CN110451950A - 一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法 - Google Patents
一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法 Download PDFInfo
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Abstract
本发明公开了一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法,先按摩尔比TiO2:Ta2O5:Eu2O3=97:0.015:0.015进行配料,经过球磨、烘干、过筛后进行造粒,再压制成坯体,排胶后于1400~1450℃烧结,制成二氧化钛基电介质陶瓷材料;再利用直流磁控溅射方法,制备出具有超宽温度范围巨介电常数低损耗的二氧化钛基电介质陶瓷材料。本发明具有优良的介电性能,介电常数ε25℃为1553219,介电损耗tanσ为0.4293,开发出能满足当今小型化MLCC制备与应用要求的电介质陶瓷材料。
Description
技术领域
本发明属于一种以成分为特征的陶瓷组合物,具体涉及一种具有巨介电常数的二氧化钛基电介质陶瓷材料及其制备与改性方法。(介电常数大于10000即ε>104,称之为“巨介电常数”)
背景技术
目前,全球微电子行业正向微型化、高集成化、大容量化、低功耗等方向发展。对电子元器件提出更小的体积空间以及更好的存储能力的要求。高储能、微型化电容器的制备关键在于实现填充的介质材料具有非常高的介电常数,传统的介质材料已经不能满足对应的性能要求。
目前高介电常数瓷料在电子器件电容器小型化方面具有广泛的应用前景,由于受材料本身性能的制约,只改变烧结温度与压片工艺很难制备出满足要求的介质材料。为了制备出满器件小型化要求的高介电常数介质瓷料,选择二氧化钛作为基体材料进行研究。
发明内容
本发明的目的,在于通过Eu元素与Ta元素共掺杂,并在此基础上利用直流磁控溅射的方式,改性材料本性的介电性能,进一步提高材料的介电常数。采用传统固相反应方法以及磁控溅射改性方法,提供具有巨介电常数的TiO2基电介质陶瓷材料及其制备与改性方法,以期望开发出能满足当今小型化MLCC制备与应用要求的材料。
本发明通过如下技术方案予以实现。
一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法,具体步骤如下:
(1)按摩尔比TiO2:Ta2O5:Eu2O3=97:0.75:0.75进行配料,在去离子水中混合球磨12小时,再于120℃烘干,并过40目分样筛;
(2)造粒:将步骤(1)过筛后的粉料,添加8wt%石蜡作为粘结剂,过80目筛进行造粒,再用粉末压片机压制成坯体;
(3)排胶:将制备好的坯体进行排胶;
(4)烧结:将排胶后的坯体置于烧结炉中,烧结温度为1400~1450℃,保温10h,制成二氧化钛基电介质陶瓷材料;
(5)改性:烧结完成后,将陶瓷制品冷却至室温,利用直流磁控溅射方法,设定溅射电流为4mA~6mA,溅射Au金属,制备出具有巨介电常数的二氧化钛基电介质陶瓷材料。
所述步骤(1)的去离子水:锆球:粉料的质量比=2:1:1。
所述步骤(2)的坯体为Ф10×2.0~3.0mm的圆片坯体。
所述步骤(3)是坯体经3.5h由室温升温至550℃排胶。
所述步骤(4)是坯体由550℃再经10h升温至1400~1450℃进行烧结。
所述步骤(4)烧结温度为1440℃。
本发明的有益效果如下:
1.原料使用施/受主元素Ta5+/Eu3+掺杂二氧化钛基介质材料,可以使介质材料中产生氧空位,从而保证电介质具有高的介电常数。
2.利用磁控溅射仪溅射Au元素至TiO2基陶瓷制品上进行修饰,制备出具有巨介电常数的二氧化钛基电介质陶瓷材料。
3.本发明公开的Au金属修饰的二氧化钛基电介质材料具有优良的介电性能,通过调节磁控溅射的溅射电流,使得材料性能达到了介电常数ε25℃~1553219,介电损耗tanσ~0.4293。
具体实施方式
下面将结合具体实施例对本发明作进一步的详细描述,本发明不局限于如下实施例。
实施例1
首先,用电子天平称量TiO2、Ta2O5、Eu2O3按摩尔比97:0.75:0.75进行配料,以去离子水:锆球:粉料质量比=2:1:1,混合后球磨12h,于120℃烘干,烘干后过40目筛,再外加质量百分比为8%的石蜡,过80目分样筛进行造粒。
将造粒后的粉料在2MPa下压制成Ф10×2mm的圆片生坯,经3.5h空气中由室温升温至550℃排胶,再经10h升温至1440℃烧结,保温10h,制得二氧化钛基电介质陶瓷材料。
利用磁控溅射仪在4mA直流电流条件下对所得制品上下表面进行Au修饰,制得具有巨介电常数的二氧化钛基电介质陶瓷材料。
再对所得制品测试介电性能,测试结果详见表1。
实施例2
首先,用电子天平称量TiO2、Ta2O5、Eu2O3按摩尔比97:0.75:0.75进行配料,以去离子水:锆球:粉料质量比=2:1:1掺入去离子水、锆球,混合后球磨12h,于120℃烘干,烘干后过40目筛,再外加质量百分比为8%的石蜡,过80目分样筛造粒。
将造粒后的粉料在2MPa下压制成Ф10×2.1mm的圆片生坯,经3.5h空气中由室温升温至550℃排胶,再经10h升温至1440℃烧结,保温10h,制得二氧化钛基电介质陶瓷材料。
利用磁控溅射仪在6mA直流电流条件下对所得制品上下表面进行Au修饰,制得具有巨介电常数的二氧化钛基电介质陶瓷材料。
再对所得制品测试介电性能。测试结果详见表1。
本发明的测试方法和检测设备如下:
(1)介电性能测试(交流测试信号:频率为20Hz~1MHz,电压为1V)
使用TH2828S 1MHz同惠精密LCR数字电桥测试样品的电容量C和损耗tanδ,并计算出样品的介电常数,计算公式为:
表1
本发明并不局限于上述实施例,很多细节的变化是可能的,但这并不因此违背本发明的范围和精神。
Claims (6)
1.一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法,具体步骤如下:
(1)按摩尔比TiO2:Ta2O5:Eu2O3=97:0.75:0.75进行配料,在去离子水中混合球磨12小时,再于120℃烘干,并过40目分样筛;
(2)造粒:将步骤(1)过筛后的粉料,添加8wt%石蜡作为粘结剂,过80目筛进行造粒,再用粉末压片机压制成坯体;
(3)排胶:将制备好的坯体进行排胶;
(4)烧结:将排胶后的坯体置于烧结炉中,烧结温度为1400~1450℃,保温10h,制成二氧化钛基电介质陶瓷材料。
(5)改性:烧结完成后,将陶瓷制品冷却至室温,利用直流磁控溅射方法,设定溅射电流为4mA~6mA,溅射Au金属,制备出具有巨介电常数的二氧化钛基电介质陶瓷材料。
2.根据权利要求1所述的一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法,其特征在于,所述步骤(1)的去离子水:锆球:粉料的质量比=2:1:1。
3.根据权利要求1所述的一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法,其特征在于,所述步骤(2)的坯体为Ф10×2.0~3.0mm的圆片坯体。
4.根据权利要求1所述的一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法,其特征在于,所述步骤(3)是坯体经3.5h由室温升温至550℃排胶。
5.根据权利要求1所述的一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法,其特征在于,所述步骤(4)是坯体由550℃再经10h升温至1400~1450℃进行烧结。
6.根据权利要求1所述的一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法,其特征在于,所述步骤(4)烧结温度为1440℃。
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Application publication date: 20191115 |