CN105837205A - 一种钛酸铋钠体系无铅压电陶瓷及其制备方法 - Google Patents
一种钛酸铋钠体系无铅压电陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种钛酸铋钠体系无铅压电陶瓷及其制备方法,其原料组分及其摩尔百分比含量为0.96(Bi0.5Na0.44‑xK0.06Lix)TiO3‑0.04BaTiO3,其中x=0.005~0.065。先将Bi2O3、K2CO3、Na2CO3、TiO2、Li2CO3、和Ba2CO3,混合配料,经过球磨、烘干,于850℃预烧,再经过二次球磨、烘干、造粒、成型、排胶后,于1100~1200℃烧结,再经过被银与极化后,制得无铅压电陶瓷。本发明材料的主晶相为钙钛矿结构,在每毫米6.5千伏的电场下存在最大0.37%的应变,具有较好的压电性能,且制备工艺稳定,可重复,具有实用性。该无铅压电陶瓷材料可用于压电打火机、驱动器、传感器等多种领域。
Description
技术领域
本发明属于一种以成分为特征的陶瓷组合物,特别是涉及一种钛酸铋钠体系无铅压电陶瓷及其制备方法。
背景技术
压电陶瓷是一种能够将机械能和电能互相转换的功能陶瓷材料,是一类重要的电功能材料,广泛应用于驱动器、传感器、换能器等多种器件的制作,其应用领域涉及到机械、电子、通讯、精密控制、国防军事等各个方面。
由于铅基压电陶瓷具有大的电致应变特性,因而长久以来含铅电致应变材料在电子信息产品中有着举足轻重的不可替代作用,但Pb的毒性使得该体系陶瓷在生产、使用及废弃过程中,会给人类的生态环境造成严重后果。各主要工业国及我国政府都颁布了相应的法律法规,限制或在不久的将来全面禁止含铅等有害物质在电子信息产品中的使用。因此研究和开发无铅的电致应变材料是一项重要而紧迫的课题。
由于Bi0.5Na0.5TiO3(BNT)基无铅压电陶瓷具有很高的剩余极化强度和较高的居里温度被认为是最有望取代含铅压电陶瓷的候选体系之一。然而纯的BNT陶瓷存在室温下矫顽场强大、漏电流高、化学稳定性差、难以获得致密陶瓷体等不足,为了提高陶瓷的压电性能,添加第二组元进行掺杂改性发展了二元、三元体系,且研究表明其具有比纯BNT体系陶瓷更好的烧结特性和压电性能,获得了良好的电致应变效应。然而,BNT基无铅压电陶瓷的综合压电性能还相对偏低,为了获得更优的电致应变效应,对于钛酸铋钠体系进行Li等价掺杂的研究鲜有报道。
发明内容
本发明的目的,是克服现有技术的缺点和不足,提供一种具有良好的压电性能、烧结性能稳定的钛酸铋钠体系压电陶瓷制备及其制备方法。
本发明通过如下技术方案予以实现。
一种钛酸铋钠体系无铅压电陶瓷,其原料组分及其摩尔百分比含量为0.96(Bi0.5Na0.44-xK0.06Lix)TiO3-0.04BaTiO3,所述x=0.005~0.065。
上述压电陶瓷的制备方法如下:
(1)配料合成
按0.96(Bi0.5Na0.44-xK0.06Lix)TiO3-0.04BaTiO3,其中x=0.005~0.065的化学计量比称取原料Bi2O3、K2CO3、Na2CO3、TiO2、Li2CO3、和Ba2CO3,混合均匀后装入球磨罐中,以无水乙醇和氧化锆球为球磨介质进行球磨,再将球磨后的料浆于80℃烘干;
(2)预烧
将步骤(1)烘干后的粉料放入氧化铝坩埚内,置于马弗炉中于850℃预烧,保温5h,然后自然冷却至室温,再将预烧后的粉料置于球磨机中进行二次球磨,再于80℃烘干;
(3)造粒
将步骤(2)烘干后的粉料在研钵中研细,外加质量百分比含量为5%的聚乙烯醇缩丁醛酒精溶液,充分研磨至粉料呈粒状,得到颗粒均匀的粒料;
(4)成型
采用干压成型,将步骤(3)得到的粒料放入模具内,压制成型为坯体;
(5)排胶
将步骤(4)得到的坯体置于马弗炉中进行排胶,以3℃/min的升温速度从室温升温至600℃,保温排胶5h,然后自然冷却至室温;
(6)烧结
将步骤(5)排胶后的坯片放置在氧化铝片上,坩埚倒扣密封,置于马弗炉中,以5℃/min的升温速率升温至1100~1200℃烧结,保温1~2h,随炉自然冷却至室温,制得无铅压电陶瓷;
(7)被银
