CN110643951B - 一种抗高温氧化的铝铬硅氮与氧化铝多层复合涂层及其制备方法 - Google Patents
一种抗高温氧化的铝铬硅氮与氧化铝多层复合涂层及其制备方法 Download PDFInfo
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Abstract
本发明公布的抗高温氧化的铝铬硅氮与氧化铝多层复合涂层是由CrAlTiZrY高熵合金粘结层、α‑Cr2O3氧化物模板层、α‑Al2O3氧化物核心层、AlCrSiN氮化物表层四个子层构成的整体,这四个子层的顺序是由内至外,涂层总厚度为1~3μm。其制备方法为:对基底进行加热和离子刻蚀后,先利用电弧蒸发镀工艺在基底上沉积CrAlTiZrY层;然后,使用阴极电弧离子镀工艺,再继续依次沉积α‑Cr2O3层、α‑Al2O3层和AlCrSiN层。由于各子涂层的抗氧化协同作用,铝铬硅氮与氧化铝多层复合涂层的抗高温氧化性能被进一步提高,并且涂层的耐磨性能好,制备工艺简单,易于实施,适合工业化生产与应用。
Description
技术领域
本发明属于切削刀具表面涂层技术领域,具体涉及一种抗高温氧化的铝铬硅氮与氧化铝多层复合涂层及其制备方法。
背景技术
随着切削加工技术的发展进步和切削加工要求的提高,切削刀具包括其表面上的涂层材料面临挑战。以干切屑、高速切削为代表的新切削技术的特点是,切削区域温度升高,刀具切削部位承受的温度相应提高,因此涂层刀具除了表面磨损失效之外,涂层也时常发生氧化失效。氮化物硬质涂层是切削刀具表面上广泛使用的涂层材料,氮化物涂层在高温条件下易与空气中的氧气作用,氮化物转变成氧化物,晶格膨胀,很容易剥落。因此,氮化物硬质涂层在干切屑、高速切削条件下的应用面临难题。氧化物涂层的优势是涂层本身是氧化物,不存在涂层氧化的问题或者涂层自身就是抗氧化的,这类涂层更适宜于刀具在高温条件下工作。α-Al2O3由于结构致密、化学稳定性好、热稳定性好以及具有较高的硬度和韧性,是高温条件下切削加工的理想刀具表面涂层材料。
物理气相沉积法是制备刀具涂层材料的重要方法,该法沉积温度低,适用于多种基底材料的表面涂层处理。但是,由于物理气相沉积法的沉积温度低,导致该方法沉积α-Al2O3的能量不足,物理气相沉积法制备的Al2O3涂层通常为非晶态或其它晶形结构,难以获得理想的使用效果。另外,Al2O3涂层硬度较氮化物涂层低,单一的Al2O3涂层抗磨损性能不足,具有复杂结构的涂层体系是今后涂层的重要发展方向。
发明内容
本发明的目的是克服现有技术存在的问题,提供一种抗高温氧化的铝铬硅氮与氧化铝多层复合涂层。
本发明的另一目的是提供一种上述抗高温氧化的铝铬硅氮与氧化铝多层复合涂层的制备方法。
本发明提供的抗高温氧化的铝铬硅氮与氧化铝多层复合涂层,其特征在于,涂层是由高熵合金粘结层、氧化物模板层、氧化物核心层、氮化物表层四个子层构成的整体,这四个子层的顺序是由内至外,涂层总厚度为1~3μm。
其中,上述涂层中,所述高熵合金粘结层为CraAlbTicZrdYe,a+b+c+d+e=1,a、b、c、d、e的取值范围为0.15~0.4,厚度为50~200nm。
其中,上述涂层中,所述氧化物模板层为α-Cr2O3,厚度为150~300nm;所述氧化物核心层为α-Al2O3,厚度为500~2000nm;所述氮化物表层为AlCrSiN,厚度为300~500nm。
本发明提供的上述抗高温氧化的铝铬硅氮与氧化铝多层复合涂层的制备方法,包括以下步骤:
A、将清洁的基底材料装入涂层设备真空室中,抽真空并加热;
B、对基底表面进行离子刻蚀;
C、利用电弧蒸镀工艺制备高熵合金粘结层;
D、利用阴极电弧镀膜工艺制备氧化物模板层;
E、利用阴极电弧镀膜工艺制备氧化物核心层;
F、利用阴极电弧镀膜工艺制备氮化物表层。
