CN112458442B - 一种提高钛铝合金与氧化物涂层结合强度的制备方法 - Google Patents

一种提高钛铝合金与氧化物涂层结合强度的制备方法 Download PDF

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CN112458442B
CN112458442B CN202011316960.0A CN202011316960A CN112458442B CN 112458442 B CN112458442 B CN 112458442B CN 202011316960 A CN202011316960 A CN 202011316960A CN 112458442 B CN112458442 B CN 112458442B
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titanium
tio
aluminum alloy
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CN112458442A (zh
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何俊
张衍
马天驹
翟大鹏
张永和
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Lanzhou Institute of Physics of Chinese Academy of Space Technology
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Abstract

本发明属于高温抗氧化涂层技术领域，具体涉及一种提高钛铝合金与氧化物涂层结合强度的制备方法，包括如下步骤：步骤1，通过溶胶凝胶法在钛铝合金表面制备TiO2缓冲层；步骤2，利用高能氩离子对TiO2缓冲层表面进行离子轰击处理；步骤3，在离子轰击处理过的TiO2缓冲层表面浸涂料浆，烘干烧结后，完成钛铝合金与氧化物涂层的结合。本发明通过溶胶凝胶、高能离子轰击以及料浆烧结三种方式相结合的方法共同制备出高温抗氧化涂层，使钛铝合金与其氧化物涂层能够紧密结合，结合强度高，抗热抗震性能强。