将步骤(6)得到的无铅压电陶瓷进行清洁处理后,采用丝网印刷法在其表面涂覆低温银浆,然后在550℃下保温30min制成电极,冷却至室温;
(8)极化
将步骤(7)冷却至室温的压电陶瓷在室温下浸入硅油中进行极化处理,即得到0.96(Bi0.5Na0.44-xK0.06Lix)TiO3-0.04BaTiO3无铅压电陶瓷元件。
所述步骤(1)和步骤(2)的球磨中,其配料:磨球:无水乙醇质量比为2:1:0.5,球磨机转速为800转/分,球磨时间为5h。
所述步骤(4)的模具为直径13mm的不锈钢模具,压制成型的坯体为厚度1mm的圆片状。
所述步骤(4)的成型压力为65~130Mpa。
所述步骤(6)的烧结温度为1160℃~1180℃,保温2h。
所述步骤(8)的极化时间为10~30min,极化电场为2~4kV/mm。
本发明的优点在于,采用钛酸铋钠钾-钛酸钡为基体掺杂制备的钙钛矿体系无铅压电陶瓷,仅包含钙钛矿结构,无杂相出现,随着锂掺杂量的增加,压电陶瓷伴随着铁电相到弛豫相的转变,最优性能的压电陶瓷在每毫米6.5千伏下存在大应变0.37%和小的弥散损耗能,在单极和双极电场下具有高的Smax/Emax,分别为580pm/V和480pm/V。
本发明制备的无铅压电陶瓷生产成本低,压电性能好,是一种具有发展前景的作为致动器或传感器的陶瓷体系。
附图说明
图1是本发明实施例1-4制得的不同组分无铅压电陶瓷的X射线衍射图。
图2是本发明实施例1-4制得的不同组分无铅压电陶瓷单极电致应变曲线。
具体实施方式
下面结合具体实施例和附图对本发明做进一步详细说明。
本发明的一种无铅三元体系压电陶瓷,0.96(Bi0.5Na0.44-xK0.06Lix)TiO3-0.04BaTiO3,其中x=0.005~0.065。
实施例1
(1)配料合成
按0.96(Bi0.5Na0.44-xK0.06Lix)TiO3-0.04BaTiO3,x=0.005的化学计量比称取原料Bi2O3、K2CO3、Na2CO3、TiO2、Li2CO3、和Ba2CO3,混合均匀,装入球磨罐中,以无水乙醇和氧化锆球为球磨介质,在每分钟为800转的转速下球磨5h,再将球磨后的料浆置于烘箱内80℃下烘干;
(2)预烧
将步骤(1)烘干后的粉料放入氧化铝坩埚内,在马弗炉中于850℃预烧,保温5h,然后自然冷却至室温,再将预烧后的粉料置于球磨机中进行二次球磨,即每分钟为800转的转速下球磨5h后得到球磨料浆,再将料浆置于烘箱里80℃烘干;
(3)造粒
将步骤(2)烘干后的粉料在研钵中研细,外加质量百分比为5%的聚乙烯醇缩丁醛(PVB)酒精溶液,充分研磨至粉料呈粒状,得到颗粒均匀的粒料;
(4)成型
采用干压成型,将步骤(3)得到的粒料放入直径为13mm的不锈钢模具内,在100MPa压力下压制成型为厚度为1mm的圆片状坯体;
(5)排胶
将步骤(4)的坯体置于马弗炉中进行排胶,以3℃/min的升温速度从室温升温至600℃,保温排胶5h,然后自然冷却至室温;
(6)烧结
将步骤(5)得到的排胶后的坯体放置在氧化铝片上,坩锅倒扣密封,置于马弗炉中,以5℃/min的升温速率升温至1180℃烧结,保温2h,随炉自然冷却至室温,制得无铅压电陶瓷;
(7)被银
将步骤(6)得到的无铅压电陶瓷进行清洁处理后,采用丝网印刷法在其表面涂覆低温银浆,然后在550℃下保温30min制成电极,冷却至室温;
(8)极化
将步骤(7)得到的压电陶瓷片在室温下浸入硅油中进行极化处理,极化电场为3kV/mm,极化时间为15min,即得到钛酸铋钠体系压电陶瓷元件。
通过XRD分析本实验制备的压电陶瓷,检测结果如图1所示,表明本实验制备压电陶瓷为单一钙钛矿结构。
检测性能如下:
d33(pC/N) εr tanδ
198 1227 0.031
实施例2
实施例2的原料组成的化学计量比,其中的x=0.025,其它工艺条件与实施例1相同。
通过XRD分析本实验制备的压电陶瓷,表明该压电陶瓷为单一钙钛矿结构。
检测性能如下:
d33(pC/N) εr tanδ
210 1207 0.030
实施例3
实施例3的原料组成的化学计量比,其中的x=0.045,其它工艺条件与实施例1相同。
