CN111548146A - 一种二氧化钛基陶瓷及其制备方法 - Google Patents
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Abstract
本发明公开了一种二氧化钛基陶瓷及其制备方法,其特征在于,二氧化钛基陶瓷采用热压工艺制备,其名义化学分子式为(YbaTabNbc)xTi1‑xO2,其中,a=b=c=0.4~0.6,x的取值范围为0.005~0.015。其制备方法包括以下步骤:1)按照名义化学分子式(YbaTabNbc)xTi1‑xO2,称取金红石型TiO2、Yb2O3、Ta2O5和Nb2O5粉体,进行球磨、烘干;2)将烘干的粉体预烧,二次球磨,所得粉体烘干后,在60~70Mpa压强下,温度900~1200℃,热压1‑3h,即可得到超高介电常数低介电损耗的二氧化钛基陶瓷。
Description
技术领域
本发明属于电介质功能材料领域,具体涉及一种二氧化钛基陶瓷及其制备方法。
背景技术
包括5G网络在内的微电子信息技术的迅猛发展,对电子元器件的微型化、集成化和便携化提出了更高的要求。作为电子元器件的重要组成部分,电介质陶瓷的研究受到人们越来越多的关注。具有良好温度和频率稳定性的高介电常数低介电损耗的电介质材料有十分广泛的应用前景,例如通讯行业和全球定位系统中使用的电容器、谐振器、滤波器和信号接收发射天线等,都要用到电介质材料。然而传统的高介电材料依旧存在一些难以克服的缺陷,如CaCu3Ti4O12介电陶瓷,虽然具有超高的介电常数,但介电损耗较大,一般高于0.1。SrTiO3介电陶瓷通过掺杂可以诱发铁电相,在常温下获得高介电常数,但是材料存在铁电-顺电相转变,稳定较性差。
据报道,TiO2陶瓷通过In3+、Nb5+离子共掺杂可以在宽温宽频范围内保持高介电常数,且具有较低的介电损耗。然而在迄今为止的报道中,离子共掺杂TiO2陶瓷的介电性能和掺杂离子种类以及制备工艺有密切关系,因此,离子共掺杂的TiO2陶瓷的介电性能也良莠不齐,在宽频范围内介电常数高于105且介电损耗低于0.05的二氧化钛基陶瓷材料并不多见,依然不能满足电子元器的需求。
CN111205085A公开了一种二氧化钛基陶瓷及其制备方法,其特征在于,二氧化钛基陶瓷采用热压工艺制备,其名义化学分子式为(Lu0.5Nb0.5)xTi1-xO2,其中,x的取值范围是1.0%~2.0%。其制备方法包括以下步骤:1)按照名义化学分子式(Lu0.5Nb0.5)xTi1-xO2,称取金红石型TiO2、Lu2O3和Nb2O5粉体,进行球磨、烘干;2)将烘干的粉体预烧,二次球磨,所得粉体烘干后,在50Mpa压强下,温度1000~1100℃,热压0.5-1h,即可得到超高介电常数低介电损耗的二氧化钛基陶瓷。本发明制备的(Lu0.5Nb0.5)xTi1-xO2陶瓷在宽频范围内,介电常数高于105,介电损耗小于0.03,在温度-130~150℃范围内,介电性能具有良好的温度稳定性。本发明制备温度低、工期短,工艺简单、节能,重复性好,适合推广应用。然而该文献的的介电常数仍较低,而介电损耗仍比较高。
因而,如何提高在20℃ 频率为1Hz时的介电常数并降低介电损耗仍急需解决的问题。
发明内容
针对上述问题。本发明提供了一种二氧化钛基陶瓷及其制备方法。与传统的固相烧结工艺相比,该方法制备的Yb3+、Ta5+和Nb5+离子共掺杂二氧化钛基陶瓷,孔隙度低,质地致密,晶粒大小均一,具有超高介电常数和低介电损耗,并且有良好的温度和频率稳定性。此外,该方法简化了制备工艺步骤,大幅降低了TiO2基陶瓷的烧结温度,缩短了烧结时间,节约能源,适合推广应用。
