CN112759401A - 一种利用微波烧结制备高熵硼陶瓷表面材料的方法 - Google Patents
一种利用微波烧结制备高熵硼陶瓷表面材料的方法 Download PDFInfo
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Abstract
本发明公开了一种利用微波烧结制备高熵硼陶瓷表面材料的方法,包括将氮化物陶瓷基片坯料放入微波烧结腔内的辅热保温结构内,叠放整齐,氮化物陶瓷基片坯料与氮化物陶瓷基片坯料之间设置有石墨板,微波烧结频率为2.45GHz,通入含氢7~10%的氮气氛,常压微波烧结温度为500~3000℃,升温速率为8~10℃/min,保温2‑10小时,随炉冷却,至400℃以下时开炉取出,得到致密的高质量氮化物陶瓷基片烧结体。本发明的有益效果是:本发明是一种加快反应烧结进程,在较低的温度、较短的时间内,在常压下烧结氮化物陶瓷材料的微波烧结氮化物陶瓷材料的方法,具有升温速度快,烧结温度低,保温时间短,性能较好,节约能源,生产效率高的特点,适合大规模生产。
Description
技术领域
本发明涉及陶瓷技术领域,尤其涉及一种利用微波烧结制备高熵硼陶瓷表面材料的方法。
背景技术
氮化物陶瓷材料是一类用途非常广泛的新型陶瓷材料,它包括氮化铝陶瓷、氮化硅陶瓷、氮化硼陶瓷等,其复合材料更是数不胜数,正因为其在材料领域的重要地位,所以日益受到材料研究者及应用者的广泛重视。
但由于氮化物陶瓷材料大都是固相烧结,虽然可以利用添加剂的形式进行液相烧结,但其烧结温度仍然较高,保温时间仍需较长的时间,难以烧结,能耗高,生产效率极低,例如氮化铝陶瓷材料的烧结,添加5%的Y2O3烧结助剂,传统烧结方法需1900℃烧结温度,保温24小时才能得出性能较好的氮化铝陶瓷材料成品,所以给氮化铝陶瓷材料的生产和应用带来了极大的困难。
发明内容
本发明的目的是提供一种利用微波烧结制备高熵硼陶瓷表面材料的方法,在较低的温度、较短的时间内,在常压下烧结氮化物陶瓷材料的微波烧结氮化物陶瓷材料的方法,具有升温速度快,烧结温度低,保温时间短,性能较好,节约能源,生产效率高的特点,适合大规模生产。
本发明的技术方案是这样实现的:
一种利用微波烧结制备高熵硼陶瓷表面材料的方法,包括将氮化物陶瓷基片坯料放入微波烧结腔内的辅热保温结构内,叠放整齐,氮化物陶瓷基片坯料与氮化物陶瓷基片坯料之间设置有石墨板,微波烧结频率为2.45GHz,通入含氢7~10%的氮气氛,常压微波烧结温度为500~3000℃,升温速率为8~10℃ /min,保温2-10小时,随炉冷却,至400℃以下时开炉取出,得到致密的高质量氮化物陶瓷基片烧结体。
进一步的,所述辅热保温结构由氧化铝纤维板、氮化硼匣钵以及高纯石墨板构成。
进一步的,其特征在于,氮化物陶瓷基片坯料与石墨板之间均匀的撒上氮化硼粉末。
进一步的,其特征在于,所述微波烧结腔为类似球形或圆柱形状腔体,且以60转/min的速度匀速旋转。
进一步的,其特征在于,所述微波烧结装置为间歇式工业微波炉或连续式工业微波炉。
本发明的有益效果是:本发明是一种加快反应烧结进程,在较低的温度、较短的时间内,在常压下烧结氮化物陶瓷材料的微波烧结氮化物陶瓷材料的方法,具有升温速度快,烧结温度低,保温时间短,性能较好,节约能源,生产效率高的特点,适合大规模生产。利用微波能转化为分子的动能和热能,整体均匀加热,不易变形,且由于微波的活化性能,在较低的温度致密烧结氮化铝陶瓷基片,成本大幅度下降,再结合高纯石墨板的微波反射效果及还原性气氛的激发,通过含氢的氮气氛在烧结后期的晶界净化,最终得到高质量的氮化物陶瓷基片。
具体实施方式
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,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。
