CN112323014A - 一种渗铝硅-预氧化制备扩散阻挡层的方法 - Google Patents
一种渗铝硅-预氧化制备扩散阻挡层的方法 Download PDFInfo
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Abstract
本发明提供一种渗铝硅‑预氧化制备扩散阻挡层的方法,该方法是通过硅粉、铝粉按照一定比例混合,加入适当的粘结剂和蒸馏水配制成喷涂料浆,再使用喷涂的方式将料浆涂敷在零件待渗表面,涂敷的料浆层干燥后进行渗铝硅处理得到所需的铝硅渗层,然后通过高温预氧化在铝硅渗层表面生成一层氧化铝膜,该氧化铝膜层可以作为扩散阻挡层,能有效地阻挡高温合金基体与氧化铝膜外表面涂敷面层的互扩散。
Description
技术领域
本发明属于化学热处理金属表面加工领域,具体涉及一种渗铝硅-预氧化制备扩散阻挡层的方法。
背景技术
K424、GH536、GH3128合金为广泛使用在飞机发动机上的高温合金,具有较高的高温比强度,工作最高温度可达1000℃以上,这些高温合金某些涂层需要在高温服役过程中保持其本身的功能性,但在高温长时间的条件下,涂层与基体材料之间会发生互扩散,导致表面涂层失效。因此需要在基体材料与表面涂层之间制备扩散阻挡层,有效地阻止涂层与基体发生互扩散,保证涂层的性能。目前扩散阻挡层可以采用喷涂和电镀等方法直接制备,但直接采用喷涂和电镀的方法制备的扩散阻挡层与合金基体的结合强度一般,阻扩散不佳。本发明采用间接反应制备扩散阻挡层,制备的扩散阻挡层不仅阻扩散效果优异,而且结合强度良好。
发明内容
本发明的技术任务是针对以上现有技术的不足,而提供一种渗铝硅-预氧化制备扩散阻挡层的方法,本方法可以在基体金属与表面涂层之间形成稳定、连续、致密、完整的氧化铝膜层,有效地阻挡基体材料与表面涂层发生互扩散,保持表面涂层本身的性能。
本发明解决其技术问题所采用的技术方案是:一种渗铝硅-预氧化制备扩散阻挡层的方法,包括如下步骤:
(1)渗铝硅料浆配制:按蒸馏水(ml):粘结剂(ml):铝粉(g):硅粉(g)为5:50~60:30~40:4~6比例配制渗铝硅料浆并混匀,其中粘结剂组分及配比如下:蒸馏水(ml):氧化镁(g):三氧化铬(g):磷酸(ml)为5:0.5~1.5:0.5~1.5:1~3;其中所用磷酸的质量浓度≥85%;
(2)料浆涂敷:用喷枪将料浆均匀的喷涂在试件上,喷涂结束后对料浆层进行固化处理,固化温度为300~360℃,时间为1~2h;
(3)制备铝硅渗层:将试件置于真空炉内,控制真空炉温度为950~1030℃,保温4~5h;
(4)预氧化工序:将经渗铝后的试件进行高温预氧化处理,使试件的铝硅渗层表面生成氧化铝膜层作为扩散阻挡层。
进一步地,步骤(2)中试件表面采用多次喷涂的方式,喷涂要求料浆附着均匀,不流淌,喷涂次数为3~4,每次喷涂烘干后再进行下一次喷涂,每次喷涂的重量为10~20mg/cm2(烘干后重量)。
进一步地,喷涂后的烘干温度为100~150℃,保温时间不少于60min。
进一步地,步骤(3)真空炉的真空压强不大于6.65*10-1Pa。
进一步地,所述步骤(4)可采用真空预氧化、大气预氧化两种方式中的任意一种:
真空预氧化:将试件放入真空炉中,于900℃~1070℃,保温1h~4h,然后充氩冷却;
大气预氧化:将试件置于空气炉中,于760℃~950℃,保温3h~6h,然后空冷。
进一步地,真空预氧化时,在800℃以上升温和保温过程中,真空压强控制为100~220Pa。
