温8~12h;步骤(4)所述排胶处理为依次在120~150℃,250~300℃,450~500℃,750~800℃保温1~1.5h。
9.权利要求1所述一种锆钛酸镧铅基压电陶瓷的应用。
10.根据权利要求9所述一种锆钛酸镧铅基压电陶瓷的应用,其特征在于,在换能器电子器件领域中的应用。
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