CN114232055A - 一种在镍基合金基材表面形成ysz复合涂层的方法 - Google Patents
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Abstract
本发明涉及一种在镍基合金基材表面形成YSZ复合涂层的方法，该方法包括以下步骤：将镍基合金基材切割、打磨、清洗后待用；将YSZ粉末、氧化铝粉末、分散剂溶液和溶剂混合搅拌均匀、超声，配制成电泳悬浮液；将镍基合金基材作为正极电极材料，石墨作为负极电极材料放入制备好的电泳悬浮液中，进行电泳沉积；将电泳沉积后的工件取出，进行热处理；将热处理后的工件在惰性氛围下进行烧结，烧结完成后冷却至室温后取出，即可在在镍基合金基材表面形成YSZ复合涂层。与现有技术相比，本发明具有操作简单，生产成本低等优点。
Description
技术领域
本发明涉及涂层制备技术领域，具体涉及一种在镍基合金基材表面形成YSZ复合涂层的方法。
背景技术
氧化锆由于具有融化温度高、热导系数低、抗弯强度高、硬度高、热膨胀系数高等优异的性能，广泛应用于航空航天、海洋船舶、汽车、生物等领域。
氧化锆有三种晶体形态，在不同温度下会发生转变，相的转变会引起体积的变化，容易使产品产生裂纹，限制了纯氧化锆在高温领域的应用，添加一定量的稳定剂能使氧化锆处于稳定。氧化钇稳定氧化锆(YSZ)使氧化锆处于四方晶相状态，其优异的稳定性、机械强度和耐久性，提升氧化锆不同相之间转变的稳定性，提高产品性能，在YSZ中添加一些其他氧化物可以结合各物质之间的优点，使材料性能得到提升。
目前制备YSZ涂层比较成熟的涂敷方法有：等离子喷涂法、物理气相沉积、电化学气相沉积、溶胶凝胶法、丝网印刷法、等离子-物理气相沉积等，但都存在一定缺陷，或有涂层结构不，或有制备成本高。电泳沉积以简单的操作、低成本制备YSZ涂层具有很大的优势。
电泳沉积是指在稳定的悬浮液中通过直流电场的作用，胶体的粒子在电极或沉积表面形成薄膜的过程，其过程属于颗粒共沉降制备工艺，具有许多显著的优点。第一，能够弥补传统的热障涂层制备技术而引发的涂层相变及开裂，沉积后的涂层在经过干燥和真空烧结使得高温合金基体与涂层之间的结合强度提高；第二，电泳沉积的基体形状没有限制，并且成膜厚度比较均匀；第三，电泳沉积过程一般是在有机溶剂中进行的，避免了由于水的电解而产生气体，影响复合涂层与基体的结合强度。除此以外，电泳沉积技术还具有设备操作简易，较低的生产成本，较高的沉积效率、沉积工艺易控制等优点。现有文献期刊中制备氧化锆涂层所采用的电泳沉积技术，绝大多数是阴极电泳沉积模式，制备的薄膜表面很平滑；而采用阳极电泳沉积法来制备的YSZ涂层及YSZ/Al2O3复合涂层，尚未见到相关的报道。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种操作简单，生产成本低的在镍基合金基材表面形成YSZ复合涂层的方法。
本发明的目的可以通过以下技术方案来实现：
一种在镍基合金基材表面形成YSZ复合涂层的方法，该方法包括以下步骤：
将镍基合金基材切割、打磨、清洗后待用；
将YSZ粉末、氧化铝粉末、分散剂溶液和溶剂混合搅拌均匀、超声，配制成电泳悬浮液；
将镍基合金基材作为正极电极材料，石墨作为负极电极材料放入制备好的电泳悬浮液中，进行电泳沉积；
将电泳沉积后的工件取出，进行热处理；
将热处理后的工件在惰性氛围下进行烧结，烧结完成后冷却至室温后取出，即可在在镍基合金基材表面形成YSZ复合涂层。
进一步地，所述的YSZ粉末和氧化铝粉末的质量比为9:(0-9)，优选9:(1-3)。
进一步地，所述的分散剂溶液和溶剂的体积比为1:(35-45)。
进一步地，所述分散剂溶液的浓度为0.1-0.25wt％；所述电泳悬浮液的固含量为1-20g/L。分散剂的添加可降低颗粒的团聚现象，提高悬浮液的稳定性。悬浮液中固含量也会影响沉积速率，高固含量可能导致颗粒团聚，加速颗粒沉降，固含量太低则沉积时间长，基体表面可能涂层缺损，将固含量控制在1-20g/L范围内可以使电泳沉积速率适中。
进一步地，所述的分散剂包括聚丙烯酸铵；所述的溶剂包括体积比为(0.5-2):1的无水乙醇和乙酰丙酮；所述的YSZ粉末粒径为0.05-0.5μm。研究发现，悬浮液固体颗粒粒径对电泳沉积时的迁移速率有很大影响，纳米级颗粒具有更强的能量，能获得更好的结构。
