CN107324803A - 一种共沉淀制备锆钛酸钡钙无铅压电陶瓷材料的方法 - Google Patents
一种共沉淀制备锆钛酸钡钙无铅压电陶瓷材料的方法 Download PDFInfo
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Abstract
本发明公开了一种共沉淀制备锆钛酸钡钙无铅压电陶瓷材料的方法,该方法以醋酸钡、醋酸钙、硝酸锆、四氯化钛为原料,氢氧化钠或氢氧化钾为沉淀剂,先制备高纯度、颗粒均一、活性较高的锆钛酸钡钙前驱粉体,然后将前驱粉体经过预烧、造粒、压片、排胶、烧结,得到锆钛酸钡钙无铅压电陶瓷材料。本发明采用共沉淀法制备陶瓷材料的预烧粉,不仅工艺简单,成本廉价,而且整个过程中不易引入杂质,制备的预烧粉纯度高、分散均匀、形貌均一,且活性比较高,降低了预烧温度,同时还能降低陶瓷材料的烧结温度,解决了传统固相法机械混合不均匀、易引入杂质、合成温度高等问题。
Description
技术领域
本发明属于陶瓷材料技术领域,具体涉及到一种高纯度、颗粒均一、活性较高的锆钛酸钡钙无铅压电陶瓷材料的制备方法。
背景技术
BaTiO3(BT)是最早研究的一类无铅压电陶瓷材料,在PbZrO3-PbTiO3被发现之前曾得到广泛的应用,但是由于其居里温度和压电性能均较低,因此限制了它的使用。近十年来,人们在以BaTiO3为基础,通过离子取代、添加新组元、改进制备工艺的方法对BT材料进行探索,使陶瓷材料作为压电材料,取得了重要的研究进展。2009年,BT基压电陶瓷的发展再次取得了重要突破,(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3(BCZT)被成功制备,并在其MPB处测得压电系数d33高达620pC/N,压电性可与铅基相媲美。
BCZT陶瓷材料作为一种有代表性的无铅压铁电材料,在MLCC应用方面有着举足轻重的作用。BCZT陶瓷材料通常采用固相法制备,最大的问题就是预烧温度(相关文献报道的预烧温度大都在1250℃以上)和烧结温度(1450℃~1500℃)高。除此之外,在固相法制备的过程中存在易引入杂质以及组分偏离的问题,而且得到的粉体分散性不好,这直接影响着陶瓷颗粒的均一性及陶瓷的性能。为了避免上述问题,越来越多的学者开始研究湿化学法,目的是在低温下制备出高纯、均一的BCZT粉体。其中就有关于水热法合成BCZT陶瓷材料的报道,相比于固相法,反应温度明显降低,可在300℃以下直接得到所需粉体,但是水热法存在反应条件苛刻、操作困难、反应具有一定的危险性等缺点。
发明内容
本发明所要解决的技术问题在于克服现有BCZT陶瓷材料制备方法存在的缺点,为BCZT无铅压电陶瓷材料提供一种预烧温度和烧结温度较低且陶瓷粉体形貌均一、分散程度好的制备方法。
解决上述技术问题所采用的技术方案由下述步骤组成:
1、将醋酸钡与醋酸钙按摩尔比为85:15完全溶解于蒸馏水中,得到A位前驱液;将硝酸锆与四氯化钛按摩尔比为1:9完全溶解于蒸馏水中,得到B位前驱液;然后按照醋酸钡、醋酸钙的总摩尔量与硝酸锆、四氯化钛的总摩尔量之比为1.2~1.3:1,先将B位前驱液逐滴加到6~10mol/L沉淀剂的水溶液中,常温充分搅拌均匀,然后逐滴加入A位前驱液,滴加完后常温搅拌均匀,再升温至75~95℃,恒温搅拌反应3~5小时,反应完后常温陈化12~24小时,用去离子水离心洗涤至上清液为中性,抽滤,滤饼经干燥、研磨后,得到前驱粉体。
2、将前驱粉体置于氧化铝坩埚内,用玛瑙棒轻轻压实,加盖,在850~950℃保温3~5小时进行预烧,预烧完后冷却至室温,得到(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3预烧粉。
3、将(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3预烧粉进行造粒、压片、排胶后,在1240~1400℃下恒温烧结4~7小时,得到锆钛酸钡钙无铅压电陶瓷材料。
上述步骤1中,所述的沉淀剂为KOH或NaOH,优选沉淀剂的摩尔量为醋酸钡、醋酸钙、硝酸锆、四氯化钛总摩尔量的26~43倍。
上述步骤2中,优选在900℃保温4小时进行预烧。
上述步骤3中,优选在1320℃下恒温烧结6小时。
本发明采用共沉淀法制备BCZT陶瓷材料的预烧粉,不仅工艺简单,成本廉价,而且整个过程中不易引入杂质,制备的预烧粉纯度高、分散均匀、形貌均一,且活性比较高,降低了预烧温度,同时还能降低陶瓷材料的烧结温度,解决了传统固相法机械混合不均匀、易引入杂质导致产物纯度不高、粉体活性不高以及合成温度高等问题。
