CN1453242A - 一种形状记忆陶瓷及其制备方法 - Google Patents

一种形状记忆陶瓷及其制备方法 Download PDF

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CN1453242A
CN1453242A CN 02111522 CN02111522A CN1453242A CN 1453242 A CN1453242 A CN 1453242A CN 02111522 CN02111522 CN 02111522 CN 02111522 A CN02111522 A CN 02111522A CN 1453242 A CN1453242 A CN 1453242A
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徐祖耀
金学军
张玉龙
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Emerson Electric China Holdings Co Ltd
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Abstract

一种形状记忆陶瓷及其制备方法。本发明的形状记忆陶瓷以含铈和钇的二氧化锆为基，其成分范围为7～10mol％CeO2，0.2～0.8mol％Y2O3和余量为ZrO2，较佳为7.5～8.5mol％CeO2，0.45～0.55mol％Y2O3和余量为ZrO2。其制备方法采用下列步骤：用共沉淀法制备所述各成分的超细粉，在1500±20℃空气中烧结4～6小时，烧结后逐渐冷却，得到平均晶粒尺寸为0.9～1.1μm和致密度为5.9～6.1g/cm3的四方氧化锆多晶陶瓷块材。本发明的形状记忆陶瓷在可回复应变达1.2％时仍有95～100％的形状恢复率，同时保持高的动作温度，并有3～4％的伪弹性恢复。

