CN113416955A - 一种钛合金紧固件阳极氧化与磁控溅射表面复合处理方法 - Google Patents

一种钛合金紧固件阳极氧化与磁控溅射表面复合处理方法 Download PDF

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CN113416955A
CN113416955A CN202110715590.6A CN202110715590A CN113416955A CN 113416955 A CN113416955 A CN 113416955A CN 202110715590 A CN202110715590 A CN 202110715590A CN 113416955 A CN113416955 A CN 113416955A
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titanium alloy
washing
magnetron sputtering
fastener
anodic oxidation
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庞坤
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Zhejiang Tianli Motor Parts Co ltd
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Abstract

本发明涉及钛合金紧固件的阳极氧化及磁控溅射技术的处理方法，具体涉及钛合金紧固件阳极氧化与磁控溅射表面复合处理方法，属于表面处理技术领域。其制备工艺可按如下步骤实现：(1)钛合金紧固件进行水洗、酸洗、再水洗前处理；(2)钛合金紧固件整体阳极氧化处理；(3)钛合金紧固件磁控溅射前用丙酮和酒精处理；(4)钛合金紧固件磁控溅射处理。本发明的钛合金紧固件处理工艺能够增强螺纹处的润滑和耐磨性能，增加整体的耐腐蚀性能，有效的解决钛合金紧固件不耐磨、电偶腐蚀以及螺纹处摩擦力大的问题。