通过XRD分析本实验制备的压电陶瓷,表明该压电陶瓷为单一钙钛矿结构。
检测性能如下:
d33(pC/N) εr tanδ
205 1347 0.043
实施例4
实施例4的原料组成的化学计量比,其中的x=0.065,其它工艺条件与实施例1相同。
通过XRD分析本实验制备的压电陶瓷,表明该压电陶瓷为单一钙钛矿结构。
检测性能如下:
d33(pC/N) εr tanδ
5 1240 0.050
该压电陶瓷d33值小于实施例1-3,其原因在于该钛酸铋钠体系压电陶瓷随着锂掺杂量的增加产生铁电相到弛豫相的转变,实施例4压电陶瓷弛豫相占主导地位。因此该压电陶瓷能在电场下产生更大的应变响应。
图2为本实验制备无铅压电陶瓷实施例1-4的单极电致应变曲线。在每毫米5.5千伏的电场下,实施例1-3产生0.18~0.19%的应变。实施例4存在优于实施例1-3的应变,为0.28%,该压电陶瓷在每毫米6.5千伏的电场下存在0.37%的大应变和小的弥散损耗能。在单极和双极电场下,该压电陶瓷具有高的Smax/Emax值,分别为580pm/V和480pm/V,表明了所得无铅压电陶瓷制品具有较好的压电性能。
该无铅压电陶瓷材料可用于压电打火机、驱动器、传感器等多种领域。
Claims (6)
1.一种钛酸铋钠体系无铅压电陶瓷,其原料组分及其摩尔百分比含量为0.96(Bi0.5Na0.44-xK0.06Lix)TiO3-0.04BaTiO3,所述x=0.005~0.065。
该钛酸铋钠体系无铅压电陶瓷的制备方法,具有如下步骤:
(1)配料合成
按0.96(Bi0.5Na0.44-xK0.06Lix)TiO3-0.04BaTiO3,其中x=0.005~0.065的化学计量比称取原料Bi2O3、K2CO3、Na2CO3、TiO2、Li2CO3、和Ba2CO3,混合均匀后装入球磨罐中,以无水乙醇和氧化锆球为球磨介质进行球磨,再将球磨后的料浆于80℃烘干;
(2)预烧
将步骤(1)烘干后的粉料放入氧化铝坩埚内,置于马弗炉中于850℃预烧,保温5h,然后自然冷却至室温,再将预烧后的粉料置于球磨机中进行二次球磨,再于80℃烘干;
(3)造粒
将步骤(2)烘干后的粉料在研钵中研细,外加质量百分比含量为5%的聚乙烯醇缩丁醛酒精溶液,充分研磨至粉料呈粒状,得到颗粒均匀的粒料;
(4)成型
采用干压成型,将步骤(3)得到的粒料放入模具内,压制成型为坯体;
(5)排胶
将步骤(4)得到的坯体置于马弗炉中进行排胶,以3℃/min的升温速度从室温升温至600℃,保温排胶5h,然后自然冷却至室温;
(6)烧结
将步骤(5)排胶后的坯体放置在氧化铝片上,坩锅倒扣密封,置于马弗炉中,以5℃/min的升温速率升温至1100~1200℃烧结,保温1~2h,随炉自然冷却至室温,制得无铅压电陶瓷;
(7)被银
将步骤(6)得到的无铅压电陶瓷进行清洁处理后,采用丝网印刷法在其表面涂覆低温银浆,然后在550℃下保温30min制成电极,冷却至室温;
(8)极化
将步骤(7)冷却至室温的压电陶瓷在室温下浸入硅油中进行极化处理,即得到0.96(Bi0.5Na0.44-xK0.06Lix)TiO3-0.04BaTiO3无铅压电陶瓷元件。
2.根据权利要求1所述的一种钛酸铋钠体系无铅压电陶瓷,其特征在于,所述步骤(1)和步骤(2)的球磨中,其配料:磨球:无水乙醇质量比为2:1:0.5,球磨机转速为800转/分,球磨时间为5h。
3.根据权利要求1所述的一种钛酸铋钠体系无铅压电陶瓷,其特征在于,所述步骤(4)的模具为直径13mm的不锈钢模具,压制成型的坯体为厚度1mm的圆片状。
4.根据权利要求1所述的一种钛酸铋钠体系无铅压电陶瓷,其特征在于,所述步骤(4)的成型压力为65~130Mpa。
5.根据权利要求1所述的一种钛酸铋钠体系无铅压电陶瓷,其特征在于,所述步骤(6)的烧结温度为1160℃~1180℃,保温2h。
6.根据权利要求1所述的一种钛酸铋钠体系无铅压电陶瓷,其特征在于,所述步骤(8)的极化时间为10~30min,极化电场为2~4kV/mm。
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