CN106435495B - 不锈钢薄板表面TiN-Ti复合覆层的制备方法 - Google Patents

不锈钢薄板表面TiN-Ti复合覆层的制备方法 Download PDF

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CN106435495B
CN106435495B CN201610773760.5A CN201610773760A CN106435495B CN 106435495 B CN106435495 B CN 106435495B CN 201610773760 A CN201610773760 A CN 201610773760A CN 106435495 B CN106435495 B CN 106435495B
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李铮
李鲁
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JIANGSU HUALI METAL MATERIAL Co Ltd
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Abstract

本发明涉及一种不锈钢薄板表面TiN‑Ti复合覆层的制备方法，包括以下步骤：包括以下步骤：（1）不锈钢薄板的清洗；（2）制备Ti覆层；（3）制备TiN‑Ti复合覆层；采用磁控溅射技术，覆层与不锈钢薄板之间的结合强度高，且覆层机械强度高，采用离子扩散制得TiN‑Ti复合覆层，使得TiN与Ti之间的界面扩散层连续，从而获得富TiN表层保持了TiN高硬、耐磨等优良性能；而在次表层形成的钛扩散过渡层增强了基体对硬质TiN表层的综合承载能力，使不锈钢薄板的耐磨性得到了明显的提高。

Description

不锈钢薄板表面TiN-Ti复合覆层的制备方法
技术领域
本发明涉及一种金属材料表面改性技术领域，特别涉及一种不锈钢薄板表面TiN-Ti复合覆层的制备方法。
背景技术
目前，不锈钢薄板是一种价格不高的材料，已经广泛应用于各行各业，但是客户对它的表面质量要求非常高。不锈薄板在生产过程中不可避免会出现各种缺陷，如划伤、麻点、沙孔、暗线、折痕、污染等，从而其表面质量，象划伤、折痕等这些缺陷是高级材不允许出现的，而麻点、沙孔这种缺陷在勺、匙、叉、制作时也是决不允许的，因为抛光时很难抛掉它。需要根据表面各种缺陷出现的程度和频率，来确定其表质量等级，从而来确定产品等级。
因此，现在有必要研发出一种不锈钢薄板表面TiN-Ti复合覆层的制备方法，来增加不锈钢表面的耐磨性。
发明内容
本发明要解决的技术问题是，针对现有的不足，提供一种沉积速率快、质量可控、工作效率高的不锈钢薄板表面TiN-Ti复合覆层的制备方法。
为了解决上述技术问题，本发明采用的技术方案是，该不锈钢薄板表面TiN-Ti复合覆层的制备方法，包括以下步骤：
（1）不锈钢薄板的清洗：为了去除油渍，先用浓度为3.5~4.5 %碳酸钠碱液清洗不锈钢薄板10~15min，清洗时温度为65~75℃；然后为了去除氧化皮在浓度为3.5~4.5%稀硫酸中清洗10~15min；再将不锈钢薄板先后放入丙酮溶液、乙醇溶液和去离子水中超声25~35min，以提高基板表面活性，吹干待用；
（2）制备Ti覆层：将步骤（1）中清洗后的不锈钢薄板置于磁控溅射设备的基片台上作为阳极，将金属钛靶放入磁控溅射设备的靶材座上作为阴极，且调节靶材座与基片座的距离，使两者之间的距离保持在20mm；启动机械泵，打开旁抽阀Ⅱ，对真空腔室抽真空；当真空度达到1~8Pa时，关闭旁抽阀Ⅱ，打开旁抽阀Ⅰ，并启动分子泵，打开闸板阀，采用分子泵对真空腔室进一步抽真空；当分子泵加速后稳定运行直至真空度达到1~5×10-3Pa；打开氩气阀，通入氩气，对基板进行离子束清洗，清洗时间为3~5 min；待磁控溅射设备的真空度达到4~8Pa时，调节磁控溅射沉积条件：预热不锈钢薄板至300~500℃；放电电压300V~400V、电流10~20A、沉积速率为1.0~2.0μm/min；沉积时间20~60min，制得Ti覆层的不锈钢薄板；依次关闭电流、放电电压和氩气阀，解除真空，关闭分子泵，开启进气阀，通入空气，并待不锈钢薄板冷却至室温后，取出Ti覆层的不锈钢薄板；
（3）制备TiN-Ti复合覆层：将步骤（2）制得Ti覆层的不锈钢薄板放入离子氮化炉中，选择NH3为渗氮气体，气压为450~500Pa，渗氮温度为800~900℃，阴电极电压为600~700V，渗氮8~12h后，再维持正常辉光放电冷却1h，断开电源，关闭气体，随炉冷却至室温，即得TiN-Ti复合覆层的不锈钢薄板。
进一步改进在于，在所述步骤（3）中不锈钢薄板表面沉积的Ti覆层的厚度为20~80μm。
与现有技术相比，本发明的有益效果是：采用磁控溅射技术，覆层与不锈钢薄板之间的结合强度高，且覆层机械强度高，采用离子扩散制得TiN-Ti复合覆层，使得TiN与Ti之间的界面扩散层连续，从而获得富TiN表层保持了TiN高硬、耐磨等优良性能；而在次表层形成的钛扩散过渡层增强了基体对硬质TiN表层的综合承载能力，使不锈钢薄板的耐磨性得到了明显的提高，此该制备方法工艺简单、质量可控、工作效率高，制备过程在全真空条件下，无污染环境、危害人体安全等问题，因此极其适合工业化应用；制备工艺也能适合工业化连续生产，产品成品率高，质量稳定，而且制造成本低廉。