Description

一种提高钛铝合金与氧化物涂层结合强度的制备方法
技术领域
本发明属于高温抗氧化涂层技术领域，具体涉及一种提高钛铝合金与氧化物涂层结合强度的制备方法。
背景技术
钛铝合金具有高弹性模量、低密度、高比强度等特点，使其成为航天飞机高温蒙皮、航空航天动力装置构件以及汽车发动机增压涡轮等零件的首要材料之一，被认为是最适合取代Ni基合金的高温轻质材料，但是钛铝合金的高温抗氧化性能仍有待进一步提高，尤其是当温度上升至800℃以上时，钛铝合金表面的氧化层会呈现出疏松的片状结构，并且产生大量孔隙，致使其抗氧化性能迅速下降，严重影响合金的性能，这种高温“氧脆”现象大大限制了钛铝合金在诸如喷射发动机内壁和叶片等高温工作环境的应用，因此，提高钛铝合金在高温下的抗氧化能力成为了当前该领域研究的重点。
表面抗氧化涂层的制备是最经济最易实现工业化应用的理想方案，钛铝合金表面的高温抗氧化涂层要求在给定温度和时间内下将循环暴露条件下的重量增加限制在1mg/cm2，并且要求膜层具有致密性、与基体之间良好的结合能力以及与基体相近的热膨胀系数(CTE)，因此作为基体成分之一的铝和钛所对应的氧化物便成为了比较合适的选择。现有技术大多数选择Al2O3作为氧化涂层，但是由于Al2O3具有较高的脆性及低于基体的CTE值，导致其在循环热震下容易出现开裂和剥离的现象，影响抗氧化的性能，因此如何提高合金与氧化物涂层的结合强度是目前亟待解决的问题。
发明内容
针对背景技术中存在的问题，本发明提供了一种提高钛铝合金与氧化物涂层结合强度的制备方法，通过溶胶凝胶、高能离子轰击以及料浆烧结三种方式相结合的方法共同制备出高温抗氧化涂层，使钛铝合金与其氧化物涂层能够紧密结合，结合强度高，抗热抗震性能强。
本发明提供了一种提高钛铝合金与氧化物涂层结合强度的制备方法，包括如下步骤：步骤1，通过溶胶凝胶法在钛铝合金表面制备TiO2缓冲层；步骤2，利用高能氩离子对TiO2缓冲层表面进行离子轰击处理；步骤3，在离子轰击处理过的TiO2缓冲层表面浸涂料浆，烘干烧结后，完成钛铝合金与氧化物涂层的结合。
进一步的，步骤1包括如下步骤：步骤11，配胶，将2.07-5.176ml的钛酸四丁酯搅拌加入到13.33-23.33ml的无水乙醇中配得A液体，将0.206-0.515ml的稀盐酸、0.216-0.54ml的去离子水以及4.174-10.435m的1无水乙醇混合配得B液体，将B液体缓慢注入A液体中，搅拌2-3h，陈化24-48h后得到30ml前驱体浓度为0.2-0.5mol/l的TiO2溶胶；步骤12，制备TiO2缓冲层，利用溶胶凝胶提拉法在钛铝合金表面涂敷TiO2溶胶，并在80-100℃温度下烘干20min，然后放入烧结炉中，以1℃/min的升温速率升温至700℃，保温1h后，获得TiO2缓冲层。
进一步的，步骤2包括如下步骤：步骤21，将步骤1中制备得到的钛铝合金与TiO2缓冲层放置到磁控溅射仪中，开启机械泵和分子泵抽真空至9×10-4Pa；步骤22，向磁控溅射仪中冲入氩气，控制溅射气压为0.1-1Pa，打开偏压电源，调控直流电源为0.1-0.3A，轰击TiO2缓冲层表面5-30min。
进一步的，步骤3包括如下步骤：步骤31，配制料浆，将原料Al2O3、TiO2、粘结剂Al(H2PO4)3、固化剂Na2SiO3、溶剂乙二醇甲醚和水按一定比例配成料浆；步骤32，浸涂料浆，在步骤22轰击处理后的TiO2缓冲层表面上均匀浸涂一层料浆，室温下水平静置1h，然后在200℃温度下烘干1h，烘干完成后，再浸涂一层料浆，并在空气中晾干，晾干后在80℃的温度下烘干1h，烘干完成后准备烧结；步骤33，烧结，将烘干完成浸涂料浆的涂层放入真空烧结炉中，保持7℃/min的升温速率，由室温升至120℃，然后保温1h，再由5℃/min的升温速率升至700-750℃，保温2h，最后随炉冷却至室温，完成钛铝合金与氧化物涂层的结合。
进一步的，步骤31中，粘结剂与固化剂按Al(H2PO4)3∶Na2SiO3＝9∶1的比例配制得到复合粘结剂。
进一步的，步骤31中，Al2O3和TiO2与复合粘结剂的配比为1.8∶1。
本发明提供的一种提高钛铝合金与氧化物涂层结合强度的制备方法，具有以下有益效果：
本发明通过溶胶凝胶、高能离子轰击以及料浆烧结三种方式相结合的方法共同制备出高温抗氧化涂层，首先纳米尺度的氧化物溶胶具有较强的吸附性，易与金属形成紧密的界面层；其次高能离子轰击的氧化物界面层可促进原子扩散，增加界面层与金属基体的结合力，同时缓冲界面应力集中；最后料浆烧结制备厚的氧化物涂层与界面层成分相近，易于结合。利用三种工艺制备带有界面层的高温抗氧化涂层不仅增强了界面扩散又缓冲了应力，提高了钛铝合金与氧化物涂层结合的强度，增强了其抗震抗热的性能，在1000℃的高温下热震15-20次也不会出现开裂和剥离的现象，大大提高了钛铝合金在高温下的抗氧化能力。
附图说明
为了更清楚的说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单的介绍，显而易见的，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其它附图。
图1为本发明钛铝合金与氧化物涂层结合的初始状态的示意图；
图2为本发明钛铝合金与氧化物涂层结合在高温环境下热震20次的示意图。
具体实施方式
下面将结合本发明中的附图，对本发明实施例中的技术方案进行清楚、完整的描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通的技术人员在没有做出创造性劳动的前提下所获得的所有其它实施例，都属于本发明的保护范围。
如图1所示，本发明实施例提供了一种提高钛铝合金与氧化物涂层结合强度的制备方法，包括如下步骤：步骤1，通过溶胶凝胶法在钛铝合金表面制备TiO2缓冲层；步骤2，利用高能氩离子对TiO2缓冲层表面进行离子轰击处理；步骤3，在离子轰击处理过的TiO2缓冲层表面浸涂料浆，烘干烧结后，完成钛铝合金与氧化物涂层的结合。
具体的，本发明实施例主要通过溶胶凝胶、高能离子轰击以及料浆烧结三种方式相结合的方法共同制备出高温抗氧化涂层，使钛铝合金与其氧化物涂层能够紧密结合，大大提高了结合强度，并且增强了抗热抗震性能，本发明实施例中制备出来的氧化物涂层主要指的是TiO2-Al2O3涂层，其中步骤1中采用溶胶凝胶法在钛铝合金表面制备TiO2缓冲层，主要为了充分利用纳米溶胶的吸附性，易与金属形成紧密的界面层，从而能够提高钛铝合金与TiO2缓冲层的结合强度，步骤2中在真空条件下用高能氩离子对TiO2缓冲层表面进行离子轰击处理，主要利用离子轰击的扩散性，增加界面层与金属基体的结合力，同时能够缓冲界面应力集中，提高钛铝合金与TiO2缓冲层的结合强度，步骤3中利用料浆(TiO2-Al2O3)烧结法，使钛铝合金表面烧结形成致密的TiO2-Al2O3涂层，大大提高了钛铝合金与TiO2-Al2O3涂层结合的强度，使得钛铝合金在高温的环境下拥有较强的抗氧化性和抗震性。
下面结合具体的实验数据对本发明实施例进行具体的说明：
进一步的，步骤1包括如下步骤：
步骤11，配胶，将5.176ml的钛酸四丁酯搅拌加入到13.33ml的无水乙醇中配得A液体，将0.515ml的稀盐酸、0.54ml的去离子水以及10.435ml的无水乙醇混合配得B液体，将B液体缓慢注入A液体中，搅拌2h，陈化24h后得到30ml前驱体浓度为0.5mol/l的TiO2溶胶；
步骤12，制备TiO2缓冲层，利用溶胶凝胶提拉法在钛铝合金表面涂敷TiO2溶胶，并在80-100℃温度下烘干20min，然后放入烧结炉中，以1℃/min的升温速率升温至700℃，保温1h后，获得TiO2缓冲层。
进一步的，步骤2包括如下步骤：
步骤21，将步骤1中制备得到的钛铝合金与TiO2缓冲层放置到磁控溅射仪中，开启机械泵和分子泵抽真空至9×10-4Pa；
步骤22，向磁控溅射仪中冲入氩气，控制溅射气压为0.1Pa，打开偏压电源，调控直流电源为0.1A，轰击TiO2缓冲层表面5min。
进一步的，步骤3包括如下步骤：
步骤31，配制料浆，将原料Al2O3、TiO2、粘结剂Al(H2PO4)3、固化剂Na2SiO3、溶剂乙二醇甲醚和水按一定比例配成料浆；其中，粘结剂与固化剂按Al(H2PO4)3∶Na2SiO3＝9∶1的份数比例配制得到复合粘结剂，Al2O3和TiO2与复合粘结剂的份数配比为1.8∶1。
步骤32，浸涂料浆，在步骤22轰击处理后的TiO2缓冲层表面上均匀浸涂一层料浆，室温下水平静置1h，然后在200℃温度下烘干1h，烘干完成后，再浸涂一层料浆，并在空气中晾干，晾干后在80℃的温度下烘干1h，烘干完成后准备烧结，此外，浸涂提拉的速度会影响涂层的厚度和均匀性，因此，基片在提拉浸涂料浆时要保持匀速拉动，使涂层保持均匀；
步骤33，烧结，将烘干完成浸涂料浆的涂层放入真空烧结炉中，保持7℃/min的升温速率，由室温升至120℃，然后保温1h，再由5℃/min的升温速率升至700-750℃，保温2h，最后随炉冷却至室温，制备得到TiO2-Al2O3涂层，完成钛铝合金与氧化物涂层的结合。
如图2所示，采用本发明实施例制备得到的氧化物涂层，能够使钛铝合金在1000℃高温下热震15-20次，不会出现开裂和剥离的现象，大大提高了钛铝合金与氧化物涂层结合的强度。
以上借助具体实施例对本发明做了进一步描述，但是应该理解的是，这里具体的描述，不应理解为对本发明的实质和范围的限定，本领域内的普通技术人员在阅读本说明书后对上述实施例做出的各种修改，都属于本发明所保护的范围。

