CN111471969A - 一种用于在高温下抗氧化的Cr/CrN/CrAlN梯度涂层及制备方法 - Google Patents

一种用于在高温下抗氧化的Cr/CrN/CrAlN梯度涂层及制备方法 Download PDF

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CN111471969A
CN111471969A CN202010194388.9A CN202010194388A CN111471969A CN 111471969 A CN111471969 A CN 111471969A CN 202010194388 A CN202010194388 A CN 202010194388A CN 111471969 A CN111471969 A CN 111471969A
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杨文晟
郭汉杰
陈胜吉
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University of Science and Technology Beijing USTB
Ming Chi University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3464—Sputtering using more than one target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon

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Abstract

本发明公开了一种用于在高温下抗氧化的Cr/CrN/CrAlN梯度涂层及制备方法，属于表面工程技术。在9‑12％Cr耐热钢表面沉积Cr/CrN/CrAlN涂层，采用Cr靶、Al靶直流反应共溅的方式获得Cr/CrN/CrAlN涂层，基片温度为150‑200℃，Ar和N2采用微电脑控制，其流量分别为5‑7SCCM(标准立方米每分钟)和6‑8SCCM，工作气压为5‑10mtorr。为提高涂层和基体的结合力，选用Cr底层，并施加100‑150V的基体负偏压。所获得的涂层底层为Cr层，中间层为CrN层，外层为CrAlN层。涂层在600‑800℃空气中氧化后的主要产物为Al2O3。高温氧化实验表明Cr/CrN/CrAlN涂层具有很好的高温抗氧化能力。应用本发明可显著提高耐热钢的高温抗氧化能力。