具体实施方式
实施例1：不锈钢薄板表面TiN-Ti复合覆层的制备方法，包括如下步骤：
（1）不锈钢薄板的清洗：为了去除油渍，先用浓度为3.5 %碳酸钠碱液清洗不锈钢薄板15min，清洗时温度为75℃；然后为了去除氧化皮在浓度为3.5%稀硫酸中清洗15min；再将不锈钢薄板先后放入丙酮溶液、乙醇溶液和去离子水中超声25min，以提高基板表面活性，吹干待用；
（2）制备Ti覆层：将步骤（1）中清洗后的不锈钢薄板置于磁控溅射设备的基片台上作为阳极，将金属钛靶放入磁控溅射设备的靶材座上作为阴极，且调节靶材座与基片座的距离，使两者之间的距离保持在20mm；启动机械泵，打开旁抽阀Ⅱ，对真空腔室抽真空；当真空度达到6Pa时，关闭旁抽阀Ⅱ，打开旁抽阀Ⅰ，并启动分子泵，打开闸板阀，采用分子泵对真空腔室进一步抽真空；当分子泵加速后稳定运行直至真空度达到5×10-3Pa；打开氩气阀，通入氩气，对基板进行离子束清洗，清洗时间为5 min；待磁控溅射设备的真空度达到4Pa时，调节磁控溅射沉积条件：预热不锈钢薄板至300℃；放电电压300V、电流15A、沉积速率为1.2μm/min；沉积时间40min，制得Ti覆层的不锈钢薄板；Ti覆层的厚度为48μm；依次关闭电流、放电电压和氩气阀，解除真空，关闭分子泵，开启进气阀，通入空气，并待不锈钢薄板冷却至室温后，取出Ti覆层的不锈钢薄板；
（3）制备TiN-Ti复合覆层：将步骤（2）制得Ti覆层的不锈钢薄板放入离子氮化炉中，选择NH3为渗氮气体，气压为500Pa，渗氮温度为800℃，阴电极电压为700V，渗氮9h后，再维持正常辉光放电冷却1h，断开电源，关闭气体，随炉冷却至室温，即得TiN-Ti复合覆层的不锈钢薄板。
实施例2：不锈钢薄板表面TiN-Ti复合覆层的制备方法，包括如下步骤：
（1）不锈钢薄板的清洗：为了去除油渍，先用浓度为4.5 %碳酸钠碱液清洗不锈钢薄板10min，清洗时温度为65℃；然后为了去除氧化皮在浓度为4.5%稀硫酸中清洗10min；再将不锈钢薄板先后放入丙酮溶液、乙醇溶液和去离子水中超声35min，以提高基板表面活性，吹干待用；
（2）制备Ti覆层：将步骤（1）中清洗后的不锈钢薄板置于磁控溅射设备的基片台上作为阳极，将金属钛靶放入磁控溅射设备的靶材座上作为阴极，且调节靶材座与基片座的距离，使两者之间的距离保持在20mm；启动机械泵，打开旁抽阀Ⅱ，对真空腔室抽真空；当真空度达到5Pa时，关闭旁抽阀Ⅱ，打开旁抽阀Ⅰ，并启动分子泵，打开闸板阀，采用分子泵对真空腔室进一步抽真空；当分子泵加速后稳定运行直至真空度达到5×10-3Pa；打开氩气阀，通入氩气，对基板进行离子束清洗，清洗时间为5 min；待磁控溅射设备的真空度达到6Pa时，调节磁控溅射沉积条件：预热不锈钢薄板至500℃；放电电压400V、电流20A、沉积速率为2.0μm/min；沉积时间30min，制得Ti覆层的不锈钢薄板；Ti覆层的厚度为60μm；依次关闭电流、放电电压和氩气阀，解除真空，关闭分子泵，开启进气阀，通入空气，并待不锈钢薄板冷却至室温后，取出Ti覆层的不锈钢薄板；
（3）制备TiN-Ti复合覆层：将步骤（2）制得Ti覆层的不锈钢薄板放入离子氮化炉中，选择NH3为渗氮气体，气压为450Pa，渗氮温度为900℃，阴电极电压为600V，渗氮12h后，再维持正常辉光放电冷却1h，断开电源，关闭气体，随炉冷却至室温，即得TiN-Ti复合覆层的不锈钢薄板。
实施例3：不锈钢薄板表面TiN-Ti复合覆层的制备方法，包括如下步骤：
（1）不锈钢薄板的清洗：为了去除油渍，先用浓度为4.5 %碳酸钠碱液清洗不锈钢薄板10min，清洗时温度为65℃；然后为了去除氧化皮在浓度为4.5%稀硫酸中清洗10min；再将不锈钢薄板先后放入丙酮溶液、乙醇溶液和去离子水中超声35min，以提高基板表面活性，吹干待用；
（2）制备Ti覆层：将步骤（1）中清洗后的不锈钢薄板置于磁控溅射设备的基片台上作为阳极，将金属钛靶放入磁控溅射设备的靶材座上作为阴极，且调节靶材座与基片座的距离，使两者之间的距离保持在20mm；启动机械泵，打开旁抽阀Ⅱ，对真空腔室抽真空；当真空度达到5Pa时，关闭旁抽阀Ⅱ，打开旁抽阀Ⅰ，并启动分子泵，打开闸板阀，采用分子泵对真空腔室进一步抽真空；当分子泵加速后稳定运行直至真空度达到5×10-3Pa；打开氩气阀，通入氩气，对基板进行离子束清洗，清洗时间为5 min；待磁控溅射设备的真空度达到6Pa时，调节磁控溅射沉积条件：预热不锈钢薄板至400℃；放电电压350V、电流16A、沉积速率为1.5μm/min；沉积时间52min，制得Ti覆层的不锈钢薄板；Ti覆层的厚度为78μm；依次关闭电流、放电电压和氩气阀，解除真空，关闭分子泵，开启进气阀，通入空气，并待不锈钢薄板冷却至室温后，取出Ti覆层的不锈钢薄板；
（3）制备TiN-Ti复合覆层：将步骤（2）制得Ti覆层的不锈钢薄板放入离子氮化炉中，选择NH3为渗氮气体，气压为400Pa，渗氮温度为850℃，阴电极电压为650V，渗氮10h后，再维持正常辉光放电冷却1h，断开电源，关闭气体，随炉冷却至室温，即得TiN-Ti复合覆层的不锈钢薄板。
以上显示和描述了本发明的基本原理、主要特征及优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。

