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CN1321939C - 一种用三氧化二铝弥散强化钛二铝氮陶瓷复合材料及其制备方法 - Google Patents

一种用三氧化二铝弥散强化钛二铝氮陶瓷复合材料及其制备方法 Download PDF

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CN1321939C
CN1321939C CNB2004100209704A CN200410020970A CN1321939C CN 1321939 C CN1321939 C CN 1321939C CN B2004100209704 A CNB2004100209704 A CN B2004100209704A CN 200410020970 A CN200410020970 A CN 200410020970A CN 1321939 C CN1321939 C CN 1321939C
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李菊英
崔玉友
杨锐
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Institute of Metal Research of CAS
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Abstract

本发明提供一种Al2O3弥散强化Ti2AlN陶瓷复合材料，由Ti2AlN基体和Al2O3强化相组成，Al2O3颗粒弥散分布在Ti2AlN基体中，Al2O3颗粒为0.8～1.2微米，Al2O3的体积分数为25～50%。其制备方法是：在0.8～1.2个大气压的N2、H2和Ar混合气氛中，N2占总气量的2～15%，H2与Ar之体积比为1∶0.8～1.2，在连续供给母合金棒的条件下，用氢等离子金属反应制备方法合成纳米粉；再用真空热压方法将纳米粉致密化，温度为800℃～1200℃，压力为40～60MPa，时间为4～6h，真空度为2×10-2～5×10-3Pa。该材料的优点在于：显微硬度是Ti2AlN的2.5倍，强化效果显著；呈现金属特性电阻率曲线，室温电阻率是0.5μΩ·m；热压温度低，时间短可以节约大量能源。

