CN108504977A - 一种钛合金抗高温氧化涂层的制备方法 - Google Patents
一种钛合金抗高温氧化涂层的制备方法 Download PDFInfo
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Abstract
本发明公开一种钛合金抗高温氧化涂层的制备方法。其制备步骤为:用砂纸打磨基体的氧化皮,然后依次置于丙酮、无水乙醇中超声清洁,最后采用棕刚玉砂喷砂处理;采用超音速火焰喷涂在基体表面制备涂层;在所制备的涂层表面蒸镀金属铝;最后再热扩散处理上述沉积有金属铝的涂层。本发明的特点在于通过金属铝与金属间涂层的热扩散反应,能提高TiA13的相含量,所制备的涂层致密性更高,从而具有优异的抗高温氧化性能。
Description
技术领域
本发明涉及一种钛合金抗高温氧化涂层的制备方法,属于材料化学领域。
背景技术
钛是20世纪50年代发展起来的一种重要的结构金属,钛合金具有相对密度小、比强度高等特点被广泛应用于航空航天领域,被誉为“太空金属”。钛合金具有优异的抗腐蚀能力、无磁性等,是一种优秀的军用舰船结构材料,被誉为“海洋金属”。近年来,随着钛工业的不断发展,钛合金在民用领域中也得到了广泛应用,如汽车、建筑、医学、文体用品等方面,被誉为“全能金属”。
但是,钛合金仍存在一些缺陷,如耐磨性差、易氧化等缺点。通过表面处理在钛合金表面制备Ti-Al系金属间化合物涂层可以改善以上缺点,这类涂层不仅具有很好的高温抗氧化和抗热腐蚀性能,而且有很好的韧性和抗热疲劳强度。其中,TiA13在氧化过程中能形成单一的外Al2O3膜,最具高温抗氧化性能。
通常,对钛合金进行固体粉末包埋渗铝,通过高温扩散反应可以在钛合金表面获得富含TiAl3相的涂层,但是,这类方法有一个严重缺点,涂层与基体的互扩散容易导致基体性能下降,对于钛合金来说,影响尤为显著。另外,扩散反应难形成高含量的TiA13。相比较下,采用物理或化学沉积涂层则具有成本低,实用性高的特点。这类涂层不易与基体发生扩散,由于工艺温度较低,对钛合金的力学性能影响也较小。其中,热喷涂方法已被广泛用于制备具有一定致密度和结合强度的耐磨抗蚀涂层。据此,申请号为201510820050.9的发明专利“一种钛合金TiA13-Al复合涂层制备方法”将TiA13粉与纯Al粉按比例混合,采用低温超音速火焰喷涂方法或冷喷涂方法在钛合金基材表面制备涂层。但是,热喷涂所制备的涂层具有明显的层状结构,涂层中容易产生气孔,且涂层与基体之间的结合大多是机械结合,难以满足重载条件下的服役要求。基于此现状,本发明提供一种新的钛合金抗高温氧化涂层的制备方法。
发明内容
本发明的目的之一是针对现有技术中存在的缺陷或不足,提供一种钛合金抗高温氧化涂层的制备方法,其具体制备步骤如下:
(1)用砂纸打磨基体的氧化皮,然后依次置于丙酮、无水乙醇中超声清洁,去除基体表面的油污、氧化物以及其他杂物,最后采用24#棕刚玉砂喷砂处理,喷砂压力为0.2~0.4MPa;
(2)采用超音速火焰喷涂在基体表面制备厚度为50~200μm的涂层;
(3)在步骤2制备的涂层表面蒸镀一层厚度为5~10μm的金属铝;
(4)热扩散处理上述沉积有金属铝的涂层。
步骤(2)所述超音速火焰喷涂的喂料是:TiA13破碎料或团聚粉末,粒径为15~40μm。
步骤(2)所述超音速火焰喷涂的参数是:燃烧室压力1.5~2.4MPa,氧气流量700~900L/min,煤油流量15~25L/h,喷枪移动速率700~1000mm/s,喷涂距离100~200mm。