Description

一种用于在高温下抗氧化的Cr/CrN/CrAlN梯度涂层及制备 方法
技术领域
本发明属于表面工程技术，具体是一种用于耐热钢高温抗氧化的Cr/CrN/CrAlN防护涂层及制备方法。
背景技术
9-12％Cr马氏体耐热钢因其高导热率，低热膨胀系数和低热疲劳敏感性而被广泛用于超超临界发电厂。文献1：材料工程与性能杂志(Journal of Materials Engineeringand Performance,15,3,(2006))中Viswanathan博士调查研究指出该种类耐热钢的使用温度上限为620℃。其中的一个限制性环节是更高温度下耐热钢的抗氧化能力差。目前，为了在高的蒸汽参数(630℃)下使用，主要做法是提高耐热钢中的Cr含量，以便高温下生成大量的Cr2O3氧化产物层，阻碍氧气扩散防止钢材的进一步氧化。但是，随着Cr含量的增加，钢材中铁素体含量也会增加，导致耐热钢蠕变强度降低。本发明的思想来源于文献2：美国专利(Gerhard B.Manufacture of refractory oxide coatings:U.S.Patent 3,050,409.1962-8-21)Gerhard发明了通过涂层防止金属材料氧化的方法。考虑到耐热钢涂层对硬度的要求及耐热钢成分的高Cr含量，CrN硬质涂层是第一选择。但是文献3：表面和涂层技术(Surface and Coatings Technology，202，14，(2008))Mishra等人研究发现，CrN涂层在600℃时会发生热解生成Cr2N和N2，无法在更高温度下使用。文献3：材料学报(ActaMaterialia,60,16,(2012))方峰博士等人研究发现对CrN硬质涂层进行Al掺杂可以显著提高涂层的高温抗氧化能力。为了进一步提高涂层与9-12％Cr耐热钢的结合能力，需要设计Cr底层及CrN中间层。而对于Cr/CrN/CrAlN涂层在耐热钢上的应用目前还没有报道。
发明内容
本发明的目的在于提供一种用于在高温下抗氧化的Cr/CrN/CrAlN梯度涂层及制备方法，该涂层由Cr底层、CrN中间层、CrAlN工作层三部分构成，具有与耐热钢钢基材良好的结合能力和高温抗氧化性。
本发明采用的技术方案是：
一种用于在高温下抗氧化的Cr/CrN/CrAlN梯度涂层；其特征在于：所述涂层底层为Cr，中间层为CrN，外层为CrAlN。
进一步地，Cr底层厚度范围为0.2-1μm，CrN中间层厚度为0.2-1μm，CrAlN工作层厚度为0.2-1μm。
如上所述一种用于在高温下抗氧化的Cr/CrN/CrAlN梯度涂层的制备方法，其特征在于：采用Al靶、Cr靶在氮气和氩气混合气氛中双靶共溅的方式制备Cr/CrN/CrAlN梯度涂层，工作压力为5-10mtorr，基体的温度为150-200℃，施加基体负偏压以提高涂层和基体的粘附性能。
进一步地，其特征在于：所述Cr靶重量纯度≥99.9％，功率范围为40-100W；Al靶重量纯度≥99.9％，功率范围为0-100W。
进一步地，所施加的基体负偏压范围为100-150V。
本发明的优点是：
1、涂层具有优良的高温抗氧化性。Cr/CrN/CrAlN涂层在高于600℃的空气中氧化时表面生成Al2O3保护膜，可以有效地防护基材氧化。
2、而且，在提高耐热钢高温抗氧化性能的同时还可以改善耐热钢的表面力学性能，非常适合在既需要提高高温抗氧化性又对表面力学性能有一定要求的工业环境的材料上应用。通常情况下，这是其他种类高温防护涂层难以达到的。
3、工艺简单，成分容易调整。在调节涂层中的Al含量时不需要熔炼不同成分的合金靶，只需要调节两个溅射靶的功率即可。
4、本发明在9-12％Cr耐热钢表面获得的Cr/CrN/CrAlN涂层再宽温度范围内抗高温氧化，宽温度范围为600-800℃。
附图说明：
图1为Cr/CrN/CrAlN涂层的X射线衍射谱。
图2为涂层的刮痕形貌，其中图(a)为CrN/CrAlN涂层的刮痕形貌，图(b)为Cr/CrN/CrAlN涂层的刮痕形貌
图3为Cr/CrN/CrAlN涂层在800℃的恒温氧化动力学曲线，为说明其防护效果的同时给出了9-12％Cr耐热钢的氧化动力学曲线。
具体实施方式
下面结合附图及具体实施例对本发明作进一步的详细说明。
实施例1
将表面经过喷砂预处理，尺寸为7mm×7mm×1mm的9-12％Cr耐热钢的基片放进真空镀膜设备，抽真空至小于4.8×10-6pa，后对基片加热至200℃。打开进气阀充入7SCCM的氩气，调节基片偏压为-700V以便去除基片表面氧化层。随后调节基片偏压为-100V，打开连接在Cr靶上的直流电源，在功率为100W下溅射Cr底层，时间为20min，Cr底层厚度为200nm。然后通入7SCCM的N2，保持Cr靶功率为100W溅射CrN中间层，时间为40min，CrN中间层厚度为200nm。最后打开连接在Al靶上的直流电源，调节Cr靶功率为40W，Al靶功率为100W，共溅Cr-Al-N层，Cr-Al-N层厚度为250nm。经X射线分析为涂层具有CrN结构，如图1所示。
实施例2
和实施例1不同的是CrN/CrAlN涂层不需要溅射Cr底层，CrN层溅射时间为80min。由图2(a)CrN/CrAlN涂层的刮痕形貌与(b)Cr/CrN/CrAlN涂层的刮痕形貌可知，增加Cr底层后Cr/CrN/CrAlN涂层的Lc1(临界破裂载荷)远大于CrN/CrAlN涂层的Lc1，即增加Cr底层后可以显著提高涂层与钢的结合能力。
实施例3
对9-12％Cr耐热钢和Cr/CrN/CrAlN涂层进行800℃恒温氧化实验，如图3所示。800℃下Cr/CrN/CrAlN涂层的抗氧化能力明显强于9-12％Cr耐热钢。
由实施例1、实施例2、实施例3可见，Cr/CrN/CrAlN涂层不但具有与9-12％Cr耐热钢较好的结合能力，并且具有良好的抗高温氧化能力。

Claims (5)

1.一种用于在高温下抗氧化的Cr/CrN/CrAlN梯度涂层；其特征在于：所述涂层底层为Cr，中间层为CrN，外层为CrAlN。
2.根据权利要求1所述的Cr/CrN/CrAlN梯度涂层，其特征在于：Cr底层厚度范围为0.2-1μm，CrN中间层厚度为0.2-1μm，CrAlN工作层厚度为0.2-1μm。
3.根据权利要求1所述的用于在高温下抗氧化的Cr/CrN/CrAlN梯度涂层的制备方法，其特征在于：采用Al靶、Cr靶在氮气和氩气混合气氛中双靶共溅的方式制备Cr/CrN/CrAlN梯度涂层，工作压力为5-10mtorr，基体的温度为150-200℃，施加基体负偏压以提高涂层和基体的粘附性能。
4.根据权利要求3所述的Cr/CrN/CrAlN梯度涂层的制备方法，其特征在于：所述Cr靶重量纯度≥99.9％，功率范围为40-100W；Al靶重量纯度≥99.9％，功率范围为0-100W。
5.根据权利要求3所述的Cr/CrN/CrAlN梯度涂层的制备方法，其特征在于：所施加的基体负偏压范围为100-150V。
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