CN110407585A - N缺位高纯Ti2AlN粉体材料及其制备方法 - Google Patents

N缺位高纯Ti2AlN粉体材料及其制备方法 Download PDF

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CN110407585A
CN110407585A CN201910833225.8A CN201910833225A CN110407585A CN 110407585 A CN110407585 A CN 110407585A CN 201910833225 A CN201910833225 A CN 201910833225A CN 110407585 A CN110407585 A CN 110407585A
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贾汶哲
马朝阳
郭锋
张鹏程
李世波
黄振莺
周洋
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Beijing Jiaotong University
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Abstract

一种N缺位非化学计量比高纯Ti2AlN MAX粉体材料及其制备方法。本发明的镁基复合材料成分如下：Ti2AlN中的N含量不在是1，而是可处于0.85和1.0区间内，如摘要图所示，a和c轴的晶格参数可以通过N含量来进行调节；其N缺位的Ti2AlN陶瓷显微结构为疏松多孔，而且Ti2AlN的晶粒大小可以调控。制备方法：(1)配料：将商用的Ti粉,Al粉and AlN粉按照Ti:Al:N＝2:(1.05‑1.0):(0.85‑1.0)的比例进行配比；(2)混料；(3)压坯；(4)烧结温度升在1400℃‑1480℃，保温在10‑40mins；(5)破碎及球磨；(6)干燥并过筛。