其中,上述方法步骤A中,所述抽真空并加热是先将背底真空抽至0.03Pa及以下时,打开炉壁的辅助加热装置对基底进行加热,同时打开机架转动电源使基底在真空室内进行自转和公转运动,至基底温度达到380℃。
其中,上述方法步骤B中,所述离子刻蚀是向真空室中通入氩气,调节氩气流量保证压强为0.1~0.25Pa,然后对基底施加-100~-200V的直流偏压和-200~-400V的脉冲偏压,利用离化的Ar+对基底表面进行刻蚀,刻蚀30~90min。
其中,上述方法步骤C中,所述电弧蒸镀工艺制备高熵合金粘结的工作压强为0.1~0.2Pa,蒸镀坩埚上通过的电弧电流为180~220A,蒸镀坩埚内放置的材料为CraAlbTicZrdYe高熵合金, a+b+c+d+e=1,a、b、c、d、e的取值范围为0.15~0.4,蒸镀时间为5~10min。
其中,上述方法步骤D中,所述阴极电弧镀膜工艺制备氧化物模板层的工作气体为Ar+O2,工作压强为1.5~3.5Pa,工作靶材为Cr电弧靶,靶电流为50~100A,基底施加的偏压为-30~-80V,沉积时间10~20min。
其中,上述方法步骤E中,所述阴极电弧镀膜工艺制备氧化物核心层的工作气体为Ar+O2,工作压强为1.0~3.0Pa,工作靶材为Al电弧靶,靶电流为80~120A,基底施加的偏压为-30~-80V,沉积时间40~150min。
其中,上述方法步骤F中,所述阴极电弧镀膜工艺制备氮化物表层的工作气体为N2,工作压强为1.5~3.5Pa,工作靶材为AlCrSi合金电弧靶,靶电流为80~120A,基底施加的偏压为-30~-80V,沉积时间20~35min。
本发明与现有技术相比,具有如下优点:
1)本发明提供的抗高温氧化的铝铬硅氮与氧化铝多层复合涂层由功能与成分均不同的四个子层构成,首先,高熵合金粘结层相比于传统的Cr、Ti纯金属粘结层及TiAl合金粘结层而言,具有更高的强韧性,能在刀具基底材料与表面涂层材料之间起到很好的粘结作用,使涂层与基底结合稳固;其次,使用的α-Cr2O3氧化物模板层有利于Al2O3按照α-Cr2O3的晶体结构结构外延生长,解决了物理气相沉积法由于温度低制备α-Al2O3困难的问题;再次,α-Al2O3氧化物核心层与AlCrSiN氮化物表层相结合,避免了单纯氧化物涂层硬度低、耐磨性不足的问题和单纯氮化物涂层抗高温氧化性能低的问题。
2)本发明提供的抗高温氧化的铝铬硅氮与氧化铝多层复合涂层的制备方法是一种以阴极电弧沉积为主、蒸发镀工艺制备粘结层为辅的组合式离子镀工艺。镀膜前通过加热使基底材料中吸附的杂质释放,同时采用离化的Ar+对基底表面进行轰击刻蚀,增强了涂层与基底的结合;采用电弧蒸镀工艺蒸发高熵合金材料,在基底上沉积高熵合金粘结层,进一步地增强涂层与基底的结合能力,电弧蒸发镀制备粘结层的优势是,沉积速率快,蒸发原料的尺寸、形状几乎不受限制,称重后装入蒸发坩埚内即可,而采用阴极电弧离子镀沉积粘结层,则需要将蒸发原料制成具有一定形状和尺寸的靶材;阴极电弧离子镀过程中的粒子离化率高且离子能量高,相比磁控溅射更容易获得α-Al2O3。在沉积涂层过程中,通过切换不同的电弧靶工作,很容易多层复合涂层的制备,操作工艺简单且易于掌握和控制。
具体实施方式
下面通过具体实施例对本发明作进一步的说明,但本发明保护的内容不局限于以下实施例。
实施例1
将清洁的金属陶瓷基底装入等离子体增强复合式离子镀膜系统的真空室中,待背底真空抽至0.02Pa时,打开炉壁的辅助加热装置对基底进行加热,同时打开转动电源使基底不停地转动,加热至基底温度达到380℃;然后向真空室中通入氩气,调节氩气流量保证压强为0.1Pa,然后对基底施加-200V的直流偏压和-400V的脉冲偏压,利用离化的Ar+对基底表面进行刻蚀,刻蚀60min;依次关闭基底偏压、调节氩气流量,保证工作压强为0.15Pa,开启蒸发镀主弧电源进行蒸发镀膜,坩埚上的主弧电流为180A,蒸发原料为Cr0.2Al0.2Ti0.2Zr0.2Y0.2块,蒸发沉积10min;关闭主弧电源,开启Cr电弧靶,靶电流设为70A,向真空室内通入氧气,调节氩气和氧气流量使工作压强为2.5Pa,对基底施加偏压-50V,沉积12min;开启Al电弧靶,靶电流设为80A,然后关闭Cr电弧靶电源,工作压强和基底偏压保持不变继续沉积120min;开启AlCrSi合金电弧靶,靶电流设为100A,然后关闭Al电弧靶电源,通入氮气、关闭氧气和氩气,调节气体流量,控制工作压强为2.0Pa,基底偏压继续保持不变,沉积30min结束。