CN103183511B - 三氧化二铝弥散强化钛四铝氮三陶瓷复合材料及制备方法 - Google Patents

三氧化二铝弥散强化钛四铝氮三陶瓷复合材料及制备方法 Download PDF

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CN103183511B
CN103183511B CN201310099914.3A CN201310099914A CN103183511B CN 103183511 B CN103183511 B CN 103183511B CN 201310099914 A CN201310099914 A CN 201310099914A CN 103183511 B CN103183511 B CN 103183511B
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CN103183511A (zh
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郑卓
李菊英
崔玉友
杨锐
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Abstract

本发明涉及陶瓷复合材料领域，具体为一种用三氧化二铝（Al2O3）弥散强化钛四铝氮三（Ti4AlN3）陶瓷复合材料及其制备方法，陶瓷复合材料具有高硬度、高强度和良好的抗氧化性能，且具有导电、可加工性。该陶瓷复合材料，主要由Ti4AlN3基体和Al2O3强化相组成，Al2O3颗粒弥散分布在Ti4AlN3基体中，Al2O3颗粒为1-2微米，Al2O3的体积分数在35-45%。本发明直接采用原料粉，为原位生成Al2O3颗粒和原位反应生成Ti4AlN3型，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40%左右。本发明采用纳米粉合成块体反应快，时间短，可以节约大量能源。