本发明采用以下技术方案:
一种二氧化钛基陶瓷的制备方法,包含以下步骤:
(1)以金红石型TiO2、Yb2O3、Ta2O5和Nb2O5粉体为原料;
(2)按照名义化学分子式(YbaTabNbc)xTi1-xO2,其中,a=b=c=0.4~0.6,x的取值范围为0.005~0.015,称量原料,采用湿法球磨,球磨介质为无水乙醇,进行球磨;
(3)球磨后的粉体烘干,预煅烧;
(4)将预烧后的粉体进行二次球磨;
(5)二次球磨后的粉体烘干,在玛瑙研钵中研磨,然后装入石墨模具,放置于热压设备中;
(6)热压开始前,打开水冷循环系统,然后将热压设备抽真空至-0.1MPa~-0.05Mpa,接着以8℃~15℃/min的速率升温至900~1200℃,保温10~30min;
(7)随后在该温度下对粉体施加60~70Mpa的压强,并保持1~3h后,卸掉压强,以8℃~15℃/min的速率降温至280℃~420℃,随后关闭加热电源,自然冷却至室温,得到二氧化钛基陶瓷;
(8)将二氧化钛基陶瓷外表层打磨掉,即可得到超高介电常数低介电损耗的二氧化钛基陶瓷。
优选的,所述步骤1)中,配料前将原料在150~250℃烘干20~40h。
优选的,所述步骤2)中,所述球磨时长为25~40h,转速为300~450 r/min,每30min转动换向一次。
优选的,所述步骤3)中,所述烘干的温度为100~150℃,所述预煅烧的条件是在1000~1100℃预煅烧2~6h,升温速率为2~4℃/min。
优选的,所述步骤4)中,所述球磨时长为25~40h,转速为300~450 r/min,每30min转动换向一次。
优选的,所述步骤5)中,所述烘干温度是120~160℃,所述研磨时间为20~40min。
本发明的另一个技术方案是,基于上述制备方法制备的一种二氧化钛基陶瓷。
优选的,在20℃ 频率为1Hz时介电常数为77324~84213,介电损耗为0.013~0.019。
与现有技术相比,本发明的有益效果是:
(1)本发明涉及的一种二氧化钛基陶瓷及其制备方法,采用热压工艺制备,与传统的固相烧结法相比,免除了造粒、排胶等中间环节,简化了制备工艺过程,缩短了制备时间。同时,由于在高压下烧结,显著降低了烧结温度,缩短了烧结时间,因而节省能源,降低了能耗。
(2)更重要的是,与传统固相法烧结制备的二氧化钛基陶瓷相比,本发明制备的二氧化钛基陶瓷孔隙度低,质地更致密,晶粒粒径分布均匀。所制备的陶瓷在宽频范围内,在20℃ 频率为1Hz时介电常数为77324~84213,介电损耗为0.013~0.019,介电性能具有良好的温度稳定性。
(3)更重要的是,通过Yb3+、Ta5+和Nb5+离子之间的协同作用,提高了二氧化钛基陶瓷的介电常数,降低了介电损耗。本发明制备的一种超高介电常数低介电损耗的二氧化钛基陶瓷是实际应用的理想材料。
具体实施方式
本发明的一种二氧化钛基陶瓷及其制备方法,包含以下步骤:
(1)以金红石型TiO2、Yb2O3、Ta2O5和Nb2O5粉体为原料;并将原料在150~ 250℃烘干20~40h。
(2)按照名义化学分子式(YbaTabNbc)xTi1-xO2,其中,a=b=c=0.4~0.6,x的取值范围为0.005~0.015,称量原料,采用湿法球磨,球磨介质为无水乙醇,进行球磨,所述球磨时长为25~40h,转速为300~450 r/min,每30min转动换向一次。
(3)球磨后的粉体在100~150℃下烘干后,在1000~1100℃预煅烧2~6h;升温速率为2~4℃/min。
(4)将预烧后的粉体进行二次球磨;所述球磨时长为25~40h,转速为300~450 r/min,每30min转动换向一次。
