CN108675795B - 一种sps烧结制备高导热和高强度氮化铝陶瓷的方法 - Google Patents
一种sps烧结制备高导热和高强度氮化铝陶瓷的方法 Download PDFInfo
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Abstract
本发明公开了一种SPS烧结制备高导热和高强度氮化铝陶瓷的方法,属于陶瓷材料制备技术领域。本发明以一次粒径小于200纳米的氮化铝粉末为原料,添加稀土金属氟化物作为烧结助剂,加入量为1wt%~4wt%。原料粉末经混粉、成形及在含氮还原性气氛中进行预烧结后,再在高纯氮气保护下进行放电等离子烧结,烧结温度1500℃~1700℃,保温时间1~6min,轴向压力30~50MPa。可制备出晶粒尺寸小于1微米,热导率不低于100W/m·K,抗弯强度不低于700MPa,硬度不低于HRC94的氮化铝陶瓷。
Description
技术领域
本发明属于陶瓷材料制备技术领域,涉及一种SPS烧结制备高导热和高强度氮化铝陶瓷的方法。
背景技术
AlN陶瓷具有高的热导率、相对较低的介电常数和介电损耗、与硅和砷化镓等芯片材料相匹配的热膨胀系数、无毒、绝缘等一系列优异性能,被认为是新一代高性能陶瓷散热器件的首选材料(氮化铝的理论热导率为320W/m·K,是氧化铝陶瓷的十倍左右;热膨胀系数约为3.5~4.8×10-6K-1,20~500℃),已被广泛应用于电子、汽车、航空航天、军事国防等领域。
近几年来,随着科学技术的发展,对所用材料的性能要求越来越高,在某些特定领域,对氮化铝材料要求高导热率的同时还要求其具备良好的力学性能,这就迫使我们探索新的材料制备方法来满足高的性能要求。关于制备高导热和高强度氮化铝陶瓷的方法,中国专利CN 102826853 A公开了一种高强度氮化铝陶瓷基板及其制造方法,其特点是通过在氮化铝粉体中添加特定含量的稀土氧化物、含硅氧化物使得第二相在烧结过程中分布于晶粒三角晶界处,第二相对晶粒间结合产生“粘结”作用,从而获得高强度氮化铝陶瓷。中国专利CN 1689732 B公开了氮化铝烧结体的制备方法,其特点是在烧结坯中加入0.005~0.1wt%的碳,并且选用碱土金属元素化合物和稀土金属元素化合物作为烧结助剂,烧结温度低于1700℃时晶粒尺寸为0.5~2微米,通过抑制晶粒生长而不增大晶粒尺寸来改善烧结体强度。中国专利CN 104973865 A公开了一种高导热氮化铝陶瓷的制备方法,其特点是采用稀土金属氟化物或其混合物作为烧结助剂,经球磨混合、成形、脱脂后,在烧结助剂熔点保温、最终烧结、降温保温后得到导热率高的氮化铝陶瓷。但是上述发明都只单方面强调高导热或者高强度,没有能同时兼顾两方面性能。
放电等离子烧结技术(Spark Plasma Sintering,简称SPS)是一种先进的材料制备技术。SPS是利用脉冲电流通过模具及导电样品,具有更高的热效率,可以实现样品的快速加热与冷却。与传统的粉末冶金技术相比,SPS能够在更低的温度下、更短的时间内实现材料的快速致密,尤其是具有较低扩散系数的高熔点材料如氮化物等可以充分利用SPS技术实现材料的快速烧结。因此能够有效抑制升降温过程晶粒的生长,保留所需的高温结构与物相成份,实现对材料物相和微观结构的灵活调控。中国专利CN 107399972 A公开了一种基于SPS方法制备透明氮化铝陶瓷的方法,其以平均粒径1μm的AlN为原料,以碳化钙和稀土氧化物为烧结助剂,在放电等离子烧结炉中进行烧结,得到晶粒细小的透明氮化铝陶瓷。但是该方法只强调制备出气孔率小、致密度高的透明氮化铝陶瓷,没有考虑氮化铝陶瓷热导率和强度的提升。
发明内容
本发明综合考虑了纳米氮化铝粉末和放电等离子烧结的优势,发明了一种SPS烧结制备高导热和高强度氮化铝陶瓷的方法,该方法将添加烧结助剂的纳米氮化铝粉末经成形和预烧结后,再进行放电等离子烧结,纳米粉末的高烧结活性和放电等离子烧结的快速升降温在促进致密化的同时保证了晶粒的细小。而在含氮还原性气氛中进行的预烧结,可有效较低坯体氧含量,从而减少晶界相数量,净化氮化铝晶格,减少铝空位等缺陷对声子的散射,提高了陶瓷的热导率,获得的氮化铝陶瓷具有抗弯强度高、热导率高的特点。
本发明的技术方案是通过以下步骤实现的:
一种SPS烧结制备高导热和高强度氮化铝陶瓷的方法,其具体工艺为:
a.原料粉末:原料为纳米氮化铝粉末,添加稀土金属氟化物为烧结助剂,烧结助剂的用量为1wt%~4wt%;