Description

N缺位高纯Ti2AlN粉体材料及其制备方法
技术领域
一种N缺位非化学计量比高纯Ti2AlN MAX粉体材料及其制备方法。
背景技术
可进行机械加工的新型三元层状金属陶瓷MAX材料，化学通式为Mn+1AXn，M为过渡金属，A主要为IIIA和IVA簇元素，n＝1～3，X为C或N，对于不同的n值(n＝1、2或3)，构成211、312和413相。目前已合成有超过60种化合物及其固溶体，典型的有Ti3SiC2、Ti3AlC2、Ti2AlC、Ti2SnC、Nb2AlC、Ti3SiAlC2和Ti2AlSnC等。例如，Ti2AlN作为MAX材料的一种，其具有分层的六方晶体结构，近乎密排的各个Ti层与Al层交叉，N原子填充Ti6N的八面体位置，Al原子则位于具有较大空间的三方柱的中心。[参考文献：N.V.Tzenov和M.W.Barsoum,J.Am.Ceram.Soc.,2000,83[4]:825]与传统硬脆的SiC和TiC陶瓷不同，MAX材料表现出优良的韧性和可加工性，如Ti2AlC的断裂韧性为6.5-7.9±0.1MPa·m1/2。Barsoum等[参考文献：Barsoum,M.W.,et al.,Nature Materials,2003.2:p.107.]发现MAX相Mg，Ti，Zr和Zn等金属同属密排六方晶系，具备微塑变形机制，即内部形成的Incipient Kinking Bands(IKB)，循环压缩过程可大大吸收外界的能量。其特殊的晶体结构中，Ti原子与N原子之间的结合为强共价键，而Ti原子与Al原子之间为弱结合，类似于层状石墨，层间由范德华力结合。0.8MPa压强和60m/s滑动速度下，对低碳钢的干摩擦系数约为0.1，磨损率约为2.510-6mm3/Nm[参考文献：H-X Zhai，et al,Mater.Sci.Forum,2005[475-479]:1251]结构决定性能，⊥c轴的层与层之间在剪切力的作用下容易发生滑动，并发生类似金属的弯折带塑形变形。
目前，MAX材料可以通过M，A和X三个位置的固溶进行自身性能的调控[参考文献：Maxim Sokol et al.,Trends in Chemistry,1,2019]。但是，通过X位置缺位进行MAX材料性能的调控，尚未见报道。前期的研究表明，二元TiN中N含量可以在0.6-1.1区间内调节，其中，12.5％的N缺位可以使TiN的硬度从190GPa降低40GPa。[参考文献：Pierson,H.O.,Processing and Apps.1996:William Andrew]N含量低时，TiNy表现出更多的金属特性，N含量高时，TiNy表现出更多的陶瓷特性。这种具有金属和共价晶体的特点，使N的p轨道低于费米能级，从而导致自由电子的运动类似于在金属的d轨道上运动。这个独特性，TiNy薄膜在微电子领域得到广泛应用，例如其对可见光和红外光的选择透滤。[参考文献：SavvidesN.,j.Appl.Phys,(64)1,1988，p.225-234]
由于Ti2AlN晶胞中包含Ti6N八面体，从理论上表明，N缺位的Ti2AlN可以合成。从而，调节Ti2AlN自身的性能，使其在高温结构件，耐强酸碱腐蚀件，耐磨损件等领域得到应用；另外，通过Ti2AlN陶瓷粉体可进行液相剥离，能够制备出N缺位的二维Ti2AlN或Ti2N纳米粉体，可应用作为锂离子电池或电容器的电极材料，储氢材料及复合材料的添加相。Ti2AlN或Ti2N中N的缺位，必然可以调控Ti2AlN或Ti2N材料自身的电负性，进而控制其对锂离子和氢离子的吸附中，达到调控的目的。由此可见，低成本大规模制备N缺位的陶瓷粉体是其在结构和功能领域得到广泛应用的首要条件。
发明内容
本发明的目的是提供一种N缺位非化学计量比高纯Ti2AlN MAX粉体材料,同时提供其相应的制备方法。
1.本发明的目的是提供一种N缺位非化学计量比高纯Ti2AlN MAX粉体材料，Ti2AlN中的N含量y＝0.85-1.0；同时，提供其简易的无压烧结制备方法。
本发明的镁基复合材料成分如下：
Ti2AlN中的N含量不在是1，而是可处于0.85和1.0区间内。
其显微结构如下：
N缺位的Ti2AlN陶瓷为疏松多孔，而且Ti2AlN的晶粒大小可以调控。
本发明所具有的有益效果：
通过N缺位达到自身性能可调控的Ti2AlN，有望在高温结构件，耐强酸碱腐蚀件，耐磨损件等领域得到应用；另外，通过Ti2AlN陶瓷粉体可进行液相剥离制备出N缺位的二维Ti2AlN或Ti2N纳米粉体，可应用作为锂离子电池或电容器的电极材料，储氢材料及复合材料的添加相。Ti2AlN或Ti2N中N的缺位，必然可以调控Ti2AlN或Ti2N材料自身的电负性，进而控制其对锂离子和氢离子的吸附中，达到调控的目的。
本发明的镁基复合材料发动机活塞制备方法包括以下各步骤：
(1)配料：将商用的Ti粉,Al粉and AlN粉按照Ti:Al:N＝2:(1.05-1.0):(0.85-1.0)的比例进行配比；
(2)混料：把配比后的粉体置于装有玛瑙球的罐中进行混料，一定混料时间后达到粉体混合均匀化的效果；
(3)压坯：将混合后的粉料装入钢模具中，施加50-80MPa左右的单向压力，将混合粉料压成坯体；
(4)烧结：干燥后，将坯体迅速装入模具中，放入真空无压烧结炉内，抽真空后通入氩气，按15-30℃/min的升温速率升温，温度升至1400℃-1480℃，保温10-20min。保温结束后，随炉冷却降温至80℃左右取出样品，即得到疏松多孔的N缺位Ti2AlN陶瓷块体；
(5)破碎及球磨：清除Ti2AlN陶瓷块体表皮，放入颚式破碎机中，破碎成小于2mm的粗粉，将破碎后的Ti2AlN粗粉与玛瑙球按球料体积比2:1的比例称取放入氧化铝球磨罐中，再加入无水乙醇。然后将球磨罐装在行星球磨机进行球磨达到粉体细化的效果；
(6)干燥并过筛：将球磨后的球料倒入不锈钢盘中，放于干燥箱中，去除无水乙醇。将Ti2AlN粉过过筛并封存装入密封袋
附图说明
图1是无压烧结制备的Ti2AlNy(y＝0.85,0.9,0.85,1.0)微观组织电镜图。
图2是无压烧结制备的Ti2AlNy(y＝0.85,0.9,0.85,1.0)XRD扫描。
图3是Ti2AlNy a和c轴晶格参数随y值的变化(y＝0.85,0.9,0.85,1.0)。
具体实施方式
实施案例1
N含量为0.85的Ti2AlN粉体制备
将商用的Ti粉,Al粉and AlN粉按照Ti:Al:N＝2:1.05:0.85进行称重配比，把配比后的粉体置于装有玛瑙球的罐中进行混料，一定混料时间后达到粉体混合均匀化的效果，将混合后的粉料装入钢模具中，施加50-80MPa左右的单向压力，将混合粉料压成坯体，干燥后，将坯体迅速装入模具中，放入真空无压烧结炉内，抽真空后通入氩气，按15-30℃/min的升温速率升温，温度升至1400℃，保温20min。保温结束后，随炉冷却降温至80℃左右取出样品，即得到疏松多孔的N缺位Ti2AlN陶瓷块体。
实施案例2
N含量为0.95的小晶粒Ti2AlN粉体制备
将商用的Ti粉,Al粉and AlN粉按照Ti:Al:N＝2:1.05:0.95进行称重配比，把配比后的粉体置于装有玛瑙球的罐中进行混料，一定混料时间后达到粉体混合均匀化的效果，将混合后的粉料装入钢模具中，施加50-80MPa左右的单向压力，将混合粉料压成坯体，干燥后，将坯体迅速装入模具中，放入真空无压烧结炉内，抽真空后通入氩气，按15-30℃/min的升温速率升温，温度升至1400℃，保温20min。保温结束后，随炉冷却降温至80℃左右取出样品，即得到疏松多孔的N缺位Ti2AlN陶瓷块体。
实施案例23
N含量为0.95的大晶粒Ti2AlN粉体制备
将商用的Ti粉,Al粉and AlN粉按照Ti:Al:N＝2:1.10:0.95进行称重配比，把配比后的粉体置于装有玛瑙球的罐中进行混料，一定混料时间后达到粉体混合均匀化的效果，将混合后的粉料装入钢模具中，施加50-80MPa左右的单向压力，将混合粉料压成坯体，干燥后，将坯体迅速装入模具中，放入真空无压烧结炉内，抽真空后通入氩气，按15-30℃/min的升温速率升温，温度升至1450℃，保温40min。保温结束后，随炉冷却降温至80℃左右取出样品，即得到疏松多孔的N缺位Ti2AlN陶瓷块体。