(5)二次球磨后的粉体在120~160℃烘干,在玛瑙研钵中研磨20~40min,然后装入石墨模具,放置于热压设备中;
(6)热压开始前,打开水冷循环系统,然后将热压设备抽真空至-0.1MPa~-0.05Mpa,接着以8℃~15℃/min的速率升温至900~1200℃,保温10~30min;
(7)随后在该温度下对粉体施加60~70Mpa的压强,并保持1~3h后,卸掉压强,以8℃~15℃/min的速率降温至280℃~420℃,随后关闭加热电源,自然冷却至室温,得到二氧化钛基陶瓷;
(8)将二氧化钛基陶瓷外表层打磨掉,即可得到超高介电常数低介电损耗的二氧化钛基陶瓷。
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。通常在所示的本发明实施例的组件可以通过各种不同的配置来布置和设计。因此,以下对本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围,而是仅仅表示本发明的选定实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种二氧化钛基陶瓷及其制备方法,包含以下步骤:
(1)以金红石型TiO2、Yb2O3、Ta2O5和Nb2O5粉体为原料;并将原料在150~ 250℃烘干20~40h。
(2)按照名义化学分子式(YbaTabNbc)xTi1-xO2,其中,a=b=c=0.5,x的取值范围为0.01,称量原料,采用湿法球磨,球磨介质为无水乙醇,进行球磨,所述球磨时长为35h,转速为300 r/min,每30min转动换向一次。
(3)球磨后的粉体在150℃下烘干后,在1100℃预煅烧2.5h;升温速率为3℃/min。
(4)将预烧后的粉体进行二次球磨;所述球磨时长为30h,转速为400 r/min,每30min转动换向一次。
(5)二次球磨后的粉体在140℃烘干,在玛瑙研钵中研磨30min,然后装入石墨模具,放置于热压设备中;
(6)热压开始前,打开水冷循环系统,然后将热压设备抽真空至-0.1MPa,接着以10℃/min的速率升温至1100℃,保温25min;
(7)随后在该温度下对粉体施加65Mpa的压强,并保持2h后,卸掉压强,以12℃/min的速率降温至350℃,随后关闭加热电源,自然冷却至室温,得到二氧化钛基陶瓷;
(8)将二氧化钛基陶瓷外表层打磨掉,即可得到超高介电常数低介电损耗的二氧化钛基陶瓷。
实施例2
一种二氧化钛基陶瓷及其制备方法,包含以下步骤:
(1)以金红石型TiO2、Yb2O3、Ta2O5和Nb2O5粉体为原料;并将原料在150℃烘干40h。
(2)按照名义化学分子式(YbaTabNbc)xTi1-xO2,其中,a=b=c=0.4,x的取值范围为0.005,称量原料,采用湿法球磨,球磨介质为无水乙醇,进行球磨,所述球磨时长为40h,转速为300 r/min,每30min转动换向一次。
(3)球磨后的粉体在100℃下烘干后,在1000℃预煅烧6h;升温速率为4℃/min。
(4)将预烧后的粉体进行二次球磨;所述球磨时长为40h,转速为300r/min,每30min转动换向一次。
(5)二次球磨后的粉体在160℃烘干,在玛瑙研钵中研磨40min,然后装入石墨模具,放置于热压设备中;
(6)热压开始前,打开水冷循环系统,然后将热压设备抽真空至-0.05Mpa,接着以8℃/min的速率升温至1200℃,保温20min;
(7)随后在该温度下对粉体施加70Mpa的压强,并保持1.5h后,卸掉压强,以8℃/min的速率降温至300℃,随后关闭加热电源,自然冷却至室温,得到二氧化钛基陶瓷;