b.混粉:将氮化铝粉末与烧结助剂采用湿法球磨进行混合,研磨介质为高纯氧化锆球,溶剂为无水乙醇,重量比约为磨球:酒精:原料=2:2:1,加入1.0wt%油酸作为表面活性剂,球磨混合均匀后干燥过筛得到混合粉末;
c.成形和预烧结:将混合粉末经压制成形得到生坯,压制压力为50~100MPa,再将生坯在常压含氮还原性气氛中1300℃~1500℃的温度下预烧结1~5小时,得到预烧结坯;
d.最终烧结:将预烧结坯在高纯氮气保护下进行放电等离子烧结,烧结温度1500℃~1700℃,升温速率为200℃/min,保温时间1~6min,轴向压力30~50MPa。
进一步地,步骤a中所述的纳米氮化铝粉末的一次粒径小于200纳米,稀土金属氟化物包括氟化钇、氟化镧等。
进一步地,步骤c中所述的含氮还原性气氛为氮气、氨气和氰化氢的混合气,气体流量为0.5~5L/min,混合气体中氮气的体积分数为70%~95%,氨气的体积分数为0~20%,氰化氢的体积分数为0.5%~10%。
通过采用前述技术方案,本发明的有益效果是:1:本发明使用的氮化铝粉末为纳米粉末,具有很高的比表面积和高的烧结活性,能够有效降低致密化温度。放电等离子烧结技术能够实现样品的快速升温和降温,可以有效抑制晶粒与颈部的生长,同时压力辅助能够增强烧结过程中纳米氮化铝的颗粒重排行为,最终获得的氮化铝陶瓷晶粒细小,力学性能优异;2:在含氮还原性气氛中预烧结,可有效较低坯体氧含量,从而减少晶界相数量,净化氮化铝晶格,减少铝空位等缺陷对声子的散射,提高了热导率;3:所制备的氮化铝陶瓷的晶粒尺寸小于1微米,热导率不低于100W/m·K,抗弯强度不低于700MPa,硬度不低于HRC94。
综上所述,本发明提供的一种SPS烧结制备高导热和高强度氮化铝陶瓷的方法,工艺简单,成本较低,更加适于实用,且具有产业上的利用价值。其具有上述诸多的优点及实用价值,并在同类制备方法中未见有类似的设计公开发表或使用而确属创新,其在制备方法上或功能上皆有较大的改进,在技术上有较大的进步,诚为一新颖、进步、实用的新设计。
上述说明仅是本发明技术方案的概述,为了能够更清楚了解本发明的技术手段,并可依照说明书的内容予以实施,以下以本发明的较佳实施例详细说明如后。
本发明的具体制备方法及其结构由以下实施例详细给出。
具体实施方式
为更进一步阐述本发明为达成预定发明目的所采取的技术手段及功效,以下结合较佳实施例,对依据本发明提出的一种SPS烧结制备高导热和高强度氮化铝陶瓷的方法其具体实施方式、步骤、结构、特征详细说明如后。
实施例1:
1.原料粉末:原料为一次粒径为100纳米的氮化铝粉末,烧结助剂为氟化钇;
2.混粉:将1000g氮化铝粉末与20g氟化钇,1wt%油酸放入球磨罐中,加入2000g高纯氧化锆磨球,2000ml无水乙醇,球磨混合10h后干燥过筛得到混合粉末;
3.成形和预烧结:将混合粉末压制成形得到生坯,压制压力为80MPa,再将生坯在常压含氮还原性气氛中1500℃的温度下预烧结4小时,气体流量为2L/min,其中氮气的体积分数为90%,氨气的体积分数为5%,氰化氢的体积分数为5%;
4.最终烧结:将预烧结坯在高纯氮气保护下进行放电等离子烧结,烧结温度1500℃,升温速率为200℃/min,保温时间5min,轴向压力40MPa。
通过本方案制备得到的氮化铝陶瓷,其晶粒尺寸小于1微米,热导率为110W/m·K,抗弯强度为760MPa,硬度为HRC97。
实施例2:
1.原料粉末:原料为一次粒径为80纳米的氮化铝粉末,烧结助剂为氟化镧;
2.混粉:将1000g氮化铝粉末与30g氟化镧,1wt%油酸放入球磨罐中,加入2000g高纯氧化锆磨球,2000ml无水乙醇,球磨混合10h后干燥过筛得到混合粉末;
3.成形和预烧结:将混合粉末压制成形得到生坯,压制压力为50MPa,再将生坯在含氮还原性气氛中1400℃的温度下预烧结4小时,气体流量为3L/min,其中氮气的体积分数为95%,氨气的体积分数为2%,氰化氢的体积分数为3%;
4.最终烧结:将预烧结坯在高纯氮气保护下进行放电等离子烧结,烧结温度1600℃,升温速率为200℃/min,保温时间6min,轴向压力30MPa。
通过本方案制备得到的氮化铝陶瓷,其晶粒尺寸小于1微米,热导率为115W/m·K,抗弯强度为740MPa,硬度为HRC96。
实施例3:
1.原料粉末:原料为一次粒径为60纳米的氮化铝粉末,烧结助剂为氟化钇;
2.混粉:将1000g氮化铝粉末与15g氟化钇,1wt%油酸放入球磨罐中,加入2000g高纯氧化锆磨球,2000ml无水乙醇,球磨混合10h后干燥过筛得到混合粉末;