进一步地，所述搅拌的时间为2-8h，超声的时间为2-30min。
进一步地，正极电极与负极电极的间距为0.5-3cm。电极之间的极间距对沉积速率和电泳膜层的成膜性有一定影响，将极间距控制在0.5-3cm范围内，即可以提高电泳成膜的成膜性，又可以控制试验溶剂的量，节约环保。
进一步地，所述电泳沉积的电压为30-120V，时间为1-10min。电压过高可能导致涂层表面产生缺陷，电压过低则耗费时间过长，当低于临界电压之下时，则不会发生沉积，将电压控制在30-120V范围内，可以有效的保证涂层的成膜质量。
进一步地，所述热处理的温度为60-200℃，热处理时间为1-3h。
进一步地，所述烧结的温度为1100-1250℃，烧结时间为4-10h。在该烧结温度和烧结时间范围内，涂层的性和表面质量等更好。
与现有技术相比，本发明提供一种制备YSZ及YSZ/Al2O3复合涂层的电泳沉积方法，采用少量聚丙烯酸铵作为分散剂，能够提高分散介质的电离度，提升悬浮液中颗粒的荷电性质，增强电泳沉积效果。
相较于用碘单质做分散剂的电泳沉积方法而言，聚丙烯酸铵使悬浮液颗粒表面带负电，因此颗粒最终沉积在阳极。通过控制各组分的配比及工艺参数，在镍基合金表面制备YSZ/Al2O3复合涂层，涂层均匀，烧结工艺简单，整体操作过程简单、仪器通用、易于控制，工艺周期短。
相比于现有的等离子喷涂和物理气相沉积等工艺，本发明的制备工艺生产成本更低。
附图说明
图1为本发明所制备YSZ涂层和YSZ/Al2O3复合涂层的SEM图；
图2为对比例3中1300℃烧结的复合涂层SEM图；
图3为本发明所用的镍基合金基底以及对比例1中YSZ涂层的XRD图谱，图中横坐标为衍射角度，纵坐标为相对强度；
图4为实施例1的复合涂层的显微结构图的XRD图谱，图中横坐标为衍射角度，纵坐标为相对强度。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，该方法包括以下步骤：
将镍基合金基材切割、打磨、清洗后待用；
将YSZ粉末、氧化铝粉末、分散剂溶液和溶剂混合搅拌均匀、超声，配制成电泳悬浮液；其中，YSZ粉末和氧化铝粉末的质量比为9:(0-9)。分散剂溶液和溶剂的体积比为1:(35-45)。分散剂溶液的浓度为0.1-0.25wt％；所述电泳悬浮液的固含量为1-20g/L。分散剂包括聚丙烯酸铵；所述的溶剂包括体积比为(0.5-2):1的无水乙醇和乙酰丙酮；YSZ粉末粒径为0.05-0.5μm。搅拌的时间为2-8h，超声的时间为2-30min。
将镍基合金基材作为正极电极材料，石墨作为负极电极材料放入制备好的电泳悬浮液中，进行电泳沉积；其中，正极电极与负极电极的间距为0.5-3cm。电泳沉积的电压为30-120V，时间为1-10min。
将电泳沉积后的工件取出，进行热处理；其中，热处理的温度为60-200℃，热处理时间为1-3h。
将热处理后的工件在惰性氛围下进行烧结，烧结完成后冷却至室温后取出，即可在在镍基合金基材表面形成YSZ复合涂层。其中，烧结的温度为1100-1250℃，烧结时间为4-10h。
实施例1
一种在镍基合金基材表面形成YSZ/Al2O3复合涂层的方法，包括以下步骤：
(1)将镍基合金基材进行加工、打磨、清洗，放入干燥箱烘干备用；
(2)将YSZ粉末、氧化铝粉末、聚丙烯酸铵溶液、混合溶剂[无水乙醇：乙酰丙酮＝1:1(v/v)]混合搅拌均匀，配制悬浮液；其中YSZ粉末粒径为0.2μm，悬浮液固含量为5g/L，YSZ：Al2O3＝9：1(w/w)，聚丙烯酸铵溶液溶度为0.15wt％。聚丙烯酸铵溶液和溶剂的体积比为PAA-NH4:EtOH-Acac＝1:40。
(3)将镍基合金作为正极，石墨作为负极放入悬浮液中，电极间距1cm，沉积电压60V，沉积时间为2min；
(4)将电泳沉积后的工件取出，放入鼓风干燥箱中进行热处理，热处理温度为80℃，热处理时间为2h。
(5)热处理后的工件放入管式高温烧结，在低压状态下、惰性氛围下进行烧结，烧结温度为1200℃，烧结时间为8h，烧结完成后待工件随炉冷却至室温后取出，即可在镍基合金表面形成涂层。
