CN116589877A - 一种MXene/8YSZ:Eu3+温敏热障涂层材料的制备方法 - Google Patents
一种MXene/8YSZ:Eu3+温敏热障涂层材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种MXene/8YSZ:Eu3+温敏热障涂层材料的制备方法。本发明以8YSZ:Eu3+陶瓷材料为基底材料，通过机械研磨混合的方法引入MXene材料，成功制备MXene/8YSZ:Eu3+温敏热障涂层材料。本发明采用的实验方法易于操作，成本低，易于控制，可控变量多，可以重复实验。获得的MXene/8YSZ:Eu3+温敏热障涂层材料具有良好的发光性能、荧光衰减寿命以及温敏性能等优点。本发明为热障涂层材料的发展提供了良好的基础，为提高稀土掺杂温敏陶瓷材料的荧光性能提供了良好的设计思路。其良好的荧光及温敏性能可以更好的应用于热障涂层材料对其服役温度进行实时监测，具有广阔的应用前景。
Description
技术领域
本发明属于温敏陶瓷材料的制备和发光技术领域，具体涉及到一种MXene/8YSZ:Eu3+温敏热障涂层材料的制备方法。
背景技术
航空发动机热端部件长期处在高温、高压、辐射、烟雾的恶劣环境下运转，难免会产生一系列复杂的“热问题”。目前航空发动机的涡轮叶片大多数采用的热障涂层(thermalbarrier coatings,简称TBCs)体系主要由合金基体、MCrAlY或Pt改性的铝化物粘结层、热生长氧化物(thermally grown oxide,简称TGO)和氧化钇稳定的氧化锆(Yttria-stabilized zirconia,简称YSZ)陶瓷层四部分组成，热障涂层的寿命很大程度上取决于TGO和YSZ陶瓷层。然而TGO和YSZ陶瓷层的工作温度又在很大程度上决定了它们的使用寿命，因此，温度监测对于热障涂层是十分重要的。
近年来，基于光学响应温度特性的荧光测温技术迅速发展，为实时监测热障涂层服役温度及预测其使用寿命带来了希望。其原理是具有温度自敏特性的稀土荧光材料受到热量激发，外层电子由激发态向基态恢复过程中电子跃迁以荧光形式释放激发能量，具有荧光强度和波长与温度变化的关联特性。稀土元素Eu、Tb、Dy等元素可作为热障涂层的温敏材料，主要包含硫化物基(Zn，CaS:Eu3+)和氧化物基(Y2O3:Eu3+，Nb2+)等，通过在涂层引入不同的稀土元素(Dy3+、Zr3+、Eu3+)，通过检测荧光强度的变化评价涂层的损耗量，从而可以非破坏性地研究涂层寿命。因此通过在YSZ陶瓷层中掺杂稀土元素，利用稀土荧光材料的发光特性来实时监测热障涂层的温度及寿命成为一种可能。研究发现，Eu3+掺杂的8YSZ(ZrO2-8％Y2O3，YSZ中Y2O3质量分数为8％)材料是一种有效地稀土光致发光材料，但是Eu3+存在荧光淬灭性。
Ti3C2Tx MXene材料是一种可调层间电子带的二维插层金属碳材料，许多方面要明显优于石墨烯，其电导率高达约104S cm-1，另外，Ti3C2Tx MXene由于其可调谐能带、功函数和费米能级等特性，在光电领域有广阔的应用前景。因此，Ti3C2Tx MXene有望进一步诱导稀土氧化物的内部压电势，改变其价带和导带的倾角，增加非结合电子的数量，最终增强荧光强度，减少寿命衰减。
在此项专利中，通过简单的机械研磨的方法将8YSZ:Eu3+陶瓷材料和MXene材料混合在一起，成功的制备了一种MXene/8YSZ:Eu3+温敏热障涂层材料。结果表明，MXene/8YSZ:Eu3+温敏热障涂层材料是一种很有前途的热障涂层材料，具有良好的荧光强度、荧光衰减寿命以及温敏特性，可以更好的应用于热障涂层中来对热障涂层的服役温度进行实时监测。
发明内容