3.成形和预烧结:将混合粉末压制成形得到生坯,压制压力为100MPa,再将生坯在含氮还原性气氛中1300℃的温度下预烧结2小时,气体流量为3L/min,其中氮气的体积分数为80%,氨气的体积分数为10%,氰化氢的体积分数为10%;
4.最终烧结:将预烧结坯在高纯氮气保护下进行放电等离子烧结,烧结温度1500℃,升温速率为200℃/min,保温时间3min,轴向压力30MPa。
通过本方案制备得到的氮化铝陶瓷,其晶粒尺寸小于1微米,热导率为100W/m·K,抗弯强度为780MPa,硬度为HRC98。
实施例4:
1.原料粉末:原料为一次粒径为100纳米的氮化铝粉末,烧结助剂为氟化钇;
2.混粉:将1000g氮化铝粉末与40g氟化钇,1wt%油酸放入球磨罐中,加入2000g高纯氧化锆磨球,2000ml无水乙醇,球磨混合10h后干燥过筛得到混合粉末;
3.成形和预烧结:将混合粉末压制成形得到生坯,压制压力为80MPa,再将生坯在含氮还原性气氛中1500℃的温度下预烧结5小时,气体流量为5L/min,其中氮气的体积分数为70%,氨气的体积分数为20%,氰化氢的体积分数为10%;
4.最终烧结::将预烧结坯在高纯氮气保护下进行放电等离子烧结,烧结温度1700℃,升温速率为200℃/min,保温时间6min,轴向压力50MPa。
通过本方案制备得到的氮化铝陶瓷,其晶粒尺寸小于1微米,热导率为120W/m·K,抗弯强度为705MPa,硬度为HRC95。
实施例5:
1.原料粉末:原料为一次粒径为40纳米的氮化铝粉末,烧结助剂为氟化镧;
2.混粉:将1000g氮化铝粉末与35g氟化镧,1wt%油酸放入球磨罐中,加入2000g高纯氧化锆磨球,2000ml无水乙醇,球磨混合10h后干燥过筛得到混合粉末;
3.成形和预烧结:将混合粉末压制成形得到生坯,压制压力为60MPa,再将生坯在含氮还原性气氛中1500℃的温度下预烧结1小时,气体流量为1L/min,其中氮气的体积分数为75%,氨气的体积分数为15%,氰化氢的体积分数为10%;;
4.最终烧结:将预烧结坯在高纯氮气保护下进行放电等离子烧结,烧结温度1550℃,升温速率为200℃/min,保温时间4min,轴向压力30MPa。
通过本方案制备得到的氮化铝陶瓷,其晶粒尺寸小于1微米,热导率为115W/m·K,抗弯强度为735MPa,硬度为HRC96。
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭露如上,然而并非用以限定本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的方法及技术内容作出些许的更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。
Claims (3)
1.一种SPS烧结制备高导热和高强度氮化铝陶瓷的方法,其特征在于具体工艺为:
a.原料粉末:原料为纳米氮化铝粉末,添加稀土金属氟化物为烧结助剂,烧结助剂的用量为1wt%~4wt%;
b.混粉:将氮化铝粉末与烧结助剂采用湿法球磨进行混合,研磨介质为高纯氧化锆球,溶剂为无水乙醇,其比例为磨球:无水乙醇:氮化铝粉末=2000g: 2000ml: 1000g,加入1.0wt%油酸作为表面活性剂,球磨混合均匀后干燥过筛得到混合粉末;
c.成形和预烧结:将混合粉末经压制成形得到生坯,压制压力为50~100MPa,再将生坯在常压含氮还原性气氛中1300℃~1500℃的温度下预烧结1~5小时,得到预烧结坯;
d.最终烧结:将预烧结坯在高纯氮气保护下进行放电等离子烧结,烧结温度1500℃~1700℃,升温速率为200℃/min,保温时间1~6min,轴向压力30~50MPa;
所制备的氮化铝陶瓷晶粒尺寸小于1微米,热导率不低于100W/m·K,抗弯强度不低于700MPa,硬度不低于HRC94。
2.根据权利要求1所述的一种SPS烧结制备高导热和高强度氮化铝陶瓷的方法,其特征在于:步骤a中所述的纳米氮化铝粉末的一次粒径小于200纳米,稀土金属氟化物为氟化钇或氟化镧。
3.根据权利要求1所述的一种SPS烧结制备高导热和高强度氮化铝陶瓷的方法,其特征在于:步骤c中所述含氮还原性气氛为氮气、氨气和氰化氢的混合气,气体流量为0.5~5L/min,混合气体中氮气的体积分数为70%~95%,氨气的体积分数为0~20%,氰化氢的体积分数为0.5%~10%。
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