CN108070857A - 超厚dlc涂层 - Google Patents
超厚dlc涂层 Download PDFInfo
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Abstract
本发明公开了一种超厚DLC涂层,由周期性排布于基底材料表面的双层调制结构构成，所述调制结构包括软质层和设于所述软质层之上的硬质层，所述软质层与硬质层周期交替排布于所述基底材料表面。本发明的超厚DLC涂层不仅能够解决硬质相厚度增加时其内部高应力导致的膜层自动崩裂的问题，而且能够大幅提升膜层的整体硬度，同时兼具优良的耐磨性能，具有广阔的应用前景；与此同时，本发明的制备方法通过调节软质层‑硬质层双层调制结构的调制周期、或者其周期数，制备出具有特定厚度的DLC涂层以满足实际生产需求，其操作过程简单，便于规模化批量生产。
Description
技术领域
本发明涉及一种DLC涂层及其制备方法，具体涉及一种超厚DLC涂层及其制备方法，所涉技术是真空PVD镀膜，属于表面处理领域。
背景技术
表面处理是一种广泛用于材料和工件表面改性的处理手段，包括热处理、电镀、喷涂、真空镀膜。近年来，得益于真空镀膜技术的发展，由其制备所得的多层复合薄膜由于具有特殊的性能而越来越受到人们的重视与关注。在此类复合薄膜结构中，通常将构成复合薄膜的周期性排布的重复结构单元称为调制结构，将该调制结构的厚度称为调制周期。
DLC(类金刚石)薄膜是当下最热门的高新材料研究和应用热点之一，DLC具有红外透过性、高硬度、低摩擦系数、高导热、绝缘、合适的禁带宽度等特性，在国防、工业制造、医疗卫生、半导体、食品加工等领域都有广泛的应用。但是，DLC薄膜内应力非常高，可达10GPa以上，膜层的厚度只能控制在0.1-0.2μm之间，否则会开裂，不能粘合在工件表面。通过调整薄膜材料组织结构或者掺杂技术，可以降低内应力，而目前行业广泛能够做到的厚度都在4μm以下，典型厚度在1-2μm之间。
厚度是薄膜的一项重要技术指标，关系到薄膜使用寿命、以及薄膜功能指标是否能够达到实际应用要求。DLC涂层主要涂覆在零件表面，以解决零件表面磨损问题，延长零件的使用寿命。实际应用中要求DLC涂层的厚度达到10μm以上，以使涂层具有足够的韧性、硬度和疲劳寿命。目前所采用的方案为：首先在基底材料上沉积一定厚度的基础层，然后在基础层上沉积DLC涂层，受现有技术的限制，通常基础层的厚度达到8μm以上，而DLC涂层的厚度都在4μm以下；除此之外，可在DLC涂层中掺杂金属元素如Cr等，以增加涂层的沉积厚度，又或者在DLC涂层中生成更多的sp2项，以降低涂层的硬度的方法来达到更厚的涂层。但是，上述方法都无法达到能够满足实际应用需求的DLC涂层的理想厚度。
发明内容
本发明的目的在于提供一种超厚DLC涂层及其制备方法，得到厚度为10μm以上的复合膜层结构的DLC涂层，以满足实际生产的要求。
为达到上述目的，本发明提供如下技术方案：一种超厚DLC涂层,由周期性排布于基底材料表面的双层调制结构构成，该调制结构包括软质层和设于软质层之上的硬质层，软质层与硬质层周期交替排布于基底材料表面。
进一步地，DLC涂层的厚度大于10μm。
进一步地，DLC涂层的厚度为10-50μm。
进一步地，调制结构的调制周期为纳米量级或微米量级调制周期。
进一步地，纳米量级调制周期为0.15-0.90μm，软质层的厚度为0.05-0.10μm，硬质层的厚度为0.10-0.80μm；或微米量级调制周期为1.50-2.80μm，软质层的厚度为0.50-0.80μm，硬质层的厚度为1.00-2.00μm。
进一步地，软质层为CrN、TiN、WC、ZrN、Cr、Ti、W、Zr中的一种，硬质层为类金刚石。
除此之外，本发明还提供了一种制备本发明的超厚DLC涂层的PVD制备方法，具体制备步骤包括：
S1、提供基底材料，进行清洗、干燥，得到干燥后的基底材料；
S2、将干燥后的基底材料置于PVD真空镀膜机的腔体内，密闭抽真空至5.0*10-3Pa时，加热到200-300℃，并继续抽真空；
S3、当压力达到1.0*10-3Pa以下时，开始制备调制结构，沉积软质层，并在软质层上沉积硬质层；
S4、重复步骤S3，以达到目标厚度。
进一步地，步骤S3中采用磁控溅射或者阴极电弧工艺沉积软质层。
进一步地，步骤S3中的调制结构的制备过程包括：通入工艺气体至0.05Pa，开启靶源，在基底材料上施加300-1000V的偏压,将电流调整到10-15A，沉积时间设为5-10min，沉积厚度为0.05-0.10μm的软质层；通入烃类含碳气体，开启离子源电源，在基底材料上施加300-1000V的偏压,电流调节到1-5A，沉积时间设为10-30min，沉积厚度为0.10-0.80μm的硬质层。
