CN106007706A - 一种高性能钛酸铋钠基无铅压电陶瓷及其制备方法 - Google Patents
一种高性能钛酸铋钠基无铅压电陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种高性能钛酸铋钠基无铅压电陶瓷,原料组分及其摩尔百分比含量为0.91(NaBi)0.5TiO3‑0.06BaTiO3‑0.03(NaK)0.5NbO3‑yCuO,其中y=0.01~0.04。先按化学式分别配取碳酸钠、碳酸钾、五氧化二铌、三氧化二铋、二氧化钛、碳酸钡和氧化铜,球磨5h,于70℃烘干,再将混合原料于700~900℃预合成,再进行造粒、成型、排胶后于960℃烧结,制得高性能钛酸铋钠基无铅压电陶瓷。本发明既弥补了碱金属丢失,又有效地降低了烧结温,为单一钙钛矿结构,其饱和极化强度Ps为37.25~39.59μC/cm2,应变S为0.267%~0.296%。
Description
技术领域
本发明属于一种以组分为特征的陶瓷组合物,特别涉及一种高性能钛酸铋钠基无铅压电陶瓷及其制备方法。
背景技术
压电陶瓷材料应用遍及社会的各个领域及人们生活的各个方面。目前,应用最广泛的铅基压电陶瓷(PZT),在制备、使用、废弃过程中由于铅的存在对人类及生态环境造成严重的危害,因此研究和开发性能优异的无铅压电陶瓷,意义深远且十分迫切。
目前人们已开发出多种无铅压电陶瓷,BaTiO3是最早发现的典型的无铅压电材料,但由于其居里点低及烧结温度高限制了其应用。钛酸铋钠基无铅压电陶瓷,因其具有大的应变和对生态环境及人类无害,被认为是最有前途取代铅基压电陶瓷的材料之一。现有技术中在0.91BNT-0.06BT-0.03KNN陶瓷的基础上对其进行CuO掺杂,利用传统固相烧结工艺得到了0.267%<S<0.296%的压电陶瓷。但是BNT基压电陶瓷在制备过程中碱金属元素丢失是一个大问题。目前人们大多通过掺杂改性和改进工艺来降低烧结温度以减少碱的挥发,本发明通过结合降低烧结温度和碱的弥补来减少碱的挥发。
发明内容
本发明的目的,是通过掺杂铜离子对0.91BNT-0.06BT-0.03KNN系压电陶瓷的铁电性能的影响,既弥补碱金属的丢失,又达到对烧结温度降低效果,提供一种氧化铜掺杂改性的钛酸铋钠基无铅压电陶瓷材料及其制备方法。
本发明为解决上述技术问题采用的技术方案如下:
一种高性能钛酸铋钠基无铅压电陶瓷,原料组分及其摩尔百分比含量为0.91(NaBi)0.5TiO3-0.06BaTiO3-0.03(NaK)0.5NbO3-yCuO,其中y=0.01~0.04。
上述高性能钛酸铋钠基无铅压电陶瓷的制备方法,具有如下步骤:
(1)按0.91(NaBi)0.5TiO3-0.06BaTiO3-0.03(NaK)0.5NbO3-yCuO,其中y=0.01~0.04的化学式分别配取基本原料碳酸钠、碳酸钾、五氧化二铌、三氧化二铋、二氧化钛、碳酸钡和氧化铜,装入球磨罐中,球磨5h,再将料浆放入烘箱内于70℃烘干;
(2)将步骤(1)的0.91(NaBi)0.5TiO3-0.06BaTiO3-0.03(NaK)0.5NbO3-yCuO混合原料于700~900℃预合成,保温4~6h;
(3)将步骤(2)的预合成原料进行加胶造粒、成型为坯体,再进行排胶;
(4)将步骤(3)排胶后的坯体,于900~1200℃烧结,保温2~4h,制得高性能钛酸铋钠基无铅压电陶瓷。
该钛酸铋钠基无铅压电陶瓷为单一钙钛矿结构。
所述钛酸铋钠基无铅压电陶瓷的饱和极化强度Ps为37.25~39.59μC/cm2,应变S为0.267%~0.296%。
所述步骤(1)的球磨介质为氧化锆球,球磨剂为无水乙醇;原料、无水乙醇和氧化锆球的质量比为1:2:2。
所述步骤(1)的球磨机转速为400转/分。
本发明的有益效果:采用传统的固相合成的方法,添加氧化铜,制备氧化铜掺杂改性的钛酸铋钠基无铅压电陶瓷材料,既弥补了碱金属丢失,又有效地降低了烧结温。本发明的钛酸铋钠基无铅压电陶瓷为单一钙钛矿结构,其饱和极化强度Ps为37.25~39.59μC/cm2,应变S为0.267%~0.296%。
附图说明
图1是本发明实施例1、2、3、4不同组分制品的电致应变图;
图2是本发明实施例1、2、3、4不同组分制品的电滞回线图。
具体实施方式
本发明为弥补碱金属的丢失和降低烧结温度,添加氧化铜,制备掺铜改性的钛酸铋钠基无铅压电陶瓷材料。本发明采用传统固相合成方法,分别按0.91(NaBi)0.5TiO3-0.06BaTiO3-0.03(NaK)0.5NbO3-yCuO,其中y=0~0.04的化学式配比混合,固相烧结制备钛酸铋钠基无铅压电陶瓷。
本发明的原料采用分析纯试剂。
下面结合具体实施例对本发明作进一步描述,但并不局限于下述实施例。
实施例1(对比实施例)
(1)配料合成