本发明的目的在于提供一种MXene/8YSZ:Eu3+温敏热障涂层材料的制备方法，其制备过程易操作、高效、省时。在已有的8YSZ:Eu3+陶瓷材料的基础上引入MXene纳米材料，所制备而得的MXene/8YSZ:Eu3+温敏热障涂层材料具备优异的荧光及温敏特性。众所周知，温敏热障涂层材料的主要特点是荧光特性及温敏特性。本发明研究的MXene/8YSZ:Eu3+温敏热障涂层材料及其制备方法能够在一定程度上满足热障涂层材料的性能追求。在具备其良好的荧光性能的同时还具有较长的荧光衰减寿命，良好的温敏特性等优点。
本发明为实现上述目的采用了以下技术方案：
(1)以ZrOCl2·8H2O、Y2O3和Eu2O3为原料，氨水为反应底液，聚乙二醇为分散剂，采用化学共沉淀法，将ZrOCl2·8H2O和Y2O3溶解于1mol/L的稀盐酸，将Eu2O3溶于去离子水，混合两个溶液，随后将混合溶液加入pH为10的NH3·H2O中，搅拌30min，加入质量分数为3.0wt％的聚乙二醇，继续搅拌30min，随后静置15h；将静置后的混合沉淀离心、洗涤、干燥，干燥完成后研磨，将研磨充分的粉末在马弗炉煅烧，煅烧温度100℃、保温4h，随后取出研磨，合成8YSZ:Eu3+陶瓷材料。
(2)以Ti3AlC2为原料，采用化学刻蚀法，将Ti3AlC2缓慢加入HF溶液中，室温下搅拌24h，离心、过滤、洗涤、干燥得到MXene材料。
(3)通过机械混合研磨的方法，将获得的8YSZ:Eu3+陶瓷材料中加入质量分数为0.6wt％的MXene材料，随后置于研钵中研磨1h，得到MXene/8YSZ:Eu3+温敏热障涂层材料。
本发明通过机械混合研磨的方法成功的制备了一种MXene/8YSZ:Eu3+温敏热障涂层材料。本发明制备工艺简单，省时，成本低。制备的MXene/8YSZ:Eu3+温敏热障涂层材料具有荧光强度高，荧光衰减寿命长，温敏性能好等优点。其中8YSZ:Eu3+陶瓷材料具有尺寸较小、熔点较低、热膨胀系数较高、韧性较好、热导率较低的特点，且具有较好地荧光性能，是热障涂层材料中应用较多的陶瓷材料。但是具有荧光淬灭性，当Eu3+的浓度较高时，其发光强度其衰减寿命会相应的降低，以及随着服役时间的增加，其荧光性能也会进一步减弱。MXene材料的引入可以解决这一问题，MXene材料具有强导电性、高导热性以及优异的压电性能，且高温稳定性较好，具有良好的光电效应广泛应用于光电领域来提高材料的发光性能。本发明为多组分复合材料的发展提供了良好的基础，为电磁波吸收材料的多组分复合方面提供了良好的设计思路。
本发明相对于其它纳米吸波材料具有的优点集中体现在以下几点：
(1)通过机械研磨法制备的MXene/8YSZ:Eu3+温敏热障涂层材料，MXene的引入不影响8YSZ:Eu3+陶瓷材料的晶体结构，8YSZ:Eu3+陶瓷材料室温下为稳定的四方相结构。
(2)MXene/8YSZ:Eu3+温敏热障涂层材料中，一部分8YSZ:Eu3+颗粒包覆在手风琴状的MXene外表面，而另一部分8YSZ:Eu3+陶瓷材料颗粒嵌入MXene层片间，MXene/8YSZ:Eu3+粒径为5μm。
(3)MXene材料的加入极大的提高了8YSZ:Eu3+陶瓷材料的发光强度以及荧光衰减寿命，改善了其高温稳定性以及温度敏感性。MXene/8YSZ:Eu3+温敏热障涂层材料的绝对灵敏度和相对灵敏度较8YSZ:Eu3+陶瓷材料均提高了1倍。
附图说明
图1为实施例1所制得的MXene/8YSZ:Eu3+温敏热障涂层材料的XRD图。
图2为实施例1所制得的MXene/8YSZ:Eu3+温敏热障涂层材料的SEM图。
图3为实施例1所制得的MXene/8YSZ:Eu3+温敏热障涂层材料的激发光谱图。
图4为实施例1所制得的MXene/8YSZ:Eu3+温敏热障涂层材料的发射光谱图。
图5为实施例1所制得的MXene/8YSZ:Eu3+温敏热障涂层材料的荧光衰减寿命图。