进一步地，步骤S3中的调制结构的制备过程包括：通入工艺气体至0.05Pa，开启靶源，在基底材料上施加300-1000V的偏压,将电流调整到60-80A，沉积时间设为5-10min，沉积厚度为0.50-0.80μm的软质层；通入烃类含碳气体，开启离子电源，在基底材料上施加300-1000V的偏压,电流调节到1-5A，沉积时间设为30-60min，沉积厚度为1.00-2.00μm的硬质层。
本发明的有益效果在于：本发明通过真空PVD技术，采用软质层与硬质层周期交替沉积的方式，设计并制备出了超厚DLC涂层；这种DLC涂层具有由软质层-硬质层双层调制结构多周期沉积而成复合膜层，该复合膜层的层间界面可以抑制晶粒的生长，降低涂层的残余应力，提高塑性变形能力，抑制裂纹的形成和扩张，提高涂层的强度和抗冲击能力，以解决硬质层厚度增加时其内部高应力导致的膜层自动崩裂的问题；并且能够提高涂层膜基结合强度，从而大幅提升膜层的整体硬度；同时兼具优良的耐磨性能，进而获得更为满意的服役寿命，具有广阔的应用前景。与此同时，本发明的制备方法通过调节软质层-硬质层双层调制结构的调制周期、或者其周期数，制备出具有特定厚度的DLC涂层以满足实际生产需求，其操作过程简单，便于规模化批量生产。
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合附图详细说明如后。
附图说明
图1为本发明中实施例一超厚DLC涂层的结构示意图，其中11为厚度为0.05-0.10μm的软质层，12为厚度为0.10-0.80μm的硬质层。
图2为本发明实施例一超厚DLC涂层的球磨截面图，其中DLC涂层的厚度为23μm。
图3为本发明中实施例二超厚DLC涂层的结构示意图，其中21为厚度为0.50-0.80μm的软质层，22为厚度为1.00-2.00μm的硬质层。
图4为本发明实施例二超厚DLC涂层的球磨截面图，其中DLC涂层的厚度为16μm。
具体实施方式
下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。
实施例一
请参阅图1，实施例一中的超厚DLC涂层包括直接形成于基底材料表面的软质层11，以及直接形成在软质层上的硬质层12，软质层11与硬质层12周期交替形成于基底材料表面。这种由软质层-硬质层构成的双层调制结构多周期沉积形成的DLC涂层的厚度为23μm，硬度为30-40GPa，摩擦系数为0.06-0.10，调制周期为0.15-0.90μm，内应力可以控制在1.5Gpa以下，与基底材料表面的结合力为81N,该调制结构中软质层11为CrN，厚度为0.05-0.10μm，硬质层12为类金刚石，厚度为0.10-0.80μm。请参阅图2，可以观察到超厚DLC涂层的调制结构的界面平整致密，各层的亮度区分明显，软质层与硬质层交替沉积阻断了大晶粒的生长，在受力的状态下,可降低涂层的残余应力使得涂层结构更加致密，提高塑性变形能力，抑制裂纹的形成和扩张，提高涂层的强度和抗冲击能力。并且该调制结构的调制周期为纳米量级，广泛应用在具有特殊加工要求的机械零部件加工领域、食品加工设备领域；有色金属刀具加工领域、精密模具加工领域、以及医疗器械加工领域。
本实施例中超厚DLC涂层采用真空PVD法制备，具体制备步骤包括：
S1、将基底材料进行超声波清洁处理；
S2、将清洁后的基底材料在真空干燥箱内进行真空干燥；
S3、将基底材料夹到PVD真空镀膜机的工件保持架上，并推入PVD真空镀膜机的腔体内；
S4、密封所述PVD真空镀膜机的腔体，并抽真空；
S5、当真空压力达到5.0*10-3Pa时，加热到200-300℃；
S6、当真空压力达到1.0*10-3Pa以下时，开始制备调制结构，沉积软质层，并在软质层上沉积硬质层。
S7、重复步骤S6，以达到目标厚度。
其中，步骤S6中制备调制结构的过程具体为：通入N2至0.05Pa，采用磁控溅射法沉积软质层，开启磁控溅射靶源，在基底材料上施加300-1000V的偏压,将电流调整到10-15A，沉积时间设为5-10min，沉积厚度为0.05-0.10μm的软质层，关闭磁控溅射靶源；通入烃类含碳气体，开启离子源电源，在基底材料上施加300-1000V的偏压,电流调节到1-5A，沉积时间设为0-30min，沉积厚度为0.10-0.80μm的硬质层，关闭离子源电源。
本发明实施例一的制备方法通过调节软质层-硬质层双层调制结构的调制周期、或者其周期数，制备出具有特定厚度以及纳米量级调制周期的DLC涂层以满足实际生产需求，其操作过程简单，便于规模化批量生产。