Description

一种用三氧化二铝弥散强化钛二铝氮陶瓷复合材料及其制备方法
技术领域
本发明涉及陶瓷复合材料及其制备方法。
背景技术
Ti2AlN的晶体结构是Jeitschko等人在二十世纪六十年代早期确定的，七十年代中期Ivchenko等人制备出致密度为90～92％的块体，显微硬度大于20GPa。近年来，Barsoum等人制备出一系列三元陶瓷材料，可用Mn+1AXn来统一表示，M为过渡元素，A是主族元素，X是C或N，n为1，2或3，如Ti3SiC2，Ti2AlC，Ti2AlN，Cr2GaC等。这些三元陶瓷具有很多共同点，如比普通陶瓷更软(3～6GPa)，容易加工，显著不同于硬度大、不易加工的二元氮化物、碳化物。
Ti2AlN是一种密排六方结构的三元氮化物陶瓷，Ti位于4f位置，Al位于2c位置，N位于Ti八面体间隙位置。由于晶胞里金属键、共价键和离子键共存，故Ti2AlN同时具有金属的良好导电导热性、加工性和陶瓷的高强度、高模量等优点。Ti2AlN一般采用纯Ti粉和AlN粉，经过1400℃/48h/40MPa反应热等静压得到，含有少量的Al2O3和Ti4AlN3相。Al2O3是一种稍畸变密排六方结构的离子氧化物，O2-位于密排六方阵点位置，Al3+填隙于O2-的八面体间隙位置，这种结构在熔点附近也具有较好的稳定性。由于Al2O3和Ti2AlN密度、热膨胀系数很接近，硬度和压缩强度互相补充，选择Al2O3弥散强化Ti2AlN基体，可提高其高温强度和抗氧化性。Al2O3和Ti2AlN的主要性能见表1。
表1 Ti2AlN和Al2O3的物理性能和力学性能
     性能     Ti2AlN     Al2O3
密度(g/cm3)     4.31     3.9
维氏硬度(GPa)     4     18
压缩强度(MPa)     450     2600
电阻率(μΩ·m)     0.25，0.312     ＞1018
热膨胀系数(K-1)     8.2×10-6     8.3×10-6
杨氏模量(GPa)     -     380386
剪切模量(GPa)     -     175
熔点(℃)     -     2054
一般采用粉末热压或热等静压成型得到Al2O3弥散强化Ti2AlN复合材料。有以下几种方法配比粉末组成：
1、采用Al2O3粉和Ti2AlN粉，属于无原位反应型；
2、采用Al2O3粉和生成Ti2AlN的原料粉，属于原位反应生成Ti2AlN型；
3、直接采用原料粉，为原位生成Al2O3颗粒和原位反应生成Ti2AlN型。
第一种和第二种方法存在的问题是Al2O3分布不均匀，易团聚，颗粒长大明显。随着Al2O3体积分数的增加，这种现象越显著。第三种方法，原位生成的Al2O3颗粒细小，呈弥散分布，体积分数可调整到高达50％。
发明内容
本发明的目的是提供一种具有高硬度、高强度和良好的抗氧化性，且具有导电、可加工性的陶瓷复合材料。
本发明提供一种Al2O3弥散强化Ti2AlN陶瓷复合材料，主要由Ti2AlN基体和Al2O3强化相组成，Al2O3颗粒弥散分布在Ti2AlN基体中，Al2O3颗粒为0.8～l.2微米，Al2O3的体积分数为25～50％。
本发明还提供一种Al2O3弥散强化Ti2AlN陶瓷复合材料的制备方法，其特征在于工艺过程如下：
首先，在0.8～1.2个大气压的N2、H2和Ar混合气氛中，其中N2占总气量的2～15％，H2与Ar之体积比为1∶0.8～1.2，在连续供给Ti30Al～Ti60Al母合金棒的条件下，采用氢等离子金属反应制备方法合成该复合材料的纳米粉；纳米粉的透射电镜形貌见图1、图2，有两种典型形貌，一种为球形或近球形颗粒(如图1)，另一种为方形颗粒(如图2)，电子衍射分析表明方形颗粒是TiN；氢等离子金属反应法制备的纳米粉的粒径分布图见图3，由此图可以看出，纳米粉的平均粒径为42纳米；
然后采用真空热压方法将纳米粉致密化，工艺参数：温度为800℃～1200℃，压力为40～60MPa，时间为4～6h，真空度为2×10-2～5×10-3Pa。制备的复合材料宏观照片见图4，样品尺寸为φ50×5，密度为4.05g/cm3。对制备的复合材料进行了金相观察、x射线物相分析、电阻率和硬度测试。制备的复合材料的金相形貌见图5，图中黑色颗粒为Al2O3，尺寸大约1微米，弥散分布在Ti2AlN基体中。制备的复合材料的x射线衍射谱见图6，结果表明该复合材料主要为生成相：Al2O3和Ti2AlN，另外含有少量反应相：TiN和TiAl3。制备的复合材料的显微硬度与载荷之间的曲线见图7，从该图中可以看出，复合材料的显微硬度是Ti2AlN硬度的2.5倍，显著强化了Ti2AlN相，且硬度随载荷变化不显著。制备的复合材料电阻率随温度的变化曲线见图8，从该图中可以看出，复合材料呈现金属特性电阻率曲线，室温电阻率是0.5μΩ·m，比Ti2AlN的电阻率高，和纯Ti的相当。
本发明提供的Al2O3弥散强化Ti2AlN陶瓷复合材料及其制备方法的优点在于：
复合材料中Ti2AlN基体和Al2O3强化相均为原位反应生成，Al2O3颗粒为0.8～1.2微米，弥散分布在Ti2AlN基体；
制备的陶瓷复合材料显微硬度是Ti2AlN的2.5倍，强化效果显著；
制备的陶瓷复合材料呈现金属特性电阻率曲线，室温电阻率是0.5μΩ·m，比Ti2AlN的电阻率稍高，和纯Ti相当；
采用平均粒径42纳米的纳米粉，故合成块体的热压温度低，比采用微米粉经反应热等静压合成的Ti2AlN温度低200～500℃左右，时间短20～40小时，可以节约大量能源。
附图说明
图1是氢等离子金属反应法制备的合金纳米粉形貌，呈圆球状粉；
图2是氢等离子金属反应法制备的合金纳米粉形貌，呈立方体状粉(内插图为电子衍射谱)；
图3是氢等离子金属反应法制备的合金纳米粉的粒径分布图。
图4是制备的陶瓷复合材料的外观图；
图5是制备的陶瓷复合材料的金相照片；
图6是制备的陶瓷复合材料的x射线衍射谱图；
图7是制备的陶瓷复合材料的显微硬度与载荷之间的关系曲线图；
图8是制备的陶瓷复合材料电阻率随温度的变化曲线图。
具体实施方式
实施例1
首先，在1个大气压的N2、H2和Ar混合气氛中，其中N2占总气量的5％，H2与Ar之体积比为1∶1，在连续供给Ti60Al(原子百分比)母合金棒的条件下，采用氢等离子金属反应制备方法合成用于制备该复合材料的纳米粉。
然后称量22克纳米粉，置于φ50×60的石墨模具腔中，把模具放在真空热压炉内，抽真空，然后升温加热到预定的850℃，到达850℃后加45MPa压力，保持温度和压力恒定4.5h。经历此热压工艺后得到2.75mm厚的样品。
所得到的复合材料中，Al2O3颗粒为0.8～1.2微米，Al2O3的体积分数为45％。
实施例2
首先，在1.2个大气压的N2、H2和Ar混合气氛中，其中N2占总气量的8％，H2与Ar之体积比为1∶1.2，在连续供给Ti50Al母合金棒的条件下，采用氢等离子金属反应制备方法合成用于制备该复合材料的纳米粉。
然后称量26克纳米粉，置于φ50×60的石墨模具腔中，把模具放在真空热压炉内，抽真空，然后升温加热到预定的950℃，到达950℃后加50MPa压力，保持温度和压力恒定5h。经历此热压工艺后得到3.28mm厚的样品。
所得到的复合材料中，Al2O3颗粒为0.8～1.2微米，Al2O3的体积分数为40％。
实施例3
首先，在0.8个大气压的N2、H2和Ar混合气氛中，其中N2占总气量的10％，H2与Ar之体积比为1∶0.9，在连续供给Ti40Al母合金棒的条件下，采用氢等离子金属反应制备方法合成用于制备该复合材料的纳米粉。
然后称量34.5克纳米粉，置于φ50×60的石墨模具腔中，把模具放在真空热压炉内，抽真空，然后升温加热到预定的1050℃，到达1050℃后加55MPa压力，保持温度和压力恒定5.5h。经历此热压工艺后得到4.45mm厚的样品。
所得到的复合材料中，Al2O3颗粒为0.8～1.2微米，Al2O3的体积分数为35％。
实施例4
首先，在1.1个大气压的N2、H2和Ar混合气氛中，其中N2占总气量的12％，H2与Ar之体积比为1∶0.8，在连续供给Ti30Al母合金棒的条件下，采用氢等离子金属反应制备方法合成用于制备该复合材料的纳米粉。
然后称量41克纳米粉，置于φ50×60的石墨模具腔中，把模具放在真空热压炉内，抽真空，然后升温加热到预定的1150℃，到达1150℃后加60MPa压力，保持温度和压力恒定6h。经历此热压工艺后得到5.15mm厚的样品。
所得到的复合材料中，Al2O3颗粒为0.8～1.2微米，Al2O3的体积分数为30％。