Description

三氧化二铝弥散强化钛四铝氮三陶瓷复合材料及制备方法
技术领域
本发明涉及陶瓷复合材料领域，具体为一种用三氧化二铝（Al2O3）弥散强化钛四铝氮三（Ti4AlN3）陶瓷复合材料及其制备方法。
背景技术
Ti4AlN3的晶体结构是J.C.Schuster等人在1984年发现的，起初认为其结构式为Ti3Al2N2。在此之后，许多学者对Ti3Al2N2材料进行了详细的研究。1997年，HeeDong Lee和William T.Petuskey发现Ti3Al2N2不完全符合化学计量比，提出更为精确的计量比应为Ti3Al1-xN2。在此基础上，W.M.Bousum等人通过研究将其化学式改为Ti4AlN3，并将其归纳为Mn+1AXn三元陶瓷材料的一种。Mn+1AXn材料中的M为过渡元素，A是主族元素，X是C或N，其中n为1,2或3，如Ti3SiC2、Ti4SiC3、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），易于加工，不同于传统二元氮化物、碳化物陶瓷硬度大，不易加工的特点。
Ti4AlN3是属于密排六方结构的三元氮化物陶瓷，空间群为P63/mmc。Ti6N八面体与Al原子层沿着c轴方向上周期堆垛。由于晶胞内金属键、共价键和离子键共存，故Ti4AlN3具有金属的导电导热性、加工性和陶瓷的高强度、高模量等优点。Ti4AlN3一般采用TiH2、AlN和TiN粉末为原料，在1275℃/24h/70MPa热等静压而成。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+填隙在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Ti4AlN3的密度，热膨胀系数很接近，硬度和压缩强度互相补充，选在Al2O3弥散强化Ti4AlN3基体，可以提高其高温强度和抗氧化性能。Al2O3和Ti4AlN3的主要性能见表1。
表1Ti4AlN3和Al2O3的物理性能和力学性能
一般采用粉末热压或热等加压成型得到的Al2O3弥散强化Ti4AlN3复合材料，有以下几种方法配比粉末组成：
（1）采用Al2O3粉和Ti4AlN3粉，属于无原位反应型；
（2）采用Al2O3粉和生成Ti4AlN3的原料粉，属于原位反应生成Ti4AlN3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，这种现象越明显。
发明内容
本发明的目的是提供一种用三氧化二铝弥散强化钛四铝氮三陶瓷复合材料及其制备方法，陶瓷复合材料具有高硬度、高强度和良好的抗氧化性能，且具有导电、可加工性。
本发明的技术方案是：
一种三氧化二铝弥散强化钛四铝氮三陶瓷复合材料，该陶瓷复合材料，主要由Ti4AlN3基体和Al2O3强化相组成，Al2O3颗粒弥散分布在Ti4AlN3基体中，Al2O3颗粒为1-2微米，Al2O3的体积分数在35-45%，Ti4AlN3的体积分数在50-60%。
所述的三氧化二铝弥散强化钛四铝氮三陶瓷复合材料，Al2O3的体积分数优选为40%。
所述的三氧化二铝弥散强化钛四铝氮三陶瓷复合材料，其余为少量的反应相Al3Ti和AlN。
所述的三氧化二铝弥散强化钛四铝氮三陶瓷复合材料的制备方法，包括如下步骤：
首先，在0.7-1.2个大气压的N2、H2和Ar混合气氛中，其中N2占总体积含量的4-15%，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法合成复合材料的纳米粉；
然后，采用热等静压方法将纳米粉致密化，工艺参数：温度为1200℃-1400℃，压力为100-160MPa，时间为1-2h，真空度为2×10-2-5×10-3Pa。
所述的三氧化二铝弥散强化钛四铝氮三陶瓷复合材料的制备方法，步骤（1）中，纳米粉的平均粒径为100-150纳米。
本发明提供的Al2O3弥散强化Ti4AlN3陶瓷复合材料及其制备方法的优点在于：
1、本发明直接采用原料粉，为原位生成Al2O3颗粒和原位反应生成Ti4AlN3型，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40%。
2、本发明复合材料中Ti4AlN3基体和Al2O3强化相均为原位反应生成，Al2O3颗粒为1-2微米，弥散分布在Ti4AlN3基体。
3、本发明制备的陶瓷复合材料显微硬度是Ti4AlN3的2.6倍，强化效果显著。
4、本发明采用纳米粉合成块体反应快，时间短，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，呈球状粉末(内插图为电视衍射谱)。
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计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射线衍射图谱。
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。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明。
本发明三氧化二铝弥散强化钛四铝氮三陶瓷复合材料，主要由Ti4AlN3基体和Al2O3强化相组成，Al2O3颗粒弥散分布在Ti4AlN3基体中，Al2O3颗粒为1-2微米，Al2O3的体积分数在35-45%（优选为40%），Ti4AlN3的体积分数在50-60%，其余为少量的反应相Al3Ti和AlN。
所述三氧化二铝弥散强化钛四铝氮三陶瓷复合材料的制备方法，包括如下步骤：
首先，在0.7-1.2个大气压的N2、H2和Ar混合气氛中，其中N2占总体积含量的4-15%，H2与Ar之体积比为1:0.8-1.2，在连续供给Ti30Al-Ti60Al（Ti原子百分含量为30-60%）母合金棒的条件下，采用氢等离子金属反应法合成复合材料的纳米粉；纳米粉的投射电镜形貌见图1、图2，有两种典型的形貌：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见图3，陶瓷复合材料的宏观照片见图4。由此可以看出，纳米粉的平均粒径为120纳米。
其中，氢等离子金属反应法采用常规技术，可参见文献：[1]孙维民,金寿日.活性等离子体—金属”反应法制备Ni—TiN复合超微粒子的研究.材料科学与工艺.1997,5(4):P26-29；[2]李星国,廖复辉.直流电弧等离子体法合成金属和陶瓷纳米颗粒.过程工程学报,2002,2(4):P295-300；[3]林峰,蒋燕麟,文永鹏,张健伟.直流电弧等离子体制备纳米粉技术及其应用.大众科技.2012,01:P99-103。
然后，采用热等静压方法将纳米粉致密化，工艺参数：温度为1200℃-1400℃，压力为100-160MPa，时间为1-2h，真空度为2×10-2-5×10-3Pa。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，尺寸大约在1.5微米，弥散分布在Ti4AlN3基体中。制备的复合材料的X射线衍射图谱见图6，结果表明该复合材料主要生成相：Al2O3和Ti4AlN3，另外含有少量的反应相Al3Ti和AlN。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Ti4AlN3硬度的2.6倍，显著强化了Ti4AlN3相，且硬度随载荷变化不显著。
实施例1
首先，在0.77个大气压的N2、H2和Ar混合气氛中，其中N2占总体积含量的9%，H2与Ar气体积比为1:1，在连续供给Ti48Al（原子百分比）母合金棒材的条件下，采用氢等离子金属反应法合成用于制备该复合材料的纳米粉，纳米粉的平均粒径为120纳米。
然后，称量25g纳米粉，至于的纯钛包套内，放入热等静压机内，抽真空，真空度为3×10-3Pa，在1280℃/150MPa条件下保温1小时。所得到的复合材料中Al2O3颗粒为1-2微米，Al2O3的体积分数为40%，Ti4AlN3的体积分数在54%，其余为少量的反应相Al3Ti和AlN。
实施例2
首先，在1.0个大气压的N2、H2和Ar混合气氛中，其中N2占总体积含量的6%，H2与Ar气体积比为1:1，在连续供给Ti48Al（原子百分比）母合金棒材的条件下，采用氢等离子金属反应法合成用于制备该复合材料的纳米粉，纳米粉的平均粒径为110纳米。
然后，称量25g纳米粉，至于的纯钛包套内，放入热等静压机内，抽真空，真空度为3×10-3Pa，在1250℃/145MPa条件下保温1.5小时。所得到的复合材料中Al2O3颗粒为1-2微米，Al2O3的体积分数为35%，Ti4AlN3的体积分数在60%，其余为少量的反应相Al3Ti和AlN。
实施例3
首先，在0.9个大气压的N2、H2和Ar混合气氛中，其中N2占总体积含量的12%，H2与Ar气体积比为1:1，在连续供给Ti48Al（原子百分比）母合金棒材的条件下，采用氢等离子金属反应法合成用于制备该复合材料的纳米粉，纳米粉的平均粒径为130纳米。
然后，称量25g纳米粉，至于的纯钛包套内，放入热等静压机内，抽真空，真空度为3×10-3Pa，在1350℃/155MPa条件下保温2小时。所得到的复合材料中Al2O3颗粒为1-2微米，Al2O3的体积分数为45%，Ti4AlN3的体积分数在50%，其余为少量的反应相Al3Ti和AlN。

Claims (3)

1.一种三氧化二铝弥散强化钛四铝氮三陶瓷复合材料，其特征在于，该陶瓷复合材料，主要由Ti4AlN3基体和Al2O3强化相组成，Al2O3颗粒弥散分布在Ti4AlN3基体中，Al2O3颗粒为1-2微米，Al2O3的体积分数在35-45%，Ti4AlN3的体积分数在50-60%；
所述的三氧化二铝弥散强化钛四铝氮三陶瓷复合材料的制备方法，包括如下步骤：
首先，在0.7-1.2个大气压的N2、H2和Ar混合气氛中，其中N2占总体积含量的4-15%，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法合成复合材料的纳米粉，纳米粉的平均粒径为100-150纳米；
然后，采用热等静压方法将纳米粉致密化，工艺参数：温度为1250℃-1400℃，压力为100-160MPa，时间为1-2h，真空度为2×10-2-5×10-3Pa。
2.按照权利要求1所述的三氧化二铝弥散强化钛四铝氮三陶瓷复合材料，其特征在于，Al2O3的体积分数为40%。
3.按照权利要求1所述的三氧化二铝弥散强化钛四铝氮三陶瓷复合材料，其特征在于，其余为少量的反应相Al3Ti和AlN。
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