按0.91(NaBi)0.5TiO3-0.06BaTiO3-0.03(NaK)0.5NbO3-yCuO(y=0)的化学计量比称取原料碳酸钠、碳酸钾、五氧化二铌、三氧化二铋、二氧化钛、氧化钡和氧化铜,进行混合,装入球磨罐中,球磨介质为无水乙醇和氧化锆球,原料、无水乙醇和氧化锆球的质量比为1:2:2,球磨5h,球磨转速为400转/分,再将料浆放入烘箱内于70℃烘干,得到混合原料;
(2)预烧
将步骤(1)得到的混合原料分别放入坩埚内,加盖,密封,在马弗炉中800℃预烧,保温5h,自然冷却到室温,出炉,得到混合粉料;
(3)二次球磨
将步骤(2)得到的粉料在研钵中研磨,装入球磨罐,球磨介质为无水乙醇和氧化锆球,球磨5h,球磨转速为400转/分,再将料浆放入烘箱于70℃烘干,得到混合粉料;
(4)造粒
将步骤(3)得到的混合粉料在研钵中研细,加入重量浓度为5%的聚乙烯醇缩丁醛(PVB),充分搅拌至粉料呈粒状,得到粒料;
(5)成型
将步骤(4)得到的粒料放入直径为13mm的不锈钢模具内,在6MPa压力下压成圆片状坯件;
(6)排胶
将步骤(5)得到的坯件放入马弗炉中,升温至550℃保温1h进行有机物排除,得到排胶坯件;
(7)烧结
将步骤(6)得到的排胶坯件放置氧化铝片上,坩锅倒扣密封,升温速度为5℃/分钟,至1150℃,保温2h,随炉自然冷却至室温,制得钛酸铋钠基无铅压电陶瓷。
实施例2
采用与实施例1相同的方法,掺杂氧化铜,氧化铜的掺杂量为1%(y=0.01),改变烧结温度为960℃,制得钛酸铋钠基无铅压电陶瓷。
实施例3
采用与实施例1相同的方法,掺杂氧化铜,氧化铜的掺杂量为2%(y=0.02),改变烧结温度为960℃,制得钛酸铋钠基无铅压电陶瓷。
实施例4
采用与实施例1相同的方法,掺杂氧化铜,氧化铜的掺杂量为4%(y=0.04),改变烧结温度为960℃,制得钛酸铋钠基无铅压电陶瓷。
选取本发明制得的钛酸铋钠基无铅压电陶瓷样品,测试不同掺杂下的铁电性能,如附图1、附图2所示。
图1是本发明不同y值的样品的电滞回线(P-E)图,从图1上可以得出掺杂铜离子对0.91BNT-0.06BT-0.03KNN基无铅压电陶瓷的饱和极化强度影响很小,此外铜离子具有增大0.91BNT-0.06BT-0.03KNN基无铅压电陶瓷剩余极化强度的作用。图2是本发明不同y值的样品的电致应变(S-E)图,从S-E图上可以得出掺杂铜离子会稍微降低0.91BNT-0.06BT-0.03KNN基无铅压电陶瓷应变性能,不同的铜离子掺杂量对0.91BNT-0.06BT-0.03KNN基无铅压电陶瓷应变(S)无太大影响。
本发明掺杂铜离子后,其烧结温度由对比实施例的1150℃明显降至960℃,但铁电性能基本无大变化。
Claims (5)
1.一种高性能钛酸铋钠基无铅压电陶瓷,原料组分及其摩尔百分比含量为0.91(NaBi)0.5TiO3-0.06BaTiO3-0.03(NaK)0.5NbO3-yCuO,其中y=0.01~0.04。
上述高性能钛酸铋钠基无铅压电陶瓷的制备方法,具有如下步骤:
(1)按0.91(NaBi)0.5TiO3-0.06BaTiO3-0.03(NaK)0.5NbO3-yCuO,其中y=0.01~0.04的化学式分别配取基本原料碳酸钠、碳酸钾、五氧化二铌、三氧化二铋、二氧化钛、碳酸钡和氧化铜,装入球磨罐中,球磨5h,再将料浆放入烘箱内于70℃烘干;
(2)将步骤(1)的0.91(NaBi)0.5TiO3-0.06BaTiO3-0.03(NaK)0.5NbO3-yCuO混合原料于700~900℃预合成,保温4~6h;
(3)将步骤(2)的预合成原料进行加胶造粒、成型为坯体,再进行排胶;
(4)将步骤(3)排胶后的坯体,于960℃烧结,保温2~4h,制得高性能钛酸铋钠基无铅压电陶瓷。
2.根据权利要求1所述的一种高性能钛酸铋钠基无铅压电陶瓷,其特征在于,该钛酸铋钠基无铅压电陶瓷为单一钙钛矿结构。
3.根据权利要求1所述的一种高性能钛酸铋钠基无铅压电陶瓷,其特征在于,该钛酸铋钠基无铅压电陶瓷的饱和极化强度Ps为37.25~39.59μC/cm2,应变S为0.267%~0.296%。
4.根据权利要求1所述的一种高性能钛酸铋钠基无铅压电陶瓷,其特征在于,所述步骤(1)的球磨介质为氧化锆球,球磨剂为无水乙醇;原料、无水乙醇和氧化锆球的质量比为1:2:2。
5.根据权利要求1所述的一种高性能钛酸铋钠基无铅压电陶瓷,其特征在于,所述步骤(1)的球磨机转速为400转/分。
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CN110963797A (zh) * | 2019-11-22 | 2020-04-07 | 清华大学 | 一种高温巨电致应变陶瓷材料及其制备方法 |
CN111151434A (zh) * | 2020-02-29 | 2020-05-15 | 桐乡清锋科技有限公司 | 低频无铅压电雾化元件 |
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