图1为本发明所制备YSZ涂层和YSZ/Al2O3复合涂层的SEM图，(a)、(b)分别为对比例1中YSZ涂层在100倍放大倍数下和50000倍放大倍数下的微观形貌图；(c)、(d)分别为实施例1中YSZ:Al2O3＝9:1时的复合涂层在100倍放大倍数下和20000倍放大倍数下的微观形貌图；(e)、(f)分别为对比例2中YSZ:Al2O3＝1:1时的复合涂层在100倍放大倍数下和20000倍放大倍数下的微观形貌图。图1中c、d中SEM结果表明，复合涂层的表面平整，与用其他方法制备的YSZ涂层结构类似，表面有一定孔隙率，在高温烧结后产生少量裂纹。
图4为实施例1的复合涂层的显微结构图的XRD图谱，图中横坐标为衍射角度，纵坐标为相对强度。
对比例1
与实施例1相比，区别仅在于悬浮液中固体颗粒未掺杂氧化铝，所得涂层结果如图1中a、b所示，涂层的孔隙率明显增加，并且裂纹数量明显增加，可见氧化铝颗粒的少量掺杂能够提高涂层的致密性，减少裂纹的产生。
图3为本发明所用的镍基合金基底以及对比例1中YSZ涂层的XRD图谱，图中横坐标为衍射角度，纵坐标为相对强度；
对比例2
与实施例1相比，区别仅在于YSZ：Al2O3的质量比例从9：1换成1：1，提高了氧化铝颗粒的掺杂比例。烧结结果如图1中e、f所示，与对实例1相比复合涂层的裂纹数量大幅度提高，孔隙率也有所提高。表明氧化铝颗粒的掺杂能提高涂层的表面质量，但含量过高也会使涂层质量变差。
对比例3
与实施例1相比，区别仅在于烧结温度的差异。在900℃下烧结8h后，基体表面涂层未陶瓷化，表明烧结温度过低，使得涂层结构并未发生较大改变；在1300℃烧结8h后，未沉积涂层的基体表面均碳化，表面有一层黑灰，表明烧结温度已超过基体承受范围。复合涂层结果如图2所示，通过在不同倍镜下可以观察到复合涂层的结构致密，但涂层表面裂纹增加，涂层表明凹凸不平。
图2为对比例3中1300℃烧结的复合涂层SEM图，(a)为50000倍放大倍数下的微观形貌图；(b)15000倍放大倍数下的微观形貌图；(c)为2000倍放大倍数下的微观形貌图；(d)为100倍放大倍数下的微观形貌图。
对比例4
与实施例1相比，差别仅在于沉积电压的差异。当在15V情况下沉积时，基体表面并未完全覆盖涂层；在150V情况下沉积，复合涂层的表面非常粗糙，因此以上情况下的涂层无法进行高温烧结处理。
实施例2
一种在镍基合金基材表面形成YSZ/Al2O3复合涂层的方法，包括以下步骤：
(1)将镍基合金基材进行加工、打磨、清洗，放入干燥箱烘干备用；
(2)将YSZ粉末、氧化铝粉末、聚丙烯酸铵溶液、混合溶剂[无水乙醇：乙酰丙酮＝1:1(v/v)]混合搅拌均匀，配制悬浮液；其中YSZ粉末粒径为0.2μm，悬浮液固含量为5g/L，YSZ：Al2O3＝7：3(w/w)，聚丙烯酸铵溶液溶度为0.15wt％。聚丙烯酸铵溶液和溶剂的体积比为PAA-NH4:EtOH-Acac＝1:40。
(3)将镍基合金作为正极，石墨作为负极放入悬浮液中，电极间距1cm，沉积电压60V，沉积时间为2min；
(4)将电泳沉积后的工件取出，放入鼓风干燥箱中进行热处理，热处理温度为80℃，热处理时间为2h。
(5)热处理后的工件放入管式高温烧结，在低压状态下、惰性氛围下进行烧结，烧结温度为1200℃，烧结时间为8h，烧结完成后待工件随炉冷却至室温后取出，即可在镍基合金表面形成涂层。
综上所述，本发明所用的阳极电泳沉积法成功在镍基合金基底上制备了YSZ/Al2O3复合涂层。从图1可看出，YSZ涂层在高温烧结后表面产生少量裂纹，并具有一定的孔隙率，氧化铝的少量掺杂可使涂层表面裂纹减少，孔隙率降低，而随着氧化铝量的增加，反而使涂层裂纹增加，由此可知，少量氧化铝掺杂可提高涂层的表面质量。当沉积电压过低时，基体表面不能获得完整涂层，电压过高，则沉积速率过快，使得涂层表面沉积质量差。当烧结温度较低时，基体表面涂层未能陶瓷化，依旧以粉末的形式附着在基体表面，而烧结温度过高，基体承受不住使表面碳化。
以上所述，仅是本发明的较佳实施例而已，并非是对本发明作其它形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。
Claims (10)
1.一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，该方法包括以下步骤：