(8)将二氧化钛基陶瓷外表层打磨掉,即可得到超高介电常数低介电损耗的二氧化钛基陶瓷。
对照例1-10
对照例1-9的通式为(YbaTabNbc)xTi1-xO2,除a、b、c不同以外,其它制备参数和条件与实施例1相同。对照例10,采用Lu2O3替代对照例2中的Yb2O3,其它制备参数和条件与对照例2相同。实施例1-2和对照例1-10,在20℃,频率1Hz时介电常数和介电损耗如下表所示。
实施例1-2和对照例1-10的介电常数和介电损耗
综上所述,本发明制备的一种超高介电常数低介电损耗的二氧化钛基陶瓷,具有高介电常数,低介电损耗,是一种理想的陶瓷材料。而且通过实施例1与对照例1-9的对比可以发现,Yb3+、Ta5+和Nb5+离子之间具有协同作用,通过同时添加Yb3+、Ta5+和Nb5+能够显著提高二氧化钛基陶瓷的介电常数,降低介电损耗。而且采用Yb3+与Ta5+复合相较于Lu3+,更加能够提高二氧化钛基陶瓷的介电常数,降低介电损耗。
以上内容仅为说明本发明的技术思想,不能以此限定本发明的保护范围,凡是按照本发明提出的技术思想,在技术方案基础上所做的任何改动,均落入本发明权利要求书的保护范围之内。
Claims (7)
1.一种二氧化钛基陶瓷的制备方法,其特征在于,包含以下步骤:
(1)以金红石型TiO2、Yb2O3、Ta2O5和Nb2O5粉体为原料;
(2)按照名义化学分子式(YbaTabNbc)xTi1-xO2,其中,a=b=c=0.4~0.6,x的取值范围为0.005~0.015,称量原料,采用湿法球磨,球磨介质为无水乙醇,进行球磨;
(3)球磨后的粉体烘干,预煅烧;
(4)将预烧后的粉体进行二次球磨;
(5)二次球磨后的粉体烘干,在玛瑙研钵中研磨,然后装入石墨模具,放置于热压设备中;
(6)热压开始前,打开水冷循环系统,然后将热压设备抽真空至-0.1MPa~-0.05Mpa,接着以8℃~15℃/min的速率升温至900~1200℃,保温10~30min;
(7)随后在该温度下对粉体施加60~70Mpa的压强,并保持1~3h后,卸掉压强,以8℃~15℃/min的速率降温至280℃~420℃,随后关闭加热电源,自然冷却至室温,得到二氧化钛基陶瓷;
(8)将二氧化钛基陶瓷外表层打磨掉,即可得到超高介电常数低介电损耗的二氧化钛基陶瓷。
2.根据权利要求1所述的一种二氧化钛基陶瓷的制备方法,其特征在于:在步骤(1)中,配料前将原料在150~250℃烘干20~40h。
3.根据权利要求1所述的一种二氧化钛基陶瓷的制备方法,其特征在于:在步骤(2)中,所述球磨时长为25~40h,转速为300~450 r/min,每30min转动换向一次。
4.根据权利要求3所述的一种二氧化钛基陶瓷的制备方法,其特征在于:在步骤(3)中,所述烘干的温度为100~150℃,所述预煅烧的条件是在1000~1100℃预煅烧2~6h,升温速率为2~4℃/min。
5.根据权利要求2所述的一种二氧化钛基陶瓷的制备方法,其特征在于:在步骤(4)中,所述球磨时长为25~40h,转速为300~450 r/min,每30min转动换向一次。
6.根据权利要求1所述的一种二氧化钛基陶瓷的制备方法,其特征在于:在步骤(5)中,所述烘干温度是120~160℃,所述研磨时间为20~40min。
7.根据权利要求1-6任一项所述的制备方法制备的一种二氧化钛基陶瓷,其特征在于:在20℃ 频率为1Hz时介电常数为77324~84213,介电损耗为0.013~0.019。
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