Claims (2)

1、一种Al2O3弥散强化Ti2AlN陶瓷复合材料，由Ti2AlN基体、强化相Al2O3，以及反应相TiN和TiAl3组成，其特征在于：Al2O3颗粒弥散分布在Ti2AlN基体中，Al2O3颗粒为0.8～1.2微米，Al2O3的体积分数为25～50％。
2、一种权利要求1所述的Al2O3弥散强化Ti2AlN陶瓷复合材料的制备方法，其特征在于工艺过程如下：
首先，在0.8～1.2个大气压的N2、H2和Ar混合气氛中，其中N2为总气量的2～15％，H2与Ar之体积比为1∶0.8～1.2，在连续供给Ti30Al～Ti60Al母合金棒的条件下，采用氢等离子金属反应制备方法合成用于制备该复合材料的纳米粉；
然后采用真空热压方法将纳米粉致密化，工艺参数：温度为800℃～1200℃，压力为40～60MPa，时间为4～6h，真空度为2×10-2～5×10-3Pa。
CNB2004100209704A 2004-07-15 2004-07-15 一种用三氧化二铝弥散强化钛二铝氮陶瓷复合材料及其制备方法 Expired - Fee Related CN1321939C (zh)

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US11/629,559 US7459408B2 (en) 2004-07-15 2005-07-15 Al2O3 dispersion-strengthened Ti2AlN composites and a method for producing the same
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