CN108531875A - 一种氮化铬基硬质涂层的过渡层的制备方法 - Google Patents

一种氮化铬基硬质涂层的过渡层的制备方法 Download PDF

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CN108531875A
CN108531875A CN201810196898.2A CN201810196898A CN108531875A CN 108531875 A CN108531875 A CN 108531875A CN 201810196898 A CN201810196898 A CN 201810196898A CN 108531875 A CN108531875 A CN 108531875A
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sputtering
gas
transition zone
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chromium nitride
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杨坤
李镇江
王博
王雪艳
刘云虎
孙茂珠
张吉东
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Shihezi University
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/024Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025Metallic sublayers
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641Nitrides
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

本发明公开了一种氮化铬基硬质涂层的过渡层的制备方法,在将真空系统抽到高真空以后,充入惰性气体Ar气作为放电气体时,其压力范围一般处于10‑1~10Pa之间。在正负电极间外加电压的作用下,电极间的气体原子将被大量电离,形成辉光放电,电子沿着电场方向加速,其轨迹为绕磁场方向螺旋前进的复杂曲线。由于在两极之间等离子体中不断振荡运动的电子可从高频电场中获得足够的能量,并能有效地与气体分子碰撞使后者发生电离,起到了维持气体放电的作用。同时射频电场起作用的同时,Ti靶会自动地处于一个负电位下,从而导致气体离子对其产生自发的轰击和溅射,从而将Ti离子沉积在基底上形成致密的过渡涂层。