所述蒸镀金属铝的参数是:蒸发功率10~12kW,蒸发时间为50~100s,真空度高于10-4pa。
所述热扩散处理的条件是:700~950℃保温1~2h,升温速率为30℃/min,氩气气氛保护,流量为100~300L/h。
本发明的有益效果:
1.与常规热喷涂方法所制备涂层相比,本技术中铝热扩散至涂层内部,填充孔隙或间隙,所制备的涂层致密性高,从而具有更优异的抗高温氧化性能。
2.常规热喷涂方法所制备涂层的TiA13的相含量较低,而本技术通过铝与金属间涂层的扩散反应,能提高TiA13的相含量。
3.相比常规的热喷涂涂层,本技术采用热扩散处理,能同时增强涂层与基体间的结合。
附图说明
图1实施例1所制备涂层的断面SEM照片:(1)TC4基体;(2)涂层。
图2 TC4基体、对比涂层及实施例1所制备涂层的700℃静态氧化动力学曲线。
具体实施方式
实施例1
(1)用砂纸打磨TC4表面的氧化皮,然后依次置于丙酮、无水乙醇中超声5分钟,去除基体表面的油污、氧化物以及其他杂物,最后采用24#棕刚玉砂喷砂处理,喷砂压力为0.3MPa;
(2)以粒径为30μm的TiAl3粉末为喂料,通过超音速火焰喷涂在基体表面制备厚度50μm的涂层,所用参数为:燃烧室压力1.9MPa,氧气流量800L/min,煤油流量20L/h,喷枪移动速率850mm/s,喷涂距离150mm。
(3)在步骤2制备涂层表面蒸镀一层厚度为5μm的金属铝,所用参数为:蒸发功率为11kW,蒸发时间为50s,蒸镀过程中,排除涂层孔隙中的吸附空气,保持真空度优于10-4pa。
(4)在工业氩气气氛保护下热扩散处理上述沉积有金属铝的涂层,所用热扩散处理参数为:780℃保温1.5h,升温速率为30℃/min,氩气流量为200L/h。
(5)样品冷却至100℃后,停气自然冷却。
涂层与基体结合紧密,取涂层断面,分析其微观组织结构,结果如图1所示。涂层的致密性优异,未见明显的间隙或者空洞,TiA13的相含量为:98.9%。
实施例2
(1)用砂纸打磨TC4表面的氧化皮,然后依次置于丙酮、无水乙醇中超声5分钟,去除基体表面的油污、氧化物以及其他杂物,最后采用24#棕刚玉砂喷砂处理,喷砂压力为0.2MPa;
(2)以粒径为25μm的TiAl3粉末为喂料,通过超音速火焰喷涂在基体表面制备厚度150μm的涂层,所用参数为:燃烧室压力1.5MPa,氧气流量700L/min,煤油流量15L/h,喷枪移动速率700mm/s,喷涂距离100mm。
(3)在步骤2制备涂层表面蒸镀一层厚度为10μm的金属铝,所用参数为:蒸发功率为10kW,蒸发时间为100s,蒸镀过程中,排除涂层孔隙中的吸附空气,保持真空度优于10- 4pa。
(4)在工业氩气气氛保护下热扩散处理上述沉积有金属铝的涂层,所用热扩散处理参数为:700℃保温1h,升温速率为30℃/min,氩气流量为100L/h。
(5)样品冷却至100℃后,停气自然冷却。
涂层与基体结合紧密,TiA13的相含量为:98.4%。
实施例3
(1)用砂纸打磨TC4表面的氧化皮,然后依次置于丙酮、无水乙醇中超声5分钟,去除基体表面的油污、氧化物以及其他杂物,最后采用24#棕刚玉砂喷砂处理,喷砂压力为0.4MPa;
(2)以粒径为40μm的TiAl3粉末为喂料,通过超音速火焰喷涂在基体表面制备厚度200μm的涂层,所用参数为:燃烧室压力2.4MPa,氧气流量900L/min,煤油流量24L/h,喷枪移动速率1000mm/s,喷涂距离200mm。