Claims (1)

1.一种不锈钢薄板表面TiN-Ti复合覆层的制备方法，其特征在于，包括以下步骤：
(1)不锈钢薄板的清洗：为了去除油渍，先用浓度为3.5～4.5％碳酸钠碱液清洗不锈钢薄板10～15min，清洗时温度为65～75℃；然后为了去除氧化皮在浓度为3.5～4.5％稀硫酸中清洗10～15min；再将不锈钢薄板先后放入丙酮溶液、乙醇溶液和去离子水中超声25～35min，以提高基板表面活性，吹干待用；
(2)制备Ti覆层：将步骤(1)中清洗后的不锈钢薄板置于磁控溅射设备的基片台上作为阳极，将金属钛靶放入磁控溅射设备的靶材座上作为阴极，且调节靶材座与基片座的距离，使两者之间的距离保持在20mm；启动机械泵，打开旁抽阀Ⅱ，对真空腔室抽真空；当真空度达到1～8Pa时，关闭旁抽阀Ⅱ，打开旁抽阀Ⅰ，并启动分子泵，打开闸板阀，采用分子泵对真空腔室进一步抽真空；当分子泵加速后稳定运行直至真空度达到1～5×10-3Pa；打开氩气阀，通入氩气，对基板进行离子束清洗，清洗时间为3～5min；待磁控溅射设备的真空度达到4～8Pa时，调节磁控溅射沉积条件：预热不锈钢薄板至300～500℃；放电电压300V～400V、电流10～20A、沉积速率为1.0～2.0μm/min；沉积时间20～60min，制得Ti覆层的不锈钢薄板；依次关闭电流、放电电压和氩气阀，解除真空，关闭分子泵，开启进气阀，通入空气，并待不锈钢薄板冷却至室温后，取出Ti覆层的不锈钢薄板；
(3)制备TiN-Ti复合覆层：将步骤(2)制得Ti覆层的不锈钢薄板放入离子氮化炉中，选择NH3为渗氮气体，气压为450～500Pa，渗氮温度为800～900℃，阴电极电压为600～700V，渗氮8～12h后，再维持正常辉光放电冷却1h，断开电源，关闭气体，随炉冷却至室温，即得TiN-Ti复合覆层的不锈钢薄板；在所述步骤(3)中不锈钢薄板表面沉积的Ti覆层的厚度为20～80μm。
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