将镍基合金基材切割、打磨、清洗后待用；
将YSZ粉末、氧化铝粉末、分散剂溶液和溶剂混合搅拌均匀、超声，配制成电泳悬浮液；
将镍基合金基材作为正极电极材料，石墨作为负极电极材料放入制备好的电泳悬浮液中，进行电泳沉积；
将电泳沉积后的工件取出，进行热处理；
将热处理后的工件在惰性氛围下进行烧结，烧结完成后冷却至室温后取出，即可在在镍基合金基材表面形成YSZ复合涂层。
2.根据权利要求1所述的一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，所述的YSZ粉末和氧化铝粉末的质量比为9:(0-9)。
3.根据权利要求1所述的一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，所述的分散剂溶液和溶剂的体积比为1:(35-45)。
4.根据权利要求1所述的一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，所述分散剂溶液的浓度为0.1-0.25wt％；所述电泳悬浮液的固含量为1-20g/L。
5.根据权利要求1所述的一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，所述的分散剂包括聚丙烯酸铵；所述的溶剂包括体积比为(0.5-2):1的无水乙醇和乙酰丙酮；所述的YSZ粉末粒径为0.05-0.5μm。
6.根据权利要求1所述的一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，所述搅拌的时间为2-8h，超声的时间为2-30min。
7.根据权利要求1所述的一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，正极电极与负极电极的间距为0.5-3cm。
8.根据权利要求1所述的一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，所述电泳沉积的电压为30-120V，时间为1-10min。
9.根据权利要求1所述的一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，所述热处理的温度为60-200℃，热处理时间为1-3h。
10.根据权利要求1所述的一种在镍基合金基材表面形成YSZ复合涂层的方法，其特征在于，所述烧结的温度为1100-1250℃，烧结时间为4-10h。
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| Title |
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| KEMAS A. ZAINI THOSIN: "A CRACK-FREE YSZ/AL2O3 COMPOSITE FILM COATING ONTO THE AISI-316L STEEL SUBSTRATE", 《MATERIALS SCIENCE AND TECHNOLOGY》, pages 165 - 172 * |
| LEYLA MOSTAFAPOUR ET. AL.: "Kinetic evaluation of YSZ/Al2O3 nanocomposite coatings fabricated by electrophoretic deposition on a nickel-based superalloy", 《PROCESSING AND APPLICATION OF CERAMICS》, vol. 15, no. 1, pages 1 - 10 * |
| 任超;何业东;王德仁;: "α-Al_2O_3/YSZ复合陶瓷涂层的抗高温氧化性能", 材料热处理学报, no. 12, pages 120 - 124 * |
| 张津;郭海明;李洪;何业东;: "32Cr2MoV钢表面电泳沉积氧化铝和氧化锆涂层", 中国表面工程, no. 04, pages 74 - 79 * |
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