文章编号:1004-0609(2015)-03-0754-07
原位合成NiTi-TiB2复合材料的显微组织与性能
姜 江1,马之远2,邵 阳2,彭文屹3,漆艳军3
(1. 江西省科学院 江西省铜钨新材料重点实验室,南昌 330029;
2. 中国石油大学(北京) 理学院,昌平 102249;
3. 南昌大学 材料科学与工程学院,南昌 330031)
摘 要:采用电弧熔炼Ti、Ni和B的方法,原位合成B含量不同的3种NiTi-TiB2复合材料,对复合材料的显微组织、成分及压缩力学性能进行研究。结果表明:材料中NiTi与TiB2之间为冶金结合,结合界面致密无孔隙,克服了以往研究中非原位复合材料常见的界面结合差以及致密度低等缺点。当B的摩尔分数超过6%以后,组织中出现粗大的Ti2Ni脆性枝晶,并伴随材料压缩性能的降低。样品力学性能的恶化与粗大TiB2陶瓷以及Ti2Ni脆性枝晶的形成有关。
关键词:NiTi -TiB2;形状记忆合金;原位合成;马氏体相变
中图分类号:TB34 文献标志码:A
Microstructure and properties of in-situ synthesized NiTi-TiB2 composite
JIANG Jiang1, MA Zhi-yuan2, SHAO Yang2, PENG Wen-yi3, QI Yan-jun3
(1. Jiangxi Key Laboratory of Advanced Copper and Tungsten Materials,
Jiangxi Academy of Sciences, Nanchang 330029, China;
2. School of Science, China University of Petroleum-Beijing, Changping 102249, China;
3. School of Materials Science and Engineering, Nanchang University, Nanchang 330031, China)
Abstract: Three in-situ NiTi-TiB2 composites with different B contents were prepared by arc melting of Ti, Ni and B. The microstructure, composition and compress property were tested. The results show that TiB2 ceramic phase disperses in NiTi shape memory alloy matrix, with metallurgical bonding interface, and no pore is observed, which can overcome the shortcomings in traditional ex-situ composites, such as poor interfacial bonding, low density, porosity, and so on. However, the coarse TiB2 ceramic and brittle Ti2Ni dentrite with tens of micrometers size is observed when the B content is over 6% (mole fraction), which causes compression performance deterioration of the composite.
Key words: NiTi-TiB2; shape memory alloy; in-situ synthesis composite; martensitic transformation
TiB2陶瓷是一种具有特殊物理性能与化学性能的陶瓷,熔点极高、化学稳定性高、硬度高、弹性模量高、耐磨性和电性能优异,常被作为增强相与其他基体复合[1-12];NiTi形状记忆合金(Shape memorial alloy,SMA)是集感知、驱动和执行功能于一体的功能材料,既可以用作传感器感知应力、应变、温度等变化,又可以用作驱动组元改变系统的形状、刚度、固有频率和阻尼等性能[13-18]。例如,将NiTi记忆合金丝复合于铝合金[19-20]、镁合金[21]、高分子[22]等基体中所制备成的复合材料,具有升温自增强[19, 21]、抑制裂纹扩展[23]和减振降噪[24-25]等功能特性。近年来,中国石油大学(北京)崔立山教授的课题组根据NiTi-Nb伪二元共晶转变,在微纳米尺度上将NiTi与Nb原位复合,制备了记忆合金-Nb纤维复合材料,该系列材料具有诸多崭新功能特性[26-32],如宽温域窄滞后相变特性[27]、宽温域负热膨胀停顿点记忆效应[28]、应变软模效应和线性超弹性[32]等。其中,HAO等[32]指出,该材料跨越了复合材料中纳米线无法表现出其本征性能的死亡谷,填补了传统金属、陶瓷和高分子三大类材料性能图表的空白区。这些研究表明,在微细尺度上将记忆合金功能材料与具有其他性能的材料进行原位复合,实现对性能的调控,获得崭新功能甚至超常性能,有望成为材料研究的一种发展趋势。