Description

一种形状记忆陶瓷及其制备方法
技术领域
本发明涉及一种形状记忆陶瓷，尤其是涉及一种以含铈和钇的二氧化锆为基的形状记忆陶瓷。
背景技术
近年来，以二氧化锆(ZrO2)为基的形状记忆陶瓷的研究和开发方面已知的有：含镁(Mg)的ZrO2形状记忆陶瓷、含铈(Ce)的ZrO2形状记忆陶瓷和含钇(Y)的ZrO2形状记忆陶瓷等二元ZrO2基形状记忆陶瓷。对于ZrO2基陶瓷，它通常是通过应力诱发t→m马氏体相变而具有高强度和韧性，同时上述所加的各成分可起到稳定ZrO2陶瓷或晶体作用。应力诱发马氏体相通过加热逆相变而呈现形状记忆效应(SME)，即给予形状记忆材料以温度变化，就能自动作功而回复形状。举例来说，在含有MgO的ZrO2基形状记忆陶瓷中，MgO起到部分稳定ZrO2陶瓷的作用。在含有Y2O3或CeO2的ZrO2基形状记忆陶瓷中，Y2O3或CeO2起到稳定四方ZrO2多晶的作用，因而它们都具有形状记忆效应，而且其动作温度较一般金属基形状记忆合金高出数百度，且兼具陶瓷材料的特点。尽管它还存在着许多不足，但有较好的研究和应用前景，已引起业界的广泛兴趣。
形状记忆效应的性能指标有形状恢复率(Shape recovery rate)和可恢复应变(reversible strain)等。为了将形状记忆陶瓷用于仪器仪表、自动控制、工程测量和传感技术等领域，人们总是希望得到形状恢复率和可恢复应变都较高的和可供应用的形状记忆陶瓷。但是，现有的二元ZrO2基形状记忆陶瓷并不能满足这种要求。
例如，在1986年美国的《自然》杂志中，M.V.Swain揭示了一种含有9.4mol％MgO的ZrO2基形状记忆陶瓷，其晶粒约为50μm。在四点弯曲试验中，加热至600℃以上时其形状能恢复，但可回复或恢复应变较小，仅为～0.42％。
在1988年美国J.American Ceramics Society杂志上，P.E.Reyes-Morel等人公开了一种12mol％Ce-TZP陶瓷，并发现该陶瓷具有伪弹性和形状记忆效应。在单轴压缩时晶粒尺寸从1.0μm到2.8μm的材料形状恢复率为≤90％，可恢复应变为≤1％。由此可见，含Ce的ZrO2的二元形状记忆陶瓷的主要问题为可回复应变较小和形状恢复不完全。
发明内容
本发明的目的是为了提供一种含铈和钇的二氧化锆基形状记忆陶瓷及其制备方法，该形状记忆陶瓷可达到高达95～100％的形状恢复率、1％以上的可回复应变和3～4％的伪弹性。
实现上述目的的技术方案是：本发明的一个方面提供以含铈和钇的二氧化锆为基的形状记忆陶瓷，其成分范围为：7～10mol％CeO2，0.2～0.8mol％Y2O3和余量为ZrO2。
如以上所述的形状记忆陶瓷，其成分范围较佳为：7.5～8.5mol％CeO2，0.45～0.55mol％Y2O3和余量为ZrO2。
所述的形状记忆陶瓷为四方氧化锆多晶陶瓷，其具有在单轴压应力下5％的压缩应变可达到3～4％的伪弹性。
如上所述四方氧化锆多晶陶瓷在可恢复应变达1.2％时仍有95～100％的形状恢复率。
本发明的另一个方面提供一种形状记忆陶瓷的制备方法，其中，采用下列步骤：用共沉淀法制备所述各成分的超细粉，在1500±20℃空气中烧结4～6小时，烧结后逐渐冷却，得到平均晶粒尺寸为0.9～1.1μm和致密度为5.9～6.1g/cm3的四方氧化锆多晶陶瓷块材。
本发明通过优化成分、烧结工艺和热处理等手段，获得具有更佳形状记忆效应(SME)的含Ce和Y的ZrO2形状记忆陶瓷，其可回复应变达1.2％时有95～100％的形状恢复率，同时保持高的动作温度和3～4％的伪弹性恢复。
附图说明
图1是一含有8mol％二氧化铈-0.5mol％三氧化二钇-二氧化锆的扫描电镜照片。
图2是一含有8mol％二氧化铈-0.5mol％三氧化二钇-二氧化锆的形状记忆效应的应力-应变-温度曲线图。
具体实施方式
实施例1
为制取成分为8mol％CeO2、0.5mol％Y2O3和余量为ZrO2的形状记忆陶瓷，用共沉淀法制备各成分的超细粉，在1500℃空气中烧结6小时，随后逐渐冷却。
采用这种方法可制得平均晶粒尺寸为1.06μm和致密度为6.03g/cm3的四方氧化锆多晶块材，如图1所示。该多晶陶瓷的可恢复应变和形状恢复率的测试数据列于表1，而根据上述测试数据制作的相应的温度—应变和应力—应变的关系曲线示于图2。从测试结果可看到，可恢复应变为1.18％时，形状恢复率仍为100％。
测试时，测得试样的压缩前长l1＝6.974mm，压缩后长l0＝6.892，升温至600℃再冷至室温长l2＝6.974，并通过形状恢复率 η = l 2 - l 0 l 1 - l 0 × 100 % 的计算公式算出形状恢复率，得到如前所述的形状恢复率和可恢复应变。
表1，8mol％CeO2-0.5mol％Y2O3-ZrO2材料形状记忆效应。
试样   初始长l0(mm)    变形后l1(mm)    膨胀后l2(mm)    应变(％)   恢复率η(％)
8mol％CeO2-0.5mol％Y2O3-ZrO2    6.97     6.89     6.976    1.15     100
   6.962     6.890     6.962    1.03     100
   6.974     6.892     6.974    1.18     100
   6.963     6.900     6.970    0.905     100
   6.957     6.888     6.958    0.992     100
实施例2
使用如同实施例1的制备和烧结方法制取成分为7.5mol％CeO2，0.45mol％Y2O3和余量为ZrO2的形状记忆陶瓷，制得的四方氧化锆块材经实施例1的同样的测试方法进行测试，得到可恢复应变为1.2％，形状恢复率为100％。
实施例3
使用如同实施例1的制备和烧结方法制取成分为8.5mol％CeO2，0.55mol％Y2O3和余量为ZrO2的形状记忆陶瓷，制得的四方氧化锆块材经实施例1的同样的测试方法进行测试，得到可恢复应变为1.1％，形状恢复率为100％。
实施例4
使用如同实施例1的制备和烧结方法制取成分为8mol％CeO2，0.6mol％Y2O3和余量为ZrO2的形状记忆陶瓷，制得的四方氧化锆块材经实施例1的同样的测试方法进行测试，得到可恢复应变为1.0％，形状恢复率为95～100％。很明显，虽然本实施例也达到形状记忆材料性能指标，但在ZrO2的形状记忆陶瓷中Y2O3含量的增加会影响到可恢复应变和形状恢复率的提高。
实施例5
使用如同实施例1的制备和烧结方法制取成分为8mol％CeO2、0.75mol％Y2O3和余量为ZrO2的形状记忆陶瓷，制得的四方氧化锆块材经实施例1的同样的测试方法进行测试，得到可恢复应变为1.0％，形状恢复率为95～100％。所得到的测试数据基本上接近实施例4的测试结果。
本发明材料系列为全新的三元ZrO2基形状记忆陶瓷，在可恢复应变达到1.0～1.2％的情况下，形状恢复率均为90～100％。形状恢复率和可恢复应变均比含Ce的二元形状记忆陶瓷有很大的提高。根据本发明的材料特别适用于特殊环境，如需高动作温度、耐蚀、绝缘和高强度的形状记忆元件。

