CN111943683A - 一种氮化硅导电陶瓷及其制备方法 - Google Patents
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Abstract
本发明公开了一种氮化硅导电陶瓷及其制备方法,该氮化硅导电陶瓷由以下质量百分比的原料制备而成,包括氮化硅陶瓷粉体65‑90%、氧化镁2‑6%、氧化钇1‑5%、碳化钛0.5‑3%、氮化钛5‑10%、高纯碳1‑10%、高纯氧化硼4‑10%。该氮化硅导电陶瓷以氮化硅陶瓷粉体为基体原料,再与其它助剂进行复配,通过脱脂脱胶、烧结的步骤制备成具有良好导电性能的氮化硅陶瓷材料,该材料在保持了陶瓷固有的优良性能的基础上,便于对其采用放电方法进行加工,降低加工难度,提高加工效率。本发明所述制备方法简单,原料易得,赋予氮化硅陶瓷优良的导电性能,扩大了氮化硅陶瓷的使用范围,因此,本发明所述制备方法具有重要的意义。
Description
技术领域
本发明属于先进陶瓷材料领域,具体涉及一种氮化硅导电陶瓷及其制备方法。
背景技术
氮化硅是一种重要的结构陶瓷材料。它是一种超硬物质,本身具有润滑性,并且耐磨损,为原子晶体;高温时抗氧化。而且它还能抵抗冷热冲击,在空气中加热到1000℃以上,急剧冷却再急剧加热,也不会碎裂。正是由于氮化硅陶瓷具有如此优异的特性,人们常常利用它来制造轴承、气轮机叶片、机械密封环、永久性模具等机械构件。
氮化硅陶瓷材料作为一种优异的高温工程材料,最能发挥优势的是其在高温领域中的应用。氮化硅今后的发展方向是:(1)充分发挥和利用氮化硅本身所具有的优异特性;(2)在氮化硅粉末烧结时,开发一些新的助熔剂,研究和控制现有助熔剂的最佳成分;(3)改善制粉、成型和烧结工艺;(5)研制氮化硅与SiC等材料的复合化,以便制取更多的高性能复合材料。
由于氮化硅陶瓷本身高强度和高硬度的性能,常以金刚石刀具进行切割,但传统的金刚石加工的方法加工效率低且成本昂贵。氮化硅陶瓷属于绝缘体,其电阻率约为1015Ω·cm量级,是不可能用放电方法进行加工的,从而使其后期加工困难。同时,在某些需要兼具导电性和氮化硅陶瓷固有性能的材料中,氮化硅导电陶瓷的研发则具有重要的意义。
发明内容
为了解决以上现有技术存在的问题,本发明的目的在于提供一种氮化硅导电陶瓷及其制备方法,从而获得一种高导电的氮化硅陶瓷材料。
为了实现上述目的,本发明提供以下技术方案:
一种氮化硅导电陶瓷,由以下质量百分比的原料制备而成,包括氮化硅陶瓷粉体65-90%、氧化镁2-6%、氧化钇1-5%、碳化钛0.5-3%、氮化钛5-10%、高纯碳1-10%、高纯氧化硼4-10%。
优选的,本发明所述的一种氮化硅导电陶瓷,由以下质量百分比的原料制备而成,包括氮化硅陶瓷粉体65-90%、氧化镁2-6%、氧化钇1-5%、碳化钛0.5-3%、氮化钛5-10%、高纯碳1-10%、高纯氧化硼4-10%。
本发明所述氮化硅导电陶瓷的制备方法,包括以下步骤:
(1)称取各原料,湿法研磨并混合均匀后干燥陈化,获得陶瓷坯体;
(2)脱脂脱胶:将步骤(1)陈化后的陶瓷坯体依次在300-430℃保温15min、430-580℃保温10min、580-600℃保温5min、600-650℃保温10min,实现陶瓷坯体的脱脂脱胶;
(3)烧结:将步骤(2)获得的陶瓷坯体在氮气气氛下加热到1750℃,8-10MPa的压力下,烧结曲线为:600℃保温18min,1300℃保温30min,1580℃保温30min,1650℃保温15 min,在1750℃保温30 min;制得氮化硅导电陶瓷制品。
进一步的,所述步骤(1)中湿法研磨的粒径为0.7-50μm。
进一步的,所述步骤(1)中干燥陈化的时间为10-20h。
进一步的,所述步骤(3)的升温速度为2℃/min。
有益效果:本发明提供了一种氮化硅导电陶瓷及其制备方法,该氮化硅导电陶瓷以氮化硅陶瓷粉体为基体原料,再与其它助剂进行复配,通过脱脂脱胶、烧结的步骤制备成具有良好导电性能的氮化硅陶瓷材料,该材料在保持了陶瓷固有的优良性能的基础上,便于对其采用放电方法进行加工,降低加工难度,提高加工效率。本发明所述制备方法简单,原料易得,赋予氮化硅陶瓷优良的导电性能,扩大了氮化硅陶瓷的使用范围,因此,本发明所述制备方法具有重要的意义。
具体实施方式
下面结合具体实施例来进一步描述本发明,但实施例仅是范例性的,并不对本发明的范围构成任何限制。本领域技术人员应该理解的是,在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换,但这些修改和替换均落入本发明的保护范围内。
实施例1