若采用NiTi记忆合金与TiB2陶瓷复合,利用记忆合金的超弹性、高阻尼性及其抑制裂纹扩展功能[23]增韧脆性陶瓷,有望使材料继承陶瓷的高模量、高硬度、高耐磨特性以及记忆合金的超弹特性和柔韧性等优点[33],同时抵消陶瓷脆性的缺点,展现出超常的力学特性。此外,与TiB2陶瓷耦合后,记忆合金的相变特征会发生改变,有望展现出崭新的功能特性。陈久明等[34]将TiB2粉末和Ni、Ti粉末混合,采用放电烧结的方法制备了TiNi-TiB2的复合材料,然而,采用粉末冶金法,非原位合成的记忆合金-陶瓷复合材料,普遍存在界面结合强度低、多孔隙以及致密度低等缺点,如以往报道的NiTi-TiC复合材料[35-37]。复合界面强度低不利于复合组元间的载荷传递,导致记忆合金与陶瓷材料耦合而产生的新功能特性难以全面而真实的体现出来;致密度低、孔隙多会降低材料的整体力学性能,难以完全体现记忆合金对陶瓷的增韧效果以及陶瓷对记忆合金的增强效果。因此,要对记忆合金-陶瓷复合材料的功能、力学特性的研究有所突破,需要原位合成界面结合良好、致密度高的记忆合金-陶瓷复合材料。
目前,有关原位合成NiTi-TiB2复合材料的研究非常少。孟庆猛等[38]针对Ti-Ni-TiB2合金体系进行了反应热力学理论分析,在一定程度上证实了熔炼法原位合成TiNi-TiB2复合材料的可行性,但他们尚没有进行具体的实验研究。HUANG等[39-40]针对不同Ni含量的Ni-Ti-B体系合金进行了实验探索,但其研究的成分 配比无法形成近等摩尔比的NiTi记忆合金。本文作者通过成分设计,利用电弧熔炼单质Ni、Ti和B得到含有NiTi记忆合金相和TiB2陶瓷相组织的合金锭,该合金是一种原位自生的NiTi-TiB2复合材料,与以往的非原位材料相比,其冶金界面结合强度高,不存在致密度低的问题,有利于材料性能及功能特性的体现。本文作者通过对3种复合材料的微观组织、成分及力学性能的初步探索,为NiTi-TiB2复合材料的设计和原位合成提供了实验基础。
1 实验
采用备有水冷铜坩埚的真空电弧熔炼炉(电弧熔炼炉来自中国科学院沈阳科学仪器研制中心有限公司生产,真空度为1×10-3 Pa),将Ti、Ni和B(纯度分别为99.8%、99.96%和99.9%,质量分数)按设计的成分比例进行熔炼,得到名义成分分别为48.9Ti-46.7Ni- 4.4B、48.5Ti-45.5Ni-6B和46.5Ti-39.5Ni-14B(摩尔分数)的合金锭各100 g。根据不同B含量,将3种样品简称为B4、B6和B14样品。采用FEI Quanta 200型扫描电镜(SEM)观察样品的微观组织,并利用配备的X射线能谱仪进行成分分析;采用德国产NETZSCH 204 F1型示差扫描量热分析仪(DSC)进行相变行为测试,3个样品均经历-80~200 ℃的升降温热循环,升降温速率为10 ℃/min,保护气氛为氩气;利用线切割将合金锭切割成直径3.7 mm、高8 mm的圆柱,并采用WDT II-20型万能拉伸试验机对其进行压缩测试,加载速率为0.3 mm/min。
2 结果与讨论
2.1 合金的成分与组织
近等摩尔比的NiTi形状记忆合金之所以具有形状记忆效应或超弹性等功能特性,是因为其能够发生可逆马氏体相变。而其他的NiTi化合物不能发生可逆相变,不具备功能特性。因此,可以通过测试样品在热循环中是否发生可逆马氏体相变,判断熔炼获得的Ni-Ti体系合金中是否含有NiTi记忆合金相。图1所示为3种样品的DSC测试曲线(吸热峰向下,放热峰向上),由图1可见,3种成分的样品在热循环中都出现了可逆马氏体相变峰,这说明样品中含有NiTi记忆合金相。因此,该系列合金是复合了NiTi记忆合金的原位复合材料。实验说明,在Ti-Ni-B体系中,通过适当调整成分比例,NiTi记忆合金相可以作为稳定相存在于合金中。由于3种样品的正相变开始温度都低于室温,因此,复合的记忆合金都处于母相(奥氏体)状态。
图2所示为3种样品的XRD谱。由图2(a)可见,3种样品中都含有NiTi母相(奥氏体)和TiB2相,且随着B含量的升高,TiB2峰逐渐增强。Ti2Ni峰在B4样品中极不明显,但随着B含量的增加,Ti2Ni峰逐渐增强。图2(b)中局部放大了2θ角度在35°~50°之间区域的XRD谱,图中清晰可见, Ti2Ni峰在B6样品中已可以分辨,在B14样品中则非常显著。通常,在近等摩尔比二元NiTi合金体系中,Ti2Ni脆性相的形成是由于合金成分中Ti含量过高。而NiTi母相的形成说明Ni含量高,即Ti含量较低。故两者一般不会同时大量存在。与之相反,在Ni-Ti-B三元体系中,Ti2Ni相和NiTi母相同时做为稳定相共存于合金中,且在B14样品中,Ti2Ni衍射峰强度较高,Ti2Ni相和NiTi母相大量共存,说明此时Ti2Ni的稳定化并非受控于Ti含量的多少,而是源于B的加入。因此,B加强了Ti2Ni相的稳定性,难以通过简单微调样品中Ti含量来消除NiTiB合金中的Ti2Ni。