附图说明
图1是实施例1和2以及对比例1和2制备的预烧粉的XRD图。
图2是实施例1制备的预烧粉的SEM图。
图3是实施例1制备的预烧粉的TEM图。
图4是对比例1烧结后所得材料的SEM图。
图5是实施例1制备的锆钛酸钡钙无铅压电陶瓷材料的SEM图。
图6是实施例2制备的锆钛酸钡钙无铅压电陶瓷材料的SEM图。
图7是对比例2制备的陶瓷材料的SEM图。
图8是实施例1和2制备的锆钛酸钡钙无铅压电陶瓷材料以及对比例2制备的陶瓷材料在10kHz的介电常数随温度的变化关系图。
图9是实施例1和2制备的锆钛酸钡钙无铅压电陶瓷材料以及对比例2制备的陶瓷材料在30kV/cm的电滞回线图。
图10是实施例1制备的锆钛酸钡钙无铅压电陶瓷材料在70kV/cm的电滞回线图。
具体实施方式
为更好地理解本发明,下面结合附图和实施例对本发明进一步详细说明,但本发明的保护范围不仅限于这些实施例。
实施例1
1、将2.7941g(10.83mmol)纯度为99%的Ba(CH3COO)2、0.3416g(1.9mmol)纯度为98%的Ca(CH3COO)2·H2O完全溶解于100mL蒸馏水中,得到A位前驱液;将0.4316g(1mmol)纯度为99%的Zr(NO3)4·5H2O、1.7420g(9mmol)TiCl4完全溶解于100mL蒸馏水中,得到B位前驱液;将B位前驱液逐滴滴加到100mL8mol/L NaOH水溶液中,常温充分搅拌均匀,然后逐滴加入A位前驱液,滴加完后常温搅拌均匀,再升温至90℃,恒温搅拌反应4小时,反应完后常温陈化24小时,用去离子水离心洗涤至上清液为中性,抽滤,滤饼在60℃干燥后,用研钵研磨,过160目筛,得到前驱粉体。
2、将步骤1所得前驱粉体置于氧化铝坩埚内,用玛瑙棒轻轻压实,加盖,在900℃保温4小时进行预烧,预烧完后自然冷却至室温,用研钵研磨,过160目筛,得到(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3预烧粉。
3、向(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3预烧粉中加入质量分数为5%聚乙烯醇水溶液,聚乙烯醇水溶液的加入量为预烧粉质量的50%,造粒,过120目筛,制成球状粉粒;将球状粉粒放入直径为11.5mm的不锈钢模具内,用60MPa的压力将其压制成圆柱状坯件;将圆柱状坯件放在氧化锆平板上并置于氧化铝密闭匣钵中,用380分钟升温至500℃,保温2小时,自然冷却到室温;将圆柱状坯件以10℃/分钟的升温速率升温至1000℃,再以3℃/分钟的升温速率升温至1320℃,恒温烧结6小时,然后以2℃/分钟的降温速率降至室温,得到锆钛酸钡钙无铅压电陶瓷材料。
实施例2
本实施例的步骤1中,将2.6471g(10.2mmol)纯度为99%的Ba(CH3COO)2、0.3236g(1.8mmol)纯度为98%的Ca(CH3COO)2·H2O完全溶解于100mL蒸馏水中,得到A位前驱液;将0.4316g(1mmol)纯度为99%的Zr(NO3)4·5H2O、1.7420g(9mmol)TiCl4完全溶解于100mL蒸馏水中,得到B位前驱液;其他步骤与实施例1相同,得到锆钛酸钡钙无铅压电陶瓷材料。
对比例1
将2.1930g(8.5mmol)纯度为99%的Ba(CH3COO)2、0.2697g(1.5mmol)纯度为98%的Ca(CH3COO)2·H2O完全溶解于100mL蒸馏水中,得到A位前驱液;将0.4316g(1mmol)纯度为99%的Zr(NO3)4·5H2O、1.7420g(9mmol)TiCl4完全溶解于100mL蒸馏水中,得到B位前驱液;该步骤的其他步骤与实施例1的步骤1相同,得到前驱粉体。将所得前驱粉体按照实施例1的方法进行预烧、造粒、压片、排胶、烧结,发现烧结后样品不能成瓷。
对比例2
将3.0883g(12mmol)纯度为99%的Ba(CH3COO)2、0.3775g(2.1mmol)纯度为98%的Ca(CH3COO)2·H2O完全溶解于100mL蒸馏水中,得到A位前驱液;将0.4316g(1mmol)纯度为99%的Zr(NO3)4·5H2O、1.7420g(9mmol)TiCl4完全溶解于100mL蒸馏水中,得到B位前驱液;其他步骤与实施例1相同,制备成陶瓷材料。