一种氮化硅导电陶瓷,由以下质量百分比的原料制备而成,包括氧化镁4%、氧化钇3%、碳化钛1.5%、氮化钛8%、高纯氧化硼6%,每组氮化硅导电陶瓷中高纯碳的含量如表1中所示,每组氮化硅导电陶瓷的其余原料为氮化硅陶瓷粉体,各原料的百分比总和为百分之百。
本发明所述氮化硅导电陶瓷的制备方法,包括以下步骤:
(1)称取各原料,湿法研磨并混合均匀后干燥陈化,获得陶瓷坯体;所述湿法研磨的粒径为0.7-50μm,所述干燥陈化的时间为15h。
(2)脱脂脱胶:将步骤(1)陈化后的陶瓷坯体依次在350℃保温15min、500℃保温10min、590℃保温5min、600-650℃保温10min,实现陶瓷坯体的脱脂脱胶;
(3)烧结:将步骤(2)获得的陶瓷坯体在氮气气氛下加热到1750℃,8-10MPa的压力下,烧结曲线为:升温速度为2℃/min,600℃保温18min,1300℃保温30min,1580℃保温30min,1650℃保温15 min,在1750℃保温30 min;制得氮化硅导电陶瓷制品。
表1 为不同高纯碳含量制得的氮化硅导电陶瓷的性能对比,从表1中得出,随着高纯碳含量的不断赠大收缩比逐渐减小,即致密性逐渐变差。随着高纯碳含量的增大,氮化硅导电陶瓷的方阻值呈现指数比例下降,即导电性不断提高;当高纯碳含量达到6% 时方阻值达到最小,导电性能达到最佳;随着高纯碳含量进一步加大,方阻值随之增大,说明致密性的变差会降低导电性能。
表1
实施例2
一种氮化硅导电陶瓷,由以下质量百分比的原料制备而成,包括氧化钇3%、碳化钛1.5%、氮化钛8%,高纯氧化硼6%、高纯碳6%,每组氮化硅导电陶瓷中氧化镁的含量如表1中所示,每组氮化硅导电陶瓷的其余原料为氮化硅陶瓷粉体,各原料的百分比总和为百分之百。
每组氮化硅导电陶瓷的制备同实施例1,表2为不同氧化镁含量制得的氮化硅导电陶瓷的性能对比,从表2中得出,随着氧化镁含量的降低,收缩率呈现减少趋势,致密性逐渐下降。电阻逐渐升高,当氧化镁含量在4%时收缩达到顶峰,阻值不再减小。
表2
对比例1
对比例1与实施例2的区别在于,将实施例2中的氧化镁替换成了氧化铝,其他条件不变。从表2和表3的比较得出,同比例的氧化镁和氧化铝,氧化镁能有效地提高致密性,且阻值相对较低,因此氧化镁对氮化硅导电陶瓷的制备具有更好的效果。
表3
实施例3
一种氮化硅导电陶瓷,由以下质量百分比的原料制备而成,包括氧化镁4%、氧化钇3%、碳化钛1.5%、氮化钛8%、高纯氧化硼6%、高纯碳6%,每组氮化硅导电陶瓷的其余原料为氮化硅陶瓷粉体,各原料的百分比总和为百分之百。
每组氮化硅导电陶瓷的制备方法同实施例1,每组氮化硅导电陶瓷的烧结温度如表4所示。
从表4中得出,随着最高烧结温度提高,收缩率变化不显著,阻值降低幅度不大;温度升至1800℃,阻值反而增大,后通过取样成分分析,发现随着温度升高,最终样品中碳含量是降低的,随着高温析出,到1800℃时碳含量已经降至5%。固在1750℃时收缩与碳含量达到最佳状态。
表4
综上所述,当使用氧化镁为烧结助剂,其含量达到4%,碳含量6%,烧结温度1750℃时其致密性与阻值达到最佳匹配,导电性能达到最佳。
Claims (6)
1.一种氮化硅导电陶瓷,其特征在于,由以下质量百分比的原料制备而成,包括氮化硅陶瓷粉体65-90%、氧化镁2-6%、氧化钇1-5%、碳化钛0.5-3%、氮化钛5-10%、高纯碳1-10%、高纯氧化硼4-10%。
2.根据权利要求1所述的一种氮化硅导电陶瓷,其特征在于,由以下质量百分比的原料制备而成,包括氮化硅陶瓷粉体65-90%、氧化镁2-6%、氧化钇1-5%、碳化钛0.5-3%、氮化钛5-10%、高纯碳1-10%、高纯氧化硼4-10%。
3.权利要求1所述氮化硅导电陶瓷的制备方法,其特征在于,包括以下步骤:
(1)称取各原料,湿法研磨并混合均匀后干燥陈化,获得陶瓷坯体;
(2)脱脂脱胶:将步骤(1)陈化后的陶瓷坯体依次在300-430℃保温15min、430-580℃保温10min、580-600℃保温5min、600-650℃保温10min,实现陶瓷坯体的脱脂脱胶;
(3)烧结:将步骤(2)获得的陶瓷坯体在氮气气氛下加热到1750℃,8-10MPa的压力下,烧结曲线为:600℃保温18min,1300℃保温30min,1580℃保温30min,1650℃保温15 min,在1750℃保温30 min;制得氮化硅导电陶瓷制品。
4.根据权利要求3所述的制备方法,其特征在于,所述步骤(1)中湿法研磨的粒径为0.7-50μm。
5.根据权利要求3所述的制备方法,其特征在于,所述步骤(1)中干燥陈化的时间为10-20h。
6.根据权利要求3所述的制备方法,其特征在于,所述步骤(3)的升温速度为2℃/min。
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