制备的抗高温氧化的铝铬硅氮与氧化铝多层复合涂层由CrAlTiZrY高熵合金粘结层、α-Cr2O3氧化物模板层、α-Al2O3氧化物核心层和AlCrSiN氮化物表层共四个子层组成,各个子层之间以及涂层与基底结合良好,在高温条件下具有良好的抗氧化性能。
实施例2
将清洁的硬质合金基底装入等离子体增强复合式离子镀膜系统的真空室中,待背底真空抽至0.03Pa时,打开炉壁的辅助加热装置对基底进行加热,同时打开转动电源使基底不停地转动,加热至基底温度达到380℃;然后向真空室中通入氩气,调节氩气流量保证压强为0.25Pa,然后对基底施加-200V的直流偏压和-350V的脉冲偏压,利用离化的Ar+对基底表面进行刻蚀,刻蚀30min;依次关闭基底偏压、调节氩气流量,保证工作压强为0.2Pa,开启蒸发镀主弧电源进行蒸发镀膜,坩埚上的主弧电流为210A,蒸发原料为Cr0.2Al0.2Ti0.2Zr0.2Y0.2块,蒸发沉积6min;关闭主弧电源,开启Cr电弧靶,靶电流设为80A,向真空室内通入氧气,调节氩气和氧气流量使工作压强为3.0Pa,对基底施加偏压-80V,沉积15min;开启Al电弧靶,靶电流设为90A,然后关闭Cr电弧靶电源,调节气体流量,控制压强为2.5Pa,基底偏压保持不变继续沉积150min;开启AlCrSi合金电弧靶,靶电流设为120A,然后关闭Al电弧靶电源,通入氮气、关闭氧气和氩气,调节气体流量,控制工作压强为2.6Pa,基底偏压继续保持不变,沉积20min结束。制备的抗高温氧化的铝铬硅氮与氧化铝多层复合涂层由CrAlTiZrY高熵合金粘结层、α-Cr2O3氧化物模板层、α-Al2O3氧化物核心层和AlCrSiN氮化物表层共四个子层组成,各个子层之间以及涂层与基底结合良好,在高温条件下具有良好的抗氧化性能。
实施例3
将清洁的金属陶瓷基底装入等离子体增强复合式离子镀膜系统的真空室中,待背底真空抽至0.03Pa时,打开炉壁的辅助加热装置对基底进行加热,同时打开转动电源使基底不停地转动,加热至基底温度达到380℃;然后向真空室中通入氩气,调节氩气流量保证压强为0.15Pa,然后对基底施加-200V的直流偏压和-400V的脉冲偏压,利用离化的Ar+对基底表面进行刻蚀,刻蚀90min;依次关闭基底偏压、调节氩气流量,保证工作压强为0.1Pa,开启蒸发镀主弧电源进行蒸发镀膜,坩埚上的主弧电流为220A,蒸发原料为Cr0.2Al0.2Ti0.2Zr0.2Y0.2块,蒸发沉积5min;关闭主弧电源,开启Cr电弧靶,靶电流设为100A,向真空室内通入氧气,调节氩气和氧气流量使工作压强为3.5Pa,对基底施加偏压-30V,沉积10min;开启Al电弧靶,靶电流设为120A,然后关闭Cr电弧靶电源,调节气体流量,控制压强为3.0Pa,基底偏压调节为-40V,镀膜70min;开启AlCrSi合金电弧靶,靶电流设为100A,然后关闭Al电弧靶电源,通入氮气、关闭氧气和氩气,调节气体流量,控制工作压强为2.8Pa,基底偏压调节为-50V,沉积30min结束。制备的抗高温氧化的铝铬硅氮与氧化铝多层复合涂层由CrAlTiZrY高熵合金粘结层、α-Cr2O3氧化物模板层、α-Al2O3氧化物核心层和AlCrSiN氮化物表层共四个子层组成,各个子层之间以及涂层与基底结合良好,在高温条件下具有良好的抗氧化性能。
实施例4