图6为实施例1所制得的MXene/8YSZ:Eu3+温敏热障涂层材料的变温光谱图。
图7为实施例1所制得的MXene/8YSZ:Eu3+温敏热障涂层材料的绝对灵敏度与相对灵敏度图。
具体实施方式
以下结合具体实施例对本发明作进一步详细的说明，但是这些实施例不以任何方式限制本发明的范围。
实施例1
一种MXene/8YSZ:Eu3+温敏热障涂层材料的制备方法,包括如下操作：
(1)按照化学计量比，称取一定质量的ZrOCl2·8H2O、Y2O3、Eu2O3。将ZrOCl2·8H2O溶于去离子水中，将Y2O3、Eu2O3溶解于1mol/L稀盐酸溶液中，随后分别搅拌、静置，待彻底溶解后，混合溶液，并利用磁力搅拌器搅拌30min；随后加入3wt％的聚乙二醇分散剂，继续搅拌30min。同时制备氨水的反应底液，将浓氨水加入烧杯中，用去离子水调整其pH至10，留作备用。待母液搅拌完成后，将混合溶液与浓氨水分别逐滴加入到反应底液中，保持反应过程中溶液的pH为10，直到反应结束。反应结束后，继续搅拌30min，然后静置15h以上，得到混合物沉淀。然后将混合物沉淀倒入离心管中，加入去离子水，放入离心机中，设置转速为8000rpm，离心3min。离心完成后倒掉上清液，继续加入去离子水，重复上述操作3到5次，直至溶液呈中性，然后用无水乙醇离心2次。将离心完成后的样品置于鼓风干燥箱中，60℃条件下保温15h烘干，随后取出，用研钵进行充分研磨，将研磨充分的粉末置于坩埚中，放入马弗炉中在800℃的温度下煅烧4h，随后取出，研磨充分，得到8YSZ:Eu3+陶瓷粉末。
(2)将10ml浓度为40-50％的HF的浓溶液加入聚四氟乙烯烧杯中，在室温下称取200-400目的Ti3AlC2粉末1.0000g缓慢加入HF溶液中，用保鲜膜封口，磁力搅拌24h。搅拌完成后将混合溶液倒入离心管中，加入去离子水进行离心，离心机转速为8000rpm，时间为6min，随后将上层溶液倒掉，继续加入去离子水进行离心，重复4-5次，直至溶液pH接近中性，随后放入鼓风干燥箱中50℃的温度下保温12h烘干，烘干完成后取出样品，留作备用。
(3)采用采用机械研磨混合的方法制备MXene/8YSZ:Eu3+温敏热障涂层材料，称取一定质量8YSZ:Eu3+陶瓷材料，然后加入0.6wt％的MXene材料，充分研磨，得到MXene/8YSZ:Eu3+温敏热障涂层材料。
将MXene/8YSZ:Eu3+温敏热障涂层材料进行XRD测试，从附图1中可以发现，与8YSZ:Eu3+陶瓷材料的XRD图谱相比，MXene/8YSZ:Eu3+材料中既存在8YSZ:Eu3+陶瓷材料的衍射峰，又存在MXene材料的特征峰。且复合材料中MXene和8YSZ:Eu3+材料的物相结构及组成没有改变，MXene材料表面官能团依然存在，8YSZ:Eu3+室温下依然为稳定的四方相结构。通过SEM测试，从附图2中可以发现大量的8YSZ:Eu3+粉末颗粒包裹着手风琴状的MXene，由于MXene层片间距与粉末颗粒直径相差较大，另一部分粉末颗粒嵌入到MXene片的中间。以上测试表明通过机械研磨，成功制备了MXene/8YSZ:Eu3+温敏热障涂层材料。将MXene/8YSZ:Eu3+温敏热障涂层材料进行荧光及温敏性能测试，从附图3、4和5中可以看出，样品在250nm的激发波长下，其发射光谱在591nm处的发光强度为6480162.5(a.u.)，荧光衰减寿命1.41ms。从附图6和7中可以看出，MXene/8YSZ:Eu3+温敏热障涂层材料随着温度的升高，其荧光强度不发生变化，且350K时，相对灵敏度SA(MXene/8YSZ:Eu3+)＝1.20％K-1@350K，绝对灵敏度SR(MXene/8YSZ:Eu3+)＝1.14％K-1@350K。从以上结果说明MXene/8YSZ:Eu3+温敏热障涂层材料具有良好的荧光以及温敏特性，可以应用于热障涂层中对其服役温度进行实时监测。