Claims (5)

1.一种形状记忆陶瓷，其特征在于，所述的形状记忆陶瓷以含铈和钇的二氧化锆为基，其成分范围为：7～10mol％CeO2，0.2～0.8mol％Y2O3和余量为ZrO2。
2.如权利要求1所述的形状记忆陶瓷，其特征在于，所述的形状记忆陶瓷成分范围为：7.5～8.5mol％CeO2，0.45～0.55mol％Y2O3和余量为ZrO2。
3.如权利要求1或2所述的形状记忆陶瓷，其特征在于，所述的形状记忆陶瓷为四方氧化锆多晶陶瓷，其具有在单轴压应力下5％的压缩应变可达到3～4％的伪弹性。
4.如权利要求3所述的形状记忆陶瓷，其特征在于，所述四方氧化锆多晶陶瓷在可恢复应变达1.2％时有95～100％的形状恢复率。
5.一种形状记忆陶瓷的制备方法，其特征在于，采用下列步骤：
用共沉淀法制备所述各成分的超细粉，在1500±20℃空气中烧结4～6小时，烧结后逐渐冷却，得到平均晶粒尺寸为0.9～1.1μm和致密度为5.9～6.1g/cm3的四方氧化锆多晶陶瓷块材。
CN 02111522 2002-04-27 2002-04-27 一种形状记忆陶瓷及其制备方法 Pending CN1453242A (zh)

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WO2014007852A1 (en) * 2012-07-02 2014-01-09 Massachusetts Institute Of Technology Ceramic structures for enhanced shape memory and pseudoelastic effects
CN104496470A (zh) * 2014-12-16 2015-04-08 广东省工业技术研究院(广州有色金属研究院) 一种高弹性纳米氧化锆基陶瓷的制备方法
CN105211310A (zh) * 2015-09-21 2016-01-06 方辉宇 一种新型大豆片型食品的生产方法
US9512039B2 (en) 2013-03-08 2016-12-06 Massachusetts Institute Of Technology Oligocrystalline ceramic structures for enhanced shape memory and pseudoelastic effects
US9548678B2 (en) 2012-07-02 2017-01-17 Massachusetts Institute Of Technology Electric field activation of shape memory ceramics
CN110815971A (zh) * 2019-11-08 2020-02-21 南京赛诺特斯材料科技有限公司 一种氧化锆陶瓷背板及其加工方法

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US9512039B2 (en) 2013-03-08 2016-12-06 Massachusetts Institute Of Technology Oligocrystalline ceramic structures for enhanced shape memory and pseudoelastic effects
CN104496470A (zh) * 2014-12-16 2015-04-08 广东省工业技术研究院(广州有色金属研究院) 一种高弹性纳米氧化锆基陶瓷的制备方法
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