Claims (3)

1.一种N缺位非化学计量比高纯Ti2AlN MAX粉体材料及其制备方法，其特征在于：Ti2AlN中的N含量y＝0.85-1.0，制备方法采用了无压烧结。
2.根据权利要求1所述的复合材料，其特征在于：Ti2AlN中的N含量不在是1，而是可处于0.85和1.0区间内；无压烧结过程中不需要压力且用时短。
3.根据权利要求1所述的镁基复合材料发动机活塞的制备方法，其特征在于：该方法包括下述步骤：(1)配料：将商用的Ti粉,Al粉and AlN粉按照Ti:Al:N＝2:(1.05-1.0):(0.85-1.0)的比例进行配比；(2)混料：把配比后的粉体置于装有玛瑙球的罐中进行混料，一定混料时间后达到粉体混合均匀化的效果；(3)压坯：将混合后的粉料装入钢模具中，施加50-80MPa左右的单向压力，将混合粉料压成坯体；(4)烧结：干燥后，将坯体迅速装入模具中，放入真空无压烧结炉内，抽真空后通入氩气，按15-30℃/min的升温速率升温，温度升至1400℃-1480℃，保温10-20min。保温结束后，随炉冷却降温至80℃左右取出样品，即得到疏松多孔的N缺位Ti2AlN陶瓷块体；(5)破碎及球磨：清除Ti2AlN陶瓷块体表皮，放入颚式破碎机中，破碎成小于2mm的粗粉，将破碎后的Ti2AlN粗粉与玛瑙球按球料体积比2:1的比例称取放入氧化铝球磨罐中，再加入无水乙醇。然后将球磨罐装在行星球磨机进行球磨达到粉体细化的效果；(6)干燥并过筛：将球磨后的球料倒入不锈钢盘中，放于干燥箱中，去除无水乙醇。将Ti2AlN粉过过筛并封存装入密封袋。
CN201910833225.8A 2019-09-04 2019-09-04 N缺位高纯Ti2AlN粉体材料及其制备方法 Pending CN110407585A (zh)

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