Description

一种钛合金紧固件阳极氧化与磁控溅射表面复合处理方法
技术领域
本发明涉及钛合金紧固件的阳极氧化及磁控溅射技术的处理方法，具体涉及钛合金紧固件阳极氧化与磁控溅射表面复合处理方法，属于表面处理技术领域。
背景技术
钛及钛合金因具有质量轻、比强度高、耐蚀耐高温等优点，被广泛应用于航空航天、船舶汽车、体育用品等领域。一般情况下钛及钛合金表面可生成一层致密的氧化膜，起到防腐蚀的作用,但是在恶劣的环境中或者氧化膜破裂以及发生缝隙腐蚀的情况下，钛合金的耐腐蚀性能将大大降低。在海洋或潮湿环境中紧固件材料都存在不可预见的腐蚀性和由此带来的故障风险，当钛合金与结构钢、铝合金等异种金属接触时，由于电偶腐蚀常常会加速其他金属及其自身的腐蚀，造成紧固件及紧固孔周围产生破裂，不仅仅如此，钛合金紧固件加工非常困难，在螺纹紧固件的安装和锁紧时，螺纹轻易擦伤或卡死。因此，必须采取合适的防护措施以保证其环境耐久性满足在实际应用中尤其是国防工业中的安全性要求。
钛合金紧固件表面处理方法也有很多种，镀镉、阳极氧化、表面合金化、有机涂层等等，但是单独的某一种表面处理技术无法满足钛合金紧固件高耐蚀性与摩擦等性能，所以在本专利中提出了一种针对紧固件不同部位进行阳极氧化与磁控溅射表面复合处理方法。
采取一种针对不同部位进行不同表面处理工艺的复合处理方法，有效的提高钛合金紧固件的耐腐蚀性和耐磨性，降低螺纹处摩擦系数。
发明内容
采取一种针对不同部位进行不同表面处理工艺的复合处理方法，有效的提高钛合金紧固件的耐腐蚀性和耐磨性，降低螺纹处摩擦系数。
如图1所示为一种典型的带有头部的钛合金紧固件，其中螺柱分为带螺纹部分与不带螺纹部分。
如图2所示为整个钛合金紧固件表面复合处理方法的工艺流程图，其中，
1)钛合金紧固件前处理工艺：将加工完成的钛合金紧固件进行超声波水洗，时间为40～50min，去除表面油污和屑渣；进一步进行化学除油采用NaOH溶液进行冲洗，NaOH溶液浓度为1～5g/L，洗涤时间为10～20s；再采用温水对紧固件进行洗涤，水温为30～50℃，冲洗时间为10～20min；为了能够快速完全去除表面反应层，而表面不会产生其他元素的污染，然后将紧固件置入HF-HNO3系酸洗液进行酸洗0.5～2.5s，HF-HNO3系酸洗液成分为HF浓度在6～8％，而HNO3在35～50％，用去离子水清洗后放入NaOH溶液进行冲洗，NaOH溶液浓度为1～5g/L，洗涤时间为1～5s，清洗完成后用去离子水将试样清洗干净后25-45℃温度下烘干。
2)阳极氧化电解液配置，其中阳极氧化电解液为：磷酸100～400ml/L，双氧水0.5～3ml/L，乙酸5～15ml/L，磷酸二氢钠1～10g/L，醋酸镍0.5～1.5g/L。
3)钛合金紧固件整体阳极氧化处理工艺。将经过前处理工艺的紧固件进行清洗后，将紧固件全部浸入电解液中，阳极氧化电参数设定为：正电压10～90V，负电压5～40V，电流密度为频率为800～1000Hz，占空比为5～20％，电解液温度保持在15～30℃，阳极氧化时间为15～30min；
5)磁控溅射工艺材料准备：定制高纯度Ti靶(Ti含量不低于99.95％)。
6)磁控溅射前处理工艺。本发明中磁控溅射采用的是空心阴极辅助多弧离子镀复合沉积设备，钛合金紧固件在磁控溅射处理前首先需要采用丙酮和酒精进行超生冲洗5～20min，沉积前先Ti靶进行轰击10～15min，初始负偏压为800-1000V，腔室压力为(5～7)╳10-3Pa，温度为100-500℃。
7)磁控溅射处理工艺。电流调节在80-100A，将反应气体N2充入，流速为0.1～0.25L/min，沉积TiN膜层10～30min；继续抽真空，进行Ti膜层的沉积5-15min；充入Ar与O2混合气(比例为3:1～8:1之间)，沉积TiO210～20min，TiN/Ti/TiO2涂层如此往复2～3次后，将反应气体N2充入，流速为0.1～0.25L/min，沉积TiN膜层10～30min，停止。
与现有技术相比，本发明的优点在于：通过将钛合金紧固件分区域并按照一定的区域顺序进行微弧氧化，不同的位置获得不同的性能，更好的对钛合金紧固件进行防护，增强螺纹处的润滑和耐磨性能，增加整体的耐腐蚀性能，有效的解决钛合金紧固件不耐磨、电偶腐蚀以及螺纹处摩擦力大的问题。
附图说明
图1为钛合金紧固件示意图。图1中1为头部，2为螺柱无螺纹部分，3为螺柱带螺纹部分。
图2为钛合金表面处理技术流程图。
具体实施方式
以下结合附图实施例对本发明作进一步详细描述。
实施例1
1)将加工完成的钛合金紧固件进行超声波水洗，时间为40min，去除表面油污和屑渣；进一步进行化学除油采用NaOH溶液进行冲洗，NaOH溶液浓度为1g/L，洗涤时间为10s；再采用温水对紧固件进行洗涤，水温为30℃，冲洗时间为10min；为了能够快速完全去除表面反应层，而表面不会产生其他元素的污染，然后将紧固件置入HF-HNO3系酸洗液进行酸洗0.5s，HF-HNO3系酸洗液成分为HF浓度在6％，而HNO3在35％，用去离子水清洗后放入NaOH溶液进行冲洗，NaOH溶液浓度为1g/L，洗涤时间为1s，清洗完成后用去离子水将试样清洗干净后25℃温度下烘干。