Claims (3)

1.一种提高钛铝合金与氧化物涂层结合强度的制备方法，其特征在于，包括如下步骤：
步骤1，通过溶胶凝胶法在钛铝合金表面制备TiO2缓冲层；
步骤11，配胶，将2.07-5.176ml的钛酸四丁酯搅拌加入到13.33-23.33ml的无水乙醇中配得A液体，将0.206-0.515ml的稀盐酸、0.216-0.54ml的去离子水以及4.174-10.435ml的无水乙醇混合配得B液体，将B液体缓慢注入A液体中，搅拌2-3h，陈化24-48h后得到30ml前驱体浓度为0.2-0.5mol/l的TiO2溶胶；
步骤12，制备TiO2缓冲层，利用溶胶凝胶提拉法在钛铝合金表面涂敷TiO2溶胶，并在80-100℃温度下烘干20min，然后放入烧结炉中，以1℃/min的升温速率升温至700℃，保温1h后，获得TiO2缓冲层；
步骤2，利用高能氩离子对TiO2缓冲层表面进行离子轰击处理；
步骤21，将步骤1中制备得到的钛铝合金与TiO2缓冲层放置到磁控溅射仪中，开启机械泵和分子泵抽真空至9×10-4Pa；
步骤22，向磁控溅射仪中冲入氩气，控制溅射气压为0.1-1Pa,打开偏压电源，调控直流电源为0.1-0.3A，轰击TiO2缓冲层表面5-30min；
步骤3，在离子轰击处理过的TiO2缓冲层表面浸涂料浆，烘干烧结后，完成钛铝合金与氧化物涂层的结合；
步骤31，配制料浆，将原料Al2O3、TiO2、粘结剂Al(H2PO4)3、固化剂Na2SiO3、溶剂乙二醇甲醚和水按一定比例配成料浆；
步骤32，浸涂料浆，在步骤22轰击处理后的TiO2缓冲层表面上均匀浸涂一层所述料浆，室温下水平静置1h，然后在200℃温度下烘干1h,烘干完成后，再浸涂一层所述料浆，并在空气中晾干，晾干后在80℃的温度下烘干1h，烘干完成后准备烧结；
步骤33，烧结，将烘干完成浸涂料浆的涂层放入真空烧结炉中，保持7℃/min的升温速率，由室温升至120℃，然后保温1h，再由5℃/min的升温速率升至700-750℃，保温2h，最后随炉冷却至室温，完成钛铝合金与氧化物涂层的结合。
2.根据权利要求1所述的提高钛铝合金与氧化物涂层结合强度的制备方法，其特征在于，所述步骤31中，所述粘结剂与所述固化剂按Al(H2PO4)3：Na2SiO3＝9:1的比例配制得到复合粘结剂。
3.根据权利要求2所述的提高钛铝合金与氧化物涂层结合强度的制备方法，其特征在于，所述步骤31中，所述Al2O3和所述TiO2与所述复合粘结剂的配比为1.8：1。
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