根据本发明的实施例,提供了一种利用微波烧结制备高熵硼陶瓷表面材料的方法。
根据本发明实施例的利用微波烧结制备高熵硼陶瓷表面材料的方法,包括将氮化物陶瓷基片坯料放入微波烧结腔内的辅热保温结构内,叠放整齐,氮化物陶瓷基片坯料与氮化物陶瓷基片坯料之间设置有石墨板,微波烧结频率为 2.45GHz,通入含氢7~10%的氮气氛,常压微波烧结温度为500~3000℃,升温速率为8~10℃/min,保温2-10小时,随炉冷却,至400℃以下时开炉取出,得到致密的高质量氮化物陶瓷基片烧结体。
实施例1:
将氮化铝粉末与质量百分比为5%的高纯Y2O3粉末混合后压成尺寸为φ40× 10mm的坯料,放置于辅热保温结构内。将辅热保温结构置于间歇式工业微波炉的烧结腔体内进行微波烧结,微波频率为2.45GHz。通入高纯氮气保护,压力为常压,烧结温度为500℃,保温2小时,所得烧结体冷却后即为成品氮化铝陶瓷材料。经测定,制得氮化铝陶瓷材料的热导率为150W/m·k,密度为3.0g/cm3, XRD分析相结构为AlN、YAlO3。
实施例2:
将质量百分比为58%的氮化硅与适量的TiC、ZrN、AlN等混合后制成Ф 10mm的小球,放置于辅热保温结构内。将辅热保温结构置于连续式工业微波炉的烧结腔体内进行微波烧结,微波频率为2.45GHz。通入高纯氮气保护,压力为常压,烧结温度为800℃,保温2小时,所得烧结体冷却后即为成品氮化硅复合陶瓷材料。经测定,制得氮化硅复合陶瓷材料成品密度为3.71g/cm 3,硬度 1520HV。
实施例3:
将氮化铝粉末与质量百分比为4%的高纯Y2O3粉末混合后压成尺寸为50mm ×50mm×10mm的坯料,放置于辅热保温结构内。将辅热保温结构置于间歇式工业微波炉的烧结腔体内进行微波烧结,微波频率为2.45GHz。通入氮气加氢气的混合气体保护,压力为常压,烧结温度为500℃,保温10小时,所得烧结体冷却后即为成品氮化铝陶瓷材料。经测定,制得氮化铝陶瓷材料的热导率为 148W/m·k,密度为3.19g/cm 3,做XRD分析相结构为AlN、YAlO3。
实施例4:
将质量百分比为90%的氮化硅与适量的Al2O3、Y2O3、AlN等混合后制成Ф 10mm小球,放置于辅热保温结构内。将辅热保温结构置于连续式工业微波炉的烧结腔体内进行微波烧结,微波频率为2.45GHz。通入高纯氮气保护,压力为常压,烧结温度为1600℃,保温2h,所得烧结体冷却后即为成品氮化硅复合陶瓷材料。经测定,制得氮化硅复合陶瓷材料成品密度为3.18g/cm3,抗弯强度 713MPa。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (5)
1.一种利用微波烧结制备高熵硼陶瓷表面材料的方法,其特征在于,包括将氮化物陶瓷基片坯料放入微波烧结腔内的辅热保温结构内,叠放整齐,氮化物陶瓷基片坯料与氮化物陶瓷基片坯料之间设置有石墨板,微波烧结频率为2.45GHz,通入含氢7~10%的氮气氛,常压微波烧结温度为500~3000℃,升温速率为8~10℃/min,保温2-10小时,随炉冷却,至400℃以下时开炉取出,得到致密的高质量氮化物陶瓷基片烧结体。
2.根据权利要求1所述的一种利用微波烧结制备高熵硼陶瓷表面材料的方法,其特征在于,所述辅热保温结构由氧化铝纤维板、氮化硼匣钵以及高纯石墨板构成。
3.根据权利要求1所述的一种利用微波烧结制备高熵硼陶瓷表面材料的方法,其特征在于,氮化物陶瓷基片坯料与石墨板之间均匀的撒上氮化硼粉末。
4.根据权利要求1所述的一种利用微波烧结制备高熵硼陶瓷表面材料的方法,其特征在于,所述微波烧结腔为类似球形或圆柱形状腔体,且以60转/min的速度匀速旋转。
5.根据权利要求1所述的一种利用微波烧结制备高熵硼陶瓷表面材料的方法,其特征在于,所述微波烧结装置为间歇式工业微波炉或连续式工业微波炉。
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