进一步地,试件在进行步骤(2)的料浆涂敷前、步骤(4)的预氧化工序前,皆需要吹砂清理试件表面,去除试件表面附着物。
本发明通过渗铝硅和预氧化在在合金表面预置α-Al2O3层,即为扩散阻挡层,可以作为基体与基体表面面层的粘结层,能够阻止基体中镍等合金元素与表面的功能面层发生互扩散,以保证面层的完整连续,进而保持表面涂层的功能性,同时也可以改善材料表面的抗氧化性、抗腐蚀性、硬度、耐磨性等,在高温合金制件防护涂层领域具有广泛的价值。
与现有技术相比,本发明的有益效果为:本发明的优点在于:
1.本发明形成的氧化铝阻挡层完整、连续、致密且在高温长时间下稳定存在;氧化铝阻挡层能够有效的阻挡表面涂层和基体材料发生互扩散,经900℃保温300h耐热试验后,表面涂层仍完好,保持其本身的特性;
2.本发明所涉及到的化学热处理和真空或常规热处理方法不受制件形状和结构的限制,工艺适应性强;
3.本发明亦可实现制件局部制备扩散阻挡层,且本发明所需的原材料成本低,工艺简单,生产效率高,对制件形状和结构的适应性强,生产效率高,具有广泛的应用前景。
附图说明
图1是实施例1试件经渗铝硅-预氧化后的截面形貌;
图2是是实施例1试件的氧化铝阻挡层经耐热试验后的表面形貌图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明,实施例中所用试剂为市售分析纯试剂,其中磷酸的质量浓度≥85%。
实施例1
(1)干吹砂:刚玉砂吹净试件表面氧化物及脏污,风压不大于0.3MPa;
(2)粘结剂配制:按蒸馏水(ml):氧化镁(g):三氧化铬(g):磷酸(ml)=5:1:1:2比例称量配制成粘结剂,粘结剂混合后搅拌不少于1h;
(3)渗铝硅料浆配制:按蒸馏水(ml):粘结剂(ml):铝粉(g):硅粉(g)=5:55:35:5的比例配制成渗铝硅料浆,球磨24h以上才能使用;
(4)料浆涂敷:用喷枪将料桨均匀的喷涂在试件上,喷涂要求料浆附着均匀,不流淌,喷涂4次,每次喷涂后在烘箱中烘干后再进行下一次喷涂,烘干温度为150℃,保温时间为60min;每次喷涂的重量为15mg/cm2(烘干后重量);
(5)料浆层的固化处理:固化温度为300℃,时间为1.5h;
(6)制备铝硅渗层:试件装入马弗罐中,盖上盖子,将马弗罐装入真空炉内,将真空炉升温到980℃,保温5h,真空压强不大于6.65*10-1Pa;
(7)液体吹砂:待炉内温度冷却至室温,取出试件,吹砂清理试件表面,去除表面附着物;
(8)真空预氧化:将试件干燥后放入真空炉,于1050℃,保温2h,然后充氩冷却,在800℃以上升温和保温过程中,真空压强控制为150~180Pa。
其中,图1是本实施例试件渗铝硅-预氧化后的截面形貌,铝硅渗层的渗层深度在0.02mm~0.06mm,表面形成0.5μm~2μm的氧化铝膜;图2是试件在氧化铝阻挡层表面涂敷面层,经900℃,300h耐热试验后的表面形貌,表面仍呈现面层涂层本身的金属银白色,表面无划伤、起皱、鼓泡、开裂、翘皮、脱落等现象说明基体材料与面层未发生互扩散。
实施例2
(1)干吹砂:刚玉砂吹净试件表面氧化物及脏污,风压不大于0.3MPa;
(2)粘结剂配制:按蒸馏水(ml):氧化镁(g):三氧化铬(g):磷酸(ml)=5:0.8:1.5:3比例称量配制成粘结剂,粘结剂混合后搅拌不少于1h;
(3)渗铝硅料浆配制:按蒸馏水(ml):粘结剂(ml):铝粉(g):硅粉(g)=5:55:40:4配制,球磨24h以上才能使用;