Description

一种氮化铬基硬质涂层的过渡层的制备方法
技术领域
本发明属于涂层制备技术领域,涉及一种氮化铬基硬质涂层的过渡层的制备方法,具体地说,涉及一种应用于钢制基底的氮化铬(CrN)基硬质涂层的过渡层的制备方法。
背景技术
氮化铬(CrN)基硬质膜涂层具有较高的硬度,良好的耐磨性、高温稳定性和化学惰性,被广泛应用于机械加工保护涂层中。此类硬质膜尝尝因为与基体的脱离和剥裂从而影响应用性能,因此采用合适的过渡层材料和制备方法,加强涂层与基体的结合强度,是提高氮化铬(CrN)基硬质膜涂层应用性能和使用寿命的关键。过渡金属钛,重量轻、强度高,有良好的抗腐蚀能力(包括海水、王水及氯气)及稳定的化学性质,具有耐高温、耐低温、抗强酸、抗强碱,以及高强度、低密度等特性。采用Ti作为氮化铬(CrN)基硬质涂层的过渡层,在钢制基底上Ti与Fe相互扩散生长,形成中间界面产物FeTi,FeTi与钢制基底及Ti过渡层之间结合良好,能有效提高氮化铬(CrN)基硬质涂层与基底的结合强度,阻止涂层表面裂纹的生成和扩散。
发明内容
本发明的目的在于克服上述技术存在的缺陷,提供一种氮化铬基硬质涂层的过渡层的制备方法,该方法制备出的涂层能提高氮化铬(CrN)基硬质膜涂层应用性能和使用寿命。
其具体技术方案为:
一种氮化铬基硬质涂层的过渡层的制备方法,包括以下步骤:
钢制基底用甲苯、丙酮和无水酒精各超声清洗10min并烘干后装入真空室。将磁控溅射真空室背底真空抽至9.0×10-4Pa后,通入高纯Ar气,Ar流量为20-60sccm,总气压保持在2.0-3.0Pa。开启Ti靶射频溅射电源,逐渐调大溅射电流,使Ti靶起辉,将Ti靶的溅射功率调至为120-200W,溅射电压为1100-1500V,溅射电流为0.11-0.13A,先进行预溅射,不打开靶材挡板对Ti靶表面进行轰击清洗10min,之后打开Ti靶挡板进行过渡层沉积,沉积时间60-120min。
与现有技术相比,本发明的有益效果:
本发明采用JGP450复合型高真空多靶磁控溅射设备,利用射频反应磁控溅射法制备硬质涂层的过渡层,可以显著降低溅射过程中的气体压力,提高溅射的效率和沉积的速率,降低薄膜污染的可能性;同时提高了溅射到衬底表面原子的能量,改善涂层和基体的结合力,并有效预防靶材中毒。
具体实施方式
下面结合具体实施例对本发明的技术方案作进一步详细地说明。
本发明在将真空系统抽到高真空以后,充入惰性气体Ar气作为放电气体时,其压力范围一般处于10-1~10Pa之间。在正负电极间外加电压的作用下,电极间的气体原子将被大量电离,形成辉光放电,电子沿着电场方向加速,其轨迹为绕磁场方向螺旋前进的复杂曲线。由于在两极之间等离子体中不断振荡运动的电子可从高频电场中获得足够的能量,并能有效地与气体分子碰撞使后者发生电离,起到了维持气体放电的作用。同时射频电场起作用的同时,Ti靶会自动地处于一个负电位下,从而导致气体离子对其产生自发的轰击和溅射,从而将Ti离子沉积在基底上形成致密的过渡涂层。
实施例1
钢制基底用甲苯、丙酮和无水酒精各超声清洗10min并烘干后装入真空室。将磁控溅射真空室背底真空抽至9.0×10-4Pa后,通入高纯Ar气,Ar流量为20sccm,总气压保持在2.0Pa。开启Ti靶射频溅射电源,逐渐调大溅射电流,使Ti靶起辉,将Ti靶的溅射功率调至为120W,溅射电压为1100V,溅射电流为0.11A,先进行预溅射,不打开靶材挡板对Ti靶表面进行轰击清洗10min,之后打开Ti靶挡板进行过渡层沉积,沉积时间60min。
实施例2
钢制基底用甲苯、丙酮和无水酒精各超声清洗10min并烘干后装入真空室。将磁控溅射真空室背底真空抽至9.0×10-4Pa后,通入高纯Ar气,Ar流量为40sccm,总气压保持在2.0-Pa。开启Ti靶射频溅射电源,逐渐调大溅射电流,使Ti靶起辉,将Ti靶的溅射功率调至为160W,溅射电压为1400V,溅射电流为0.12A,先进行预溅射,不打开靶材挡板对Ti靶表面进行轰击清洗10min,之后打开Ti靶挡板进行过渡层沉积,沉积时间90min。
实施例3
钢制基底用甲苯、丙酮和无水酒精各超声清洗10min并烘干后装入真空室。将磁控溅射真空室背底真空抽至9.0×10-4Pa后,通入高纯Ar气,Ar流量为60sccm,总气压保持在3.0Pa。开启Ti靶射频溅射电源,逐渐调大溅射电流,使Ti靶起辉,将Ti靶的溅射功率调至为200W,溅射电压为1500V,溅射电流为0.13A,先进行预溅射,不打开靶材挡板对Ti靶表面进行轰击清洗10min,之后打开Ti靶挡板进行过渡层沉积,沉积时间120min。
以上所述,仅为本发明较佳的具体实施方式,本发明的保护范围不限于此,任何熟悉本技术领域的技术人员在本发明披露的技术范围内,可显而易见地得到的技术方案的简单变化或等效替换均落入本发明的保护范围内。

Claims (1)

1.一种氮化铬基硬质涂层的过渡层的制备方法,其特征在于,包括以下步骤:
钢制基底用甲苯、丙酮和无水酒精各超声清洗10min并烘干后装入真空室;将磁控溅射真空室背底真空抽至9.0×10-4Pa后,通入高纯Ar气,Ar流量为20-60sccm,总气压保持在2.0-3.0Pa;开启Ti靶射频溅射电源,逐渐调大溅射电流,使Ti靶起辉,将Ti靶的溅射功率调至为120-200W,溅射电压为1100-1500V,溅射电流为0.11-0.13A,先进行预溅射,不打开靶材挡板对Ti靶表面进行轰击清洗10min,之后打开Ti靶挡板进行过渡层沉积,沉积时间60-120min。
CN201810196898.2A 2018-03-10 2018-03-10 一种氮化铬基硬质涂层的过渡层的制备方法 Pending CN108531875A (zh)

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