2)阳极氧化电解液配置，其中阳极氧化电解液为：磷酸100ml/L，双氧水0.5ml/L，乙酸5ml/L，磷酸二氢钠1g/L，醋酸镍0.5g/L。
3)将经过前处理工艺的紧固件进行清洗后，将紧固件全部浸入电解液中，阳极氧化电参数设定为：正电压10V，负电压5V，电流密度为频率为800Hz，占空比为5％，电解液温度保持在15℃，阳极氧化时间为15min。
4)阳极氧化后处理工艺。将完成后的钛合金紧固件在阳极氧化电解液中浸泡2min，拿出后进行热处理，热处理工艺为：将氧化后的样品在200℃进行热处理，保温1h，然后随炉冷却至室温。
5)定制高纯度Ti靶(Ti含量不低于99.95％)。
6)钛合金紧固件在磁控溅射处理前首先需要采用丙酮和酒精进行超生冲洗5min，沉积前先Ti靶进行轰击10min，初始负偏压为800V，腔室压力为5╳10-3Pa，温度为100℃。
7)电流调节在80A，将反应气体N2充入，流速为0.1L/min，沉积TiN膜层10min；继续抽真空，进行Ti膜层的沉积5min；充入Ar与O2混合气(比例为3:1)，沉积TiO2膜层10min，TiN/Ti/TiO2涂层如此往复2次后，将反应气体N2充入，流速为0.1L/min，沉积TiN膜层10min，停止。
实施例2
将加工完成的钛合金紧固件进行超声波水洗，时间为45min，去除表面油污和屑渣；进一步进行化学除油采用NaOH溶液进行冲洗，NaOH溶液浓度为3g/L，洗涤时间为15s；再采用温水对紧固件进行洗涤，水温为40℃，冲洗时间为15min；为了能够快速完全去除表面反应层，而表面不会产生其他元素的污染，然后将紧固件置入HF-HNO3系酸洗液进行酸洗1.5s，HF-HNO3系酸洗液成分为HF浓度在7％，而HNO3在45％，用去离子水清洗后放入NaOH溶液进行冲洗，NaOH溶液浓度为3g/L，洗涤时间为3s，清洗完成后用去离子水将试样清洗干净后35℃温度下烘干。
2)阳极氧化电解液配置，其中阳极氧化电解液为：磷酸250ml/L，双氧水2ml/L，乙酸10ml/L，磷酸二氢钠5g/L，醋酸镍1g/L。
3)将经过前处理工艺的紧固件进行清洗后，将紧固件全部浸入电解液中，阳极氧化电参数设定为：正电压50V，负电30V，电流密度为频率为900Hz，占空比为15％，电解液温度保持在25℃，阳极氧化时间为20min。
4)将完成后的钛合金紧固件在阳极氧化电解液中浸泡4min，拿出后进行热处理，热处理工艺为：将氧化后的样品在300℃进行热处理，保温2h，然后随炉冷却至室温。
5)定制高纯度Ti靶(Ti含量不低于99.95％)。
6)钛合金紧固件在磁控溅射处理前首先需要采用丙酮和酒精进行超生冲洗10min，沉积前先Ti靶进行轰击12min，初始负偏压为900V，腔室压力为6╳10-3Pa，温度为300℃。
7)电流调节在90A，将反应气体N2充入，流速为0.2L/min，沉积TiN膜层20min；继续抽真空，进行Ti膜层的沉积10min；充入Ar与O2混合气(比例为5:1)，沉积TiO2膜层15min，TiN/Ti/TiO2涂层如此往复2次后，将反应气体N2充入，流速为0.2L/min，沉积TiN膜层20min，停止。
实施例3
1)将加工完成的钛合金紧固件进行超声波水洗，时间为50min，去除表面油污和屑渣；进一步进行化学除油采用NaOH溶液进行冲洗，NaOH溶液浓度为5g/L，洗涤时间为20s；再采用温水对紧固件进行洗涤，水温为50℃，冲洗时间为20min；为了能够快速完全去除表面反应层，而表面不会产生其他元素的污染，然后将紧固件置入HF-HNO3系酸洗液进行酸洗2.5s，HF-HNO3系酸洗液成分为HF浓度在8％，而HNO3在50％，用去离子水清洗后放入NaOH溶液进行冲洗，NaOH溶液浓度为5g/L，洗涤时间为5s，清洗完成后用去离子水将试样清洗干净后45℃温度下烘干。
2)阳极氧化电解液配置，其中阳极氧化电解液为：磷酸400ml/L，双氧水3ml/L，乙酸15ml/L，磷酸二氢钠10g/L，醋酸镍1.5g/L。
3)将经过前处理工艺的紧固件进行清洗后，将紧固件全部浸入电解液中，阳极氧化电参数设定为：正电压90V，负电压40V，电流密度为频率为1000Hz，占空比为20％，电解液温度保持在30℃，阳极氧化时间为30min。
4)将完成后的钛合金紧固件在阳极氧化电解液中浸泡5min，拿出后进行热处理，热处理工艺为：将氧化后的样品在350℃进行热处理，保温3h，然后随炉冷却至室温。
5)定制高纯度Ti靶(Ti含量不低于99.95％)。
6)钛合金紧固件在磁控溅射处理前首先需要采用丙酮和酒精进行超生冲洗20min，沉积前先Ti靶进行轰击15min，初始负偏压为1000V，腔室压力为7╳10-3Pa，温度为500℃。
7)磁控溅射处理工艺。电流调节在100A，将反应气体N2充入，流速为0.25L/min，沉积TiN膜层30min；继续抽真空，进行Ti膜层的沉积15min；充入Ar与O2混合气(比例为8:1之间)，沉积TiO2膜层20min，TiN/Ti/TiO2涂层如此往复3次后，将反应气体N2充入，流速为0.25L/min，沉积TiN膜层30min，停止。