将清洁的硬质合金基底装入等离子体增强复合式离子镀膜系统的真空室中,待背底真空抽至0.03Pa时,打开炉壁的辅助加热装置对基底进行加热,同时打开转动电源使基底不停地转动,加热至基底温度达到380℃;然后向真空室中通入氩气,调节氩气流量保证压强为0.18Pa,然后对基底施加-200V的直流偏压和-400V的脉冲偏压,利用离化的Ar+对基底表面进行刻蚀,刻蚀45min;依次关闭基底偏压、调节氩气流量,保证工作压强为0.18Pa,开启蒸发镀主弧电源进行蒸发镀膜,坩埚上的主弧电流为200A,蒸发原料为Cr0.4Al0.15Ti0.15Zr0.15Y0.15块,蒸发沉积10min;关闭主弧电源,开启Cr电弧靶,靶电流设为70A,向真空室内通入氧气,调节氩气和氧气流量使工作压强为1.5Pa,对基底施加偏压-80V,沉积15min;开启Al电弧靶,靶电流设为120A,然后关闭Cr电弧靶电源,调节气体流量,控制压强为3.0Pa,基底偏压保持不变继续镀膜40min;开启AlCrSi合金电弧靶,靶电流设为80A,然后关闭Al电弧靶电源,通入氮气、关闭氧气和氩气,调节气体流量,控制工作压强为1.5Pa,基底偏压继续保持不变,沉积20min结束。制备的抗高温氧化的铝铬硅氮与氧化铝多层复合涂层由CrAlTiZrY高熵合金粘结层、α-Cr2O3氧化物模板层、α-Al2O3氧化物核心层和AlCrSiN氮化物表层共四个子层组成,各个子层之间以及涂层与基底结合良好,在高温条件下具有良好的抗氧化性能。
Claims (2)
1.一种抗高温氧化的铝铬硅氮与氧化铝多层复合涂层,其特征在于,涂层是由高熵合金粘结层、氧化物模板层、氧化物核心层、氮化物表层四个子层构成的整体,这四个子层的顺序是由内至外,涂层总厚度为1~3μm;所述高熵合金粘结层为CraAlbTicZrdYe,a+b+c+d+e=1,a、b、c、d、e的取值范围为0.15~0.4,厚度为50~200nm;所述氧化物模板层为α-Cr2O3,厚度为150~300nm;所述氧化物核心层为α-Al2O3,厚度为500~2000nm;所述氮化物表层为AlCrSiN,厚度为300~500nm。
2.一种权利要求1所述的抗高温氧化的铝铬硅氮与氧化铝多层复合涂层的制备方法,其特征在于,包括以下步骤:
A、将清洁的基底材料装入涂层设备真空室中,抽真空并加热,先将背底真空抽至0.03Pa及以下时,打开炉壁的辅助加热装置对基底进行加热,同时打开机架转动电源使基底在真空室内进行自转和公转运动,至基底温度达到380℃;
B、对基底表面进行离子刻蚀,向真空室中通入氩气,调节氩气流量保证压强为0.1~0.25Pa,然后对基底施加-100~-200V的直流偏压和-200~-400V的脉冲偏压,利用离化的Ar+对基底表面进行刻蚀,刻蚀30~90min;
C、利用电弧蒸镀工艺制备高熵合金粘结层,工作压强为0.1~0.2Pa,蒸镀坩埚上通过的电弧电流为180~220A,蒸镀坩埚内放置的材料为CraAlbTicZrdYe高熵合金, a+b+c+d+e=1,a、b、c、d、e的取值范围为0.15~0.4,蒸镀时间为5~10min;
D、利用阴极电弧镀膜工艺制备氧化物模板层,工作气体为Ar+O2,工作压强为1.5~3.5Pa,工作靶材为Cr电弧靶,靶电流为50~100A,基底施加的偏压为-30~-80V,沉积时间10~20min;
E、利用阴极电弧镀膜工艺制备氧化物核心层,工作气体为Ar+O2,工作压强为1.0~3.0Pa,工作靶材为Al电弧靶,靶电流为80~120A,基底施加的偏压为-30~-80V,沉积时间40~150min;
F、利用阴极电弧镀膜工艺制备氮化物表层,工作气体为N2,工作压强为1.5~3.5Pa,工作靶材为AlCrSi合金电弧靶,靶电流为80~120A,基底施加的偏压为-30~-80V,沉积时间20~35min。
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