实施例二
请参阅图3，实施例二中的超厚DLC涂层包括直接形成于基底材料表面的软质层21，以及直接形成在软质层上的硬质层22，软质层21与硬质层22交替形成于基底材料表面。这种由软质层-硬质层构成的双层调制结构多周期沉积形成的DLC涂层的厚度为16μm，硬度为26-36GPa，摩擦系数为0.06-0.10，调制周期为1.50-2.80μm，而其内应力仅为3.7GPa，与基底材料表面的结合力为76N,该调制结构中软质层21为CrN，厚度为0.50-0.80μm，硬质层22为类金刚石，厚度为1.00-2.00μm。请参阅图4，可以观察到超厚DLC涂层的调制结构的界面平整致密，各层的亮度区分明显，软质层与硬质层交替沉积阻断了大晶粒的生长，在受力的状态下,可降低涂层的残余应力使得涂层结构更加致密，提高塑性变形能力，抑制裂纹的形成和扩张，提高涂层的强度和抗冲击能力；该调制结构的调制周期为微米量级，保持了良好的硬度与耐摩擦性能，这种结构的涂层主要应用在粉末成型模具、有色金属成型模具、以及一般加工要求的机械零部件领域。
本实施例中超厚DLC涂层采用真空PVD法制备，具体制备步骤包括：
S1、将基底材料进行超声波清洁处理；
S2、将清洁后的基底材料在真空干燥箱内进行真空干燥；
S3、将基底材料夹到PVD真空镀膜机的工件保持架上，并推入PVD真空镀
膜机的腔体内；
S4、密封所述PVD真空镀膜机的腔体，并抽真空；
S5、当真空压力达到5.0*10-3Pa时，加热到200-300℃；
S6、当真空压力达到1.0*10-3Pa以下时，开始制备调制结构，沉积软质层，并在软质层上沉积硬质层。
S7、重复步骤S6，以达到目标厚度。
其中，步骤S6中制备调制结构的过程具体为：通入N2至0.05Pa，采用阴极电弧法制备软质层，开启阴极电弧靶源，在基底材料上施加300-1000V的偏压,将电流调整到60-80A，沉积时间设为5-10min，沉积厚度为0.50-0.80μm的软质层，关闭阴极电弧靶源；通入烃类含碳气体，开启离子源电源，在基底材料上施加300-1000V的偏压,电流调节到1-5A，沉积时间设为30-60min，沉积厚度为1.00-2.00μm的硬质层，关闭离子源电源。实施例二所制得的微米级调制解结构对沉积层精度的要求较低，操作更简单。
本发明实施例二的制备方法通过调节软质层-硬质层双层调制结构的调制周期、或者其周期数，制备出具有特定厚度以及微米量级调制周期的DLC涂层以满足实际生产需求，其操作过程简单，便于规模化批量生产。
通过本发明实施例一、实施例二的制备方法，重复其中的步骤S6至目标厚度，均能得到沉积厚度为50μm的DLC涂层，在此不再做赘述。
经由实施例一、实施例二制备得到的超厚DLC涂层与现有技术制备得到的DLC涂层进行比较，得出下表：
根据上表的内容可知，本发明的超厚DLC涂层与现有技术中的DLC涂层相比，厚度达到了10μm以上，硬度和结合力也大大提高，摩擦系数降低，因此，本发明的超厚DLC涂层具有高厚度、高硬度、高结合力、低摩擦系数的优点，进而使得这种涂层的应用范围更广，能够充分满足市场的需求。
本发明中PVD制备方法的优点是：可以在所有金属材料和某些陶瓷材料上加工涂层，涂层种类不同可以实现包括装饰、功能性作用；PVD真空镀膜经过生物相容性和毒性等测试，完全符合行业标准，另外，因为在高真空下镀膜的技术特点，所加工的涂层稳定性最高，对基础材料的影响最小。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (10)
1.一种超厚DLC涂层,其特征在于，由周期性排布于基底材料表面的双层调制结构构成，所述调制结构包括软质层和设于所述软质层之上的硬质层，所述软质层与硬质层周期交替排布于所述基底材料表面。
2.如权利要求1所述的超厚DLC涂层，其特征在于，所述DLC涂层的厚度大于10μm。
3.如权利要求1所述的超厚DLC涂层，其特征在于，所述DLC涂层的厚度为10-50μm。
4.如权利要求1所述的超厚DLC涂层，其特征在于，所述调制结构的调制周期为纳米量级或微米量级调制周期。
5.如权利要求4所述的超厚DLC涂层，其特征在于，所述纳米量级调制周期为0.15-0.90μm，所述软质层的厚度为0.05-0.10μm，所述硬质层的厚度为0.10-0.80μm；或所述微米量级调制周期为1.50-2.80μm，所述软质层的厚度为0.50-0.80μm，所述硬质层的厚度为1.00-2.00μm。
6.如权利要求1至5中任一项所述的超厚DLC涂层，其特征在于，所述软质层为CrN、TiN、WC、ZrN、Cr、Ti、W、Zr中的一种；所述硬质层为类金刚石。
7.如权利要