CN114672763A - 一种提高金属陶瓷表面AlCrN涂层附着力的方法 - Google Patents

一种提高金属陶瓷表面AlCrN涂层附着力的方法 Download PDF

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CN114672763A
CN114672763A CN202210198727.XA CN202210198727A CN114672763A CN 114672763 A CN114672763 A CN 114672763A CN 202210198727 A CN202210198727 A CN 202210198727A CN 114672763 A CN114672763 A CN 114672763A
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周琼
杜俊龙
张而耕
黄彪
陈强
梁丹丹
姚松骏
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Shanghai Institute of Technology
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Abstract

本发明涉及一种提高金属陶瓷表面AlCrN涂层附着力的方法，该方法包括以下步骤：(1)将金属陶瓷试样表面进行酸洗，使试样表面的晶粒暴露，然后将酸洗好的金属陶瓷试样洗涤后烘干；(2)将试样放置于阴极电弧离子镀设备炉腔内自转，并将炉腔抽至本底真空1×10‑3Pa，在金属陶瓷试样表面沉积Cr打底层；(3)在Cr打底层上沉积Cr层；(4)在Cr层上依次沉积CrN层和AlCrN层，完成金属陶瓷表面AlCrN涂层的附着。与现有技术相比，本发明的梯度复合涂层与基体具有良好的结合强度。