![](/web/fileinfo/upload/magazine/12465/308898/image002.jpg)
图1 B4、B6和B14样品的DSC测试结果
Fig. 1 DSC results of B4, B6 and B14 samples (Observed DSC peaks corresponding reversible martensitic transformation of equiatomic NiTi shape memory alloy in these samples)
![](/web/fileinfo/upload/magazine/12465/308898/image004.jpg)
图2 B4、B6和B14样品的XRD谱
Fig. 2 XRD results of B4, B6 and B14 samples
图3所示为3种样品的SEM背散射像。能谱分析显示,图中白色区域为近等原子比的NiTi记忆合金相。由于能谱无法准确识别B的含量,根据XRD成分分析结果判断,图中黑色区域为TiB2陶瓷相。由图3(a)和(b)可见,B4样品的显微组织为块状和线状的TiB2陶瓷(图中黑色区域)镶嵌于NiTi基体(图中白色区域)中。TiB2陶瓷与NiTi记忆合金的复合界面为合金相界面,界面结合强度高,不存在界面污染和孔隙问题。这些特点是以往非原位法获得的记忆合金-陶瓷复合材料难以实现的。在B6和B14样品(见图3(c)、(d)和(e)、(f))中除了TiB2陶瓷相和NiTi记忆合金相外,还出现了粗大的灰色枝晶,并且在B14样品中,枝晶明显增多。根据XRD谱结果,灰色枝晶应为Ti2Ni相。因此,B6和B14样品是TiB2和Ti2Ni复相陶瓷与NiTi记忆合金的复合材料。相比于B4和B6样品而言,B14样品中的线状TiB2陶瓷相明显减少,而块状TiB2陶瓷相增多。3种成分的样品中,除了线状的TiB2陶瓷外,其他陶瓷相都很粗大,达到几十微米级别。
2.2 合金的力学性能测试
图4(a)所示为3种样品的压缩工程应力-应变曲线。得益于NiTi基体的高韧性,3种材料的断裂应变都超过20%,强度都超过1800 MPa。其中,B4样品的断裂应变为33%,强度高达2400 MPa。然而,随着B含量的增加,样品的断裂应变和强度都逐渐降低,变化趋势如图4(b)所示。根据前面的显微组织及成分分析,样品机械性能的劣化与两方面因素有关:1) 随着B含量增加,尺寸大的块状TiB2陶瓷逐渐增多,而小尺寸的针状TiB2陶瓷减少并消失。粗大的TiB2陶瓷相的大量形成不利于材料力学性能,导致材料压缩性能随B含量增加而劣化;2) 随着B含量增加,样品中逐渐出现了粗大的Ti2Ni脆性枝晶,并且其体积分数随B含量的增加而迅速升高。可以认为,粗大的Ti2Ni脆性枝晶的出现加剧了样品的力学性能恶化。因此,在材料合成中,细化陶瓷相尺寸,阻止粗大Ti2Ni枝晶的形成,是进一步研究的重点。
![](/web/fileinfo/upload/magazine/12465/308898/image006.jpg)
图3 B4、B6和B14样品的SEM像
Fig. 3 SEM images of samples B4, B6 and B14
![](/web/fileinfo/upload/magazine/12465/308898/image008.jpg)
图4 B4、B6和B14样品的压缩性能测试结果
Fig. 4 Compression test results of samples B4, B6 and B14
3 结论
1) 通过电弧熔炼单质Ni、Ti和B得到原位自生NiTi-TiB2复合材料。该材料的显微组织为块状和线状的TiB2陶瓷相镶嵌于NiTi记忆合金相中。
2) TiB2陶瓷与NiTi记忆合金的复合界面为合金相界面,界面结合强度高。当B摩尔分数超过6%后,显微组织中出现粗大的Ti2Ni脆性枝晶,此时样品成为TiB2和Ti2Ni复相陶瓷与NiTi记忆合金的复合材料。在该材料体系中,Ti2Ni的稳定存在主要源于B的加入,而并非Ti含量的配比。
3) 由于块状TiB2陶瓷相和Ti2Ni枝晶的尺寸都达到几十微米级别,且随着Ti2Ni脆性枝晶相含量的增加,材料的压缩性能逐渐劣化。因此,在材料合成中,细化陶瓷相尺寸和阻止粗大Ti2Ni枝晶的形成是进一步研究的重点。
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(编辑 龙怀中)
基金项目:国家青年自然科学基金资助项目(51401096);江西省科学院引进博士项目(2013-YYB-5);江西省科学院普惠制项目(2013-XTPH1-33)
收稿日期:2014-07-14;修订日期:2014-11-20
通信作者:姜 江,助理研究员,博士;电话:13694889840;E-mail:superjj1981@163.com