(4)料浆涂敷:用喷枪将料桨均匀的喷涂在试件上,喷涂要求料浆附着均匀,不流淌,喷涂3次,每次喷涂后在烘箱中烘干后再进行下一次喷涂,烘干温度为120℃,保温时间100min;每次喷涂的重量为20mg/cm2(烘干后重量);
(5)料浆层的固化处理:固化温度为360℃,时间为2h;
(6)制备铝硅渗层:试件装入马弗罐中,盖上盖子,将马弗罐装入真空炉内,将真空炉升温到1030℃,保温4.5h,真空压强不大于6.65*10-1Pa;
(7)液体吹砂:待炉内温度冷却至室温,取出试件后,吹砂清理试件表面,去除表面附着物;
(8)大气预氧化:将试件干燥后置于空气炉中,于950℃,保温4h,然后空冷。
本实施例试件渗铝硅-预氧化后的截面形貌,铝硅渗层的渗层深度在0.02mm~0.06mm,表面形成0.5μm~2μm的氧化铝膜;试件在氧化铝阻挡层表面涂敷面层,经900℃,300h耐热试验后的表面仍呈现面层涂层本身的金属银白色,表面无划伤、起皱、鼓泡、开裂、翘皮、脱落等现象说明基体材料与面层未发生互扩散。
以上技术方案阐述了本发明的技术思路,不能以此限定本发明的保护范围,凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上技术方案所作的任何改动及修饰,均属于本发明技术方案的保护范围。
Claims (7)
1.一种渗铝硅-预氧化制备扩散阻挡层的方法,其特征在于,包括如下步骤:
(1)渗铝硅料浆配制:按蒸馏水(ml):粘结剂(ml):铝粉(g):硅粉(g)为5:50~60:30~40:4~6比例配制渗铝硅料浆并混匀,其中粘结剂组分及配比如下:蒸馏水(ml):氧化镁(g):三氧化铬(g):磷酸(ml)为5:0.5~1.5:0.5~1.5:1~3;其中所用磷酸的质量浓度≥85%;
(2)料浆涂敷:用喷枪将料浆均匀的喷涂在试件上,喷涂结束后对料浆层进行固化处理,固化温度为300~360℃,时间为1~2h;
(3)制备铝硅渗层:将试件置于真空炉内,控制真空炉温度为950~1030℃,保温4~5h;
(4)预氧化工序:将经渗铝后的试件进行高温预氧化处理,使试件的铝硅渗层表面生成氧化铝膜层作为扩散阻挡层。
2.根据权利要求1所述的一种渗铝硅-预氧化制备扩散阻挡层的方法,其特征在于,步骤(2)中试件表面采用多次喷涂的方式,喷涂次数为3~4,每次喷涂烘干后再进行下一次喷涂,每次喷涂的重量为10~20mg/cm2(烘干后重量)。
3.根据权利要求2所述的一种渗铝硅-预氧化制备扩散阻挡层的方法,其特征在于,喷涂后的烘干温度为100~150℃,保温时间不少于60min。
4.根据权利要求1所述的一种渗铝硅-预氧化制备扩散阻挡层的方法,其特征在于,步骤(3)真空炉的真空压强不大于6.65*10-1Pa。
5.根据权利要求1所述的一种渗铝硅-预氧化制备扩散阻挡层的方法,其特征在于,所述步骤(4)可采用真空预氧化、大气预氧化两种方式中的任意一种:
真空预氧化:将试件放入真空炉中,于900℃~1070℃,保温1h~4h,然后充氩冷却;
大气预氧化:将试件置于空气炉中,于760℃~950℃,保温3h~6h,然后空冷。
6.根据权利要求5所述的一种渗铝硅-预氧化制备扩散阻挡层的方法,其特征在于,所真空预氧化时,在800℃以上升温和保温过程中,真空压强控制为100~220Pa。
7.根据权利要求1所述的一种渗铝硅-预氧化制备扩散阻挡层的方法,其特征在于,试件在进行步骤(2)的喷涂前、步骤(4)的预氧化工序前,皆需要吹砂清理试件表面,去除试件表面附着物。
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