Description

一种提高金属陶瓷表面AlCrN涂层附着力的方法
技术领域
本发明涉及涂层改性领域，具体涉及一种提高金属陶瓷表面AlCrN涂层附着力的方法。
背景技术
CrN涂层广泛应用于刀具、齿轮、活塞环、冲压工具的耐磨保护，并且效果可观。例如以做涂层为主的Balzers公司推出用于加工镍合金、铝合金的涂层铣刀，加工后的产品具有很高的加工表面质量。
物理气相沉积技术制备CrN的涂层虽然具有很多优良的特征，并已经广泛应用于各个领域，但其较低的硬度及抗磨粒磨损能力使得涂层在使用过程中容易过早失效而无法满足很多新产生的工业应用要求，为进一步提高涂层性能。在CrN薄膜的基础上采用多元技术添加Al、Cu、Nb、Ti等得到一种综合性更好的薄膜，其中最具代表性的当属添加Al元素而形成的AlCrN涂层。
与TiN加入Al后形成了性能优越的TiAlN相似，CrN加入Al而形成的三元AlCrN涂层具有韧性高、耐磨性好、抗氧化性强、高硬度和抗腐蚀性良好的特点，因此AlCrN涂层常引入到在刀具、模具和大功率汽车活塞环的表面改性处理中。AlCrN涂层的微观特性、韧性及稳定性都大幅提高。
但是，对于AlCrN涂层而言，存在金属陶瓷表面涂层难度大，表面涂层附着力小，涂层易脱落等问题。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种提高金属陶瓷表面AlCrN涂层附着力的方法。
本发明的目的可以通过以下技术方案来实现：
一种提高金属陶瓷表面AlCrN涂层附着力的方法，该方法包括以下步骤：
(1)将金属陶瓷试样表面进行酸洗，使试样表面的晶粒大面积暴露，然后将酸洗好的金属陶瓷试样洗涤后烘干；
(2)将试样放置于阴极电弧离子镀设备炉腔内自转，并将炉腔抽至本底真空1×10-3Pa，在金属陶瓷试样表面沉积Cr打底层；
(3)在Cr打底层上沉积Cr层；
(4)在Cr层上依次沉积CrN层和AlCrN层，完成金属陶瓷表面AlCrN涂层的附着。
进一步地，沉积Cr打底层和Cr层之前，采用低能氩离子进行刻蚀。
进一步地，所述酸洗的过程为：将金属陶瓷试样置于12-18wt％甲醇溶液、30-37wt％的浓盐酸和65-85wt％氯化铁混合均匀的溶液中，于密闭反应池内持续反应。
进一步地，所述甲醇溶液、浓盐酸和氯化铁的用量比为(70-90)ml:(15-25)ml:(0.15-0.25)g，所述反应的温度为90-100℃，时间为20-30min。
进一步地，沉积Cr打底层的具体步骤为：向炉腔内通入氩气，在-600～-700V偏压下刻蚀金属陶瓷基体10-15min；将Cr靶接入140-170A的电流，在-100～-150V偏压下在试样表面沉积100nm Cr打底层。
进一步地，沉积Cr打底层的具体步骤为：向炉腔内通入200sccm氩气，在-650V偏压下刻蚀金属陶瓷基体15min；将Cr靶接入160A的电流，在-100V偏压下在试样表面沉积100nmCr打底层。
进一步地，沉积Cr层的具体步骤为：向炉腔内通入氩气，在-180～-200V偏压下刻蚀5-10min，提高Cr打底层和基体之间结合的致密性；将Cr靶接入100-120A电流，-50～-110V偏压下沉积200nm Cr层。
进一步地，沉积Cr层的具体步骤为：向炉腔内通入200sccm氩气，在-200V偏压下刻蚀5min；将Cr靶接入120A电流，-100V偏压下沉积200nm Cr层。
Cr打底层分2次沉积，首次为靶材电流140-170A，从靶材溅射出来的粒子较大，易于基体形成机械咬合；第2次靶材电流为100-120A，从靶材溅射出来的粒子较小，有利于Cr打底层与CrN层致密过渡。
进一步地，沉积CrN层和AlCrN层的具体步骤为：关闭氩气，并向炉腔内通入130-150sccm的氮气，Cr靶接入100-140A电流，沉积CrN层；AlCr靶接入100-140A电流沉积AlCrN层。
进一步地，沉积CrN层和AlCrN层的具体步骤为：关闭氩气，并向炉腔内通入150sccm的氮气，Cr靶接入120A电流，沉积CrN层；AlCr靶接入120A电流沉积AlCrN层。
与现有技术相比，本发明具有以下优点：
(1)本发明Cr打底层分2次沉积，首次为靶材电流140-170A，从靶材溅射出来的粒子较大，易于基体形成机械咬合；第2次靶材电流为100-120A，从靶材溅射出来的粒子较小，有利于Cr打底层与CrN层致密过渡；
(2)本发明制备的Cr/CrN/AlCrN涂层的结合力最大，最适合提高基材表面结合力，梯度复合涂层与基体具有良好的结合强度。
附图说明
图1为实施例1制备的涂层示意图；
图2为实施例1制备的涂层SEM图。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
实施例1
一种提高金属陶瓷表面AlCrN涂层附着力的方法。先将金属陶瓷试样置于80mL,15％甲醇溶液、20mL,37％的浓盐酸和0.2g,70％氯化铁混合均匀的溶液中，于100℃恒温水浴箱中的密闭池内持续反应25min，溶解金属陶瓷表面的微量金属氧化物，使试样表面的晶粒大面积暴露。
将酸洗好的试样依次放入无水乙醇和去离子水中超声振荡10min之后取出用干燥氮气吹干；将试样放置于转炉架上并一同置于阴极电弧离子镀设备炉腔内自转。
将炉腔抽至本底真空1×10-3Pa，首先向炉腔内通入200sccm氩气，在-650V偏压下刻蚀金属陶瓷基体15min；Cr靶接入160A电流，-100V偏压下在试样表面沉积100nm Cr打底层。
然后再向炉腔内通入200sccm氩气，在-200V偏压下刻蚀基体5min，提高Cr打底层和基体之间结合的致密性；Cr靶接入120A电流，-100V偏压下继续沉积200nm Cr层。
最后关闭氩气，并向炉腔内通入150sccm的氮气，Cr靶接入120A电流，沉积CrN层；AlCr靶接入120A电流沉积AlCrN层，得到Cr/CrN/AlCrN梯度复合涂层。
表零Cr/CrN/AlCrN涂层的组成和力学性能
Figure BDA0003528287950000041
当涂层的H/E*值接近0.1时，涂层具有良好的韧性。用划痕测试仪分析涂层与基体的结合强度，用光学显微镜观察涂层的划痕形貌。将粘结力值定义为涂层呈片状且基材连续暴露时的临界点值。因此，得到的结合力为87N，说明涂层具有良好的韧性和结合力。
对比例1
与实施例1相比，区别在于省略了CrN涂层，即为Cr/AlCrN涂层
表一Cr/AlCrN涂层的组成和力学性能
Figure BDA0003528287950000042
对比例2
与实施例1相比，区别在于增加AlCrN涂层中Ti元素含量，形成TiAlCrN涂层。
表二TiAlCrN涂层的组成和力学性能
Figure BDA0003528287950000051
对比例3
与实施例1相比，区别在于Cr涂层未采用2次沉积，而是一次性沉积出300nm Cr层。
表三 一次性沉积的AlCrN涂层的组成和力学性能
Figure BDA0003528287950000052
通过对比三种不同涂层的硬度、弹性系数、结合力、H/E*值可知只有Cr/CrN/AlCrN涂层的结合力最大，最适合提高基材表面结合力。
以上所述，仅是本发明的较佳实施例而已，并非是对本发明作其它形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。