Claims (7)

1.一种针对钛合金紧固件不同部位进行不同表面处理工艺的复合处理方法，有效的提高其耐腐蚀性和耐磨性，降低螺纹处摩擦系数。其特征在于：对钛合金紧固件进行水洗、酸洗、再水洗前处理，然后进行整体阳极氧化处理，接着对钛合金紧固用丙酮和酒精处理，最后对其进行磁控溅射处理。其制备工艺步骤为：1)钛合金紧固件前处理；2)阳极氧化电解液配置；3)钛合金紧固件整体阳极氧化处理；4)磁控溅射工艺材料准备；5)磁控溅射前处理；6)磁控溅射处理。
2.根据权利要求1所述的钛合金紧固件前处理工艺，其特征在于：将加工完成的钛合金紧固件进行超声波水洗，时间为40～50min，去除表面油污和屑渣；进一步进行化学除油采用NaOH溶液进行冲洗，NaOH溶液浓度为1～5g/L，洗涤时间为10～20s；再采用温水对紧固件进行洗涤，水温为30～50℃，冲洗时间为10～20min；为了能够快速完全去除表面反应层，而表面不会产生其他元素的污染，然后将紧固件置入HF-HNO3系酸洗液进行酸洗0.5～2.5s，HF-HNO3系酸洗液成分为HF浓度在6～8％，而HNO3在35～50％，用去离子水清洗后放入NaOH溶液进行冲洗，NaOH溶液浓度为1～5g/L，洗涤时间为1～5s，清洗完成后用去离子水将试样清洗干净后25-45℃温度下烘干。
3.根据权利要求1所述的阳极氧化电解液配置工艺，其特征在于：其中阳极氧化电解液为磷酸100～400ml/L，双氧水0.5～3ml/L，乙酸5～15ml/L，磷酸二氢钠1～10g/L，醋酸镍0.5～1.5g/L。
4.根据权利要求1所述的钛合金紧固件整体阳极氧化处理工艺，其特征在于：将经过前处理工艺的紧固件进行清洗后，将紧固件全部浸入电解液中，阳极氧化电参数设定为：正电压10～90V，负电压5～40V，电流密度为频率为800～1000Hz，占空比为5～20％，电解液温度保持在15～30℃，阳极氧化时间为15～30min。
5.根据权利要求1所述的磁控溅射工艺材料准备，其特征在于：定制高纯度Ti靶(Ti含量不低于99.95％)。
6.根据权利要求1所述的磁控溅射前处理工艺，其特征在于：磁控溅射采用的是空心阴极辅助多弧离子镀复合沉积设备，钛合金紧固件在磁控溅射处理前首先需要采用丙酮和酒精进行超生冲洗5～20min，沉积前先Ti靶进行轰击10～15min，初始负偏压为800-1000V，腔室压力为(5～7)╳10-3Pa，温度为100-500℃。
7.根据权利要求1所述的磁控溅射处理工艺，其特征在于：电流调节在80-100A，将反应气体N2充入，流速为0.1～0.25L/min，沉积TiN膜层10～30min；继续抽真空，进行Ti膜层的沉积5-15min；充入Ar与O2混合气(比例为3:1～8:1之间)，沉积TiO210～20min，TiN/Ti/TiO2涂层如此往复2～3次后，将反应气体N2充入，流速为0.1～0.25L/min，沉积TiN膜层10～30min，停止。
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