(3)在步骤2制备涂层表面蒸镀一层厚度为10μm的金属铝,所用参数为:蒸发功率为12kW,蒸发时间为100s,蒸镀过程中,排除涂层孔隙中的吸附空气,保持真空度优于10- 4pa。
(4)在工业氩气气氛保护下热扩散处理上述沉积有金属铝的涂层,所用热扩散处理参数为:950℃保温2h,升温速率为30℃/min,氩气流量为200L/h。
(5)样品冷却至100℃后,停气自然冷却。
涂层与基体结合紧密,TiA13的相含量为:98.2%。
通过700℃静态氧化实验对比测试本发明实施例1制备的涂层与常规方法制备涂层的抗高温氧化性能,具体测试过程如下:采用精度为0.0001g的电子天平分别称重TC4基体、对比涂层(常规超音速火焰喷涂制备的涂层)以及实施例1所制备涂层,另采用螺旋测微仪精确测试各试样的长度与直径,计算试样的表面积;将三个试样一起放入Al2O3方舟并置于电阻炉,设置电阻炉30min升温至700℃并保持恒温;分别在1h、6h、24h、48h、72h、96h、200h、300h、500h、650h进行取样,将试样连同方舟一起取出后,待冷却至室温,使用电子天平称重,绘制氧化动力学曲线,见说明书附图2(图2)。
从图中可以看出,约氧化40h后,TC4基体骤然失重,说明TC4钛合金在700℃氧化时无法形成保护性氧化膜。而两种涂层在氧化初期的增重速度均较慢,表现了较好的抗氧化性能。但是,经过100h氧化,对比涂层氧化增重明显,而本发明的涂层则显示出更佳的抗氧化性能。
应当指出,上述实施方式可以使本领域的技术人员更全面的理解本发明,但不以任何方式限制本发明。因此,尽管本说明书对本发明已进行了详细说明,但是,本领域技术人员应当理解,仍然可以对本发明进行修改或者等同替换;而一切不脱离本发明实质的技术方案及其改进,均应涵盖在本发明专利的保护范围当中。
Claims (5)
1.一种钛合金抗高温氧化涂层的制备方法,其特征在于步骤如下:
(1)用砂纸打磨基体的氧化皮,然后依次置于丙酮、无水乙醇中超声清洁,去除基体表面的油污、氧化物以及其他杂物,最后采用24#棕刚玉砂喷砂处理,喷砂压力为0.2~0.4MPa;
(2)采用超音速火焰喷涂在基体表面制备厚度为50~200μm的涂层;
(3)在步骤2制备的涂层表面蒸镀一层厚度为5~10μm的金属铝;
(4)热扩散处理上述沉积有金属铝的涂层。
2.如权利要求1所述的一种钛合金抗高温氧化涂层制备方法,其特征在于步骤(2)所述超音速火焰喷涂的喂料是:TiA13破碎料或团聚粉末,粒径为15~40μm。
3.如权利要求1所述的一种钛合金抗高温氧化涂层制备方法,其特征在于步骤(2)所述超音速火焰喷涂的参数是:燃烧室压力1.5~2.4MPa,氧气流量700~900L/min,煤油流量15~25L/h,喷枪移动速率700~1000mm/s,喷涂距离100~200mm。
4.如权利要求1所述的一种钛合金抗高温氧化涂层制备方法,其特征在于所述蒸镀金属铝的参数是:蒸发功率10~12kW,蒸发时间为50~100s,真空度高于10-4pa。
5.如权利要求1所述的一种钛合金抗高温氧化涂层制备方法,其特征在于步骤(4)所述热扩散处理的条件是:700~950℃保温1~2h,升温速率为30℃/min,氩气气氛保护,流量为100~300L/h。
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