分别采取X-射线衍射仪和扫描电镜、透射电镜对实施例1和2以及对比例1和2得到的预烧粉和陶瓷材料进行表征,结果见图1~7。由图1可见,所得预烧粉均为纯钙钛矿结构,且无第二相存在。由图2和3可见,所得预烧粉均为完整的单个晶粒,且分散性较好,晶粒间界限分明,晶粒呈球形、大小均一,粒径在500nm左右。在对比例1中,采用共沉淀法,完全按照(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3的化学计量比无法制备成陶瓷材料,所得样品无法观察到完整的晶粒(见图4);在实施例1和2中,醋酸钡、醋酸钙的总摩尔量与硝酸锆、四氯化钛的总摩尔量之比为1.2:1和1.3:1时,所得陶瓷材料呈现致密且大小均匀性好的微观形貌,陶瓷致密且颗粒大小均匀性好,陶瓷晶粒尺寸在10μm左右(见图5和6),通过EDS能谱验证得出实施例1和2所制备的陶瓷材料符合(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3化学计量比;而对比例2中,醋酸钡、醋酸钙的总摩尔量与硝酸锆、四氯化钛的总摩尔量之比为1.4:1时,所得陶瓷材料不符合(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3化学计量比且呈现出异常的陶瓷晶粒(见图7)。
将实施例1和2制备的锆钛酸钡钙无铅压电陶瓷材料以及对比例2制备的陶瓷材料分别选取其中一个样品表面依次用320目、800目、1500目的砂纸抛光至0.4~0.6mm厚,然后在陶瓷上下表面分别涂覆厚度为0.02mm的银浆,置于电阻炉中840℃保温30分钟,采用LCR测试仪对其介电性能进行测试,结果见图8~10。从图8~10可见,对比例2制备的陶瓷材料的居里温度严重偏离现有文献报道的(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3陶瓷材料的居里温度(93℃左右)且电滞回线不饱和,而本发明实施例1和2制备的陶瓷材料的居里温度与文献报道基本相同,且陶瓷呈现饱和的电滞回线,其中实施例1制备的陶瓷材料的最大介电常数为9250、居里温度为95℃、剩余极化强度为5.59μC/cm2、矫顽场为2.74kV/cm、储能密度为0.17J/cm3、储能效率为61%,经测试该陶瓷的压电常数为200pC/N。
Claims (5)
1.一种共沉淀制备锆钛酸钡钙无铅压电陶瓷材料的方法,所述陶瓷材料的化学式为(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3,其特征在于该陶瓷材料的制备方法由下述步骤组成:
(1)将醋酸钡与醋酸钙按摩尔比为85:15完全溶解于蒸馏水中,得到A位前驱液;将硝酸锆与四氯化钛按摩尔比为1:9完全溶解于蒸馏水中,得到B位前驱液;然后按照醋酸钡、醋酸钙的总摩尔量与硝酸锆、四氯化钛的总摩尔量之比为1.2~1.3:1,先将B位前驱液逐滴加到6~10mol/L沉淀剂的水溶液中,常温充分搅拌均匀,然后逐滴加入A位前驱液,滴加完后常温搅拌均匀,再升温至75~95℃,恒温搅拌反应3~5小时,反应完后常温陈化12~24小时,用去离子水离心洗涤至上清液为中性,抽滤,滤饼经干燥、研磨后,得到前驱粉体;
(2)将前驱粉体置于氧化铝坩埚内,用玛瑙棒轻轻压实,加盖,在850~950℃保温3~5小时进行预烧,预烧完后冷却至室温,得到(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3预烧粉;
(3)将(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3预烧粉进行造粒、压片、排胶后,在1240~1400℃下恒温烧结4~7小时,得到锆钛酸钡钙无铅压电陶瓷材料。
2.根据权利要求1所述的共沉淀制备锆钛酸钡钙无铅压电陶瓷材料的方法,其特征在于:在步骤(1)中,所述的沉淀剂为氢氧化钠或氢氧化钾。
3.根据权利要求1或2所述的共沉淀制备锆钛酸钡钙无铅压电陶瓷材料的方法,其特征在于:在步骤(1)中,所述沉淀剂的摩尔量为醋酸钡、醋酸钙、硝酸锆、四氯化钛总摩尔量的26~43倍。
4.根据权利要求1所述的共沉淀制备锆钛酸钡钙无铅压电陶瓷材料的方法,其特征在于:所述步骤(2)中,在900℃保温4小时进行预烧。
5.根据权利要求1所述的共沉淀制备锆钛酸钡钙无铅压电陶瓷材料的方法,其特征在于:所述步骤(3)中,在1320℃下恒温烧结6小时。
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