Claims (2)
1.一种MXene/8YSZ:Eu3+温敏热障涂层材料的制备方法，特征在于，采用化学共沉淀法与机械混合研磨法制备，主要步骤如下：
(1)采用化学共沉淀法，以ZrOCl2·8H2O、Y2O3和Eu2O3为原料，NH3·H2O为反应底液，聚乙二醇为分散剂，将ZrOCl2·8H2O和Y2O3溶解于1mol/L的稀盐酸，将Eu2O3溶于去离子水，混合两个溶液，随后将混合溶液加入pH为10的NH3·H2O中，搅拌30min，加入质量分数为3.0wt％的聚乙二醇，继续搅拌30min，随后静置15h；将静置后的混合沉淀离心、洗涤、干燥，干燥完成后研磨，将研磨充分的粉末在马弗炉煅烧，煅烧温度100℃、保温4h，随后取出研磨，合成8YSZ:Eu3+陶瓷材料。
(2)采用化学刻蚀法，以Ti3AlC2为原料，将其加入HF溶液中，常温下搅拌24h，随后离心、洗涤、干燥，得到MXene材料。
(3)通过机械混合研磨的方法，将获得的8YSZ:Eu3+陶瓷材料中加入质量分数为0.6wt％的MXene材料，随后置于研钵中研磨1h，得到MXene/8YSZ:Eu3+温敏热障涂层材料。
2.如权利要求1中所述的MXene/8YSZ:Eu3+温敏热障涂层材料。其特征在于，在250nm的激发波长下，发射光谱在591nm波长处，荧光强度可达到6480162.5(a.u.)，荧光衰减寿命1.41ms。350K时，相对灵敏度SA(MXene/8YSZ:Eu3+)＝1.20％K-1@350K，绝对灵敏度SR(MXene/8YSZ:Eu3+)＝1.14％K-1@350K，具有良好的荧光及温敏特性。
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| US20220106675A1 (en) * | 2019-07-22 | 2022-04-07 | Aecc Beijing Institute Of Aeronautical Materials | Method for fabricating thermal barrier coating having self-repair and temperature-sensitive functions |
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| US20220106675A1 (en) * | 2019-07-22 | 2022-04-07 | Aecc Beijing Institute Of Aeronautical Materials | Method for fabricating thermal barrier coating having self-repair and temperature-sensitive functions |
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| DONG YUNLONG ET AL.: "Effects of Ti3C2TX MXene on structure, morphology, fluorescence and temperature sensitive properties of Eu3+ doped 8YSZ powder", JOURNAL OF LUMINESCENCE, 17 March 2023 (2023-03-17), pages 2 - 2 * |
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