Claims (10)

1.一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，该方法包括以下步骤：
(1)将金属陶瓷试样表面进行酸洗，使试样表面的晶粒暴露，然后将酸洗好的金属陶瓷试样洗涤后烘干；
(2)将试样放置于阴极电弧离子镀设备炉腔内自转，并将炉腔抽至本底真空1×10-3Pa，在金属陶瓷试样表面沉积Cr打底层；
(3)在Cr打底层上沉积Cr层；
(4)在Cr层上依次沉积CrN层和AlCrN层，完成金属陶瓷表面AlCrN涂层的附着。
2.根据权利要求1所述的一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，沉积Cr打底层和Cr层之前，采用低能氩离子进行刻蚀。
3.根据权利要求1所述的一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，所述酸洗的过程为：将金属陶瓷试样置于12-18wt％甲醇溶液、30-37wt％的浓盐酸和65-85wt％氯化铁混合均匀的溶液中，于密闭反应池内持续反应。
4.根据权利要求1所述的一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，所述甲醇溶液、浓盐酸和氯化铁的用量比为(70-90)ml:(15-25)ml:(0.15-0.25)g，所述反应的温度为90-100℃，时间为20-30min。
5.根据权利要求1所述的一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，沉积Cr打底层的具体步骤为：向炉腔内通入氩气，在-600～-700V偏压下刻蚀金属陶瓷基体10-15min；将Cr靶接入140-170A的电流，在-100～-150V偏压下在试样表面沉积100nmCr打底层。
6.根据权利要求5所述的一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，沉积Cr打底层的具体步骤为：向炉腔内通入200sccm氩气，在-650V偏压下刻蚀金属陶瓷基体15min；将Cr靶接入160A的电流，在-100V偏压下在试样表面沉积100nm Cr打底层。
7.根据权利要求1所述的一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，沉积Cr层的具体步骤为：向炉腔内通入氩气，在-180～-200V偏压下刻蚀5-10min；将Cr靶接入100-120A电流，-50～-110V偏压下沉积200nm Cr层。
8.根据权利要求1所述的一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，沉积Cr层的具体步骤为：向炉腔内通入200sccm氩气，在-200V偏压下刻蚀5min；将Cr靶接入120A电流，-100V偏压下沉积200nm Cr层。
9.根据权利要求1所述的一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，沉积CrN层和AlCrN层的具体步骤为：关闭氩气，并向炉腔内通入130-150sccm的氮气，Cr靶接入100-140A电流，沉积CrN层；AlCr靶接入100-140A电流沉积AlCrN层。
10.根据权利要求9所述的一种提高金属陶瓷表面AlCrN涂层附着力的方法，其特征在于，沉积CrN层和AlCrN层的具体步骤为：关闭氩气，并向炉腔内通入150sccm的氮气，Cr靶接入120A电流，沉积CrN层；AlCr靶接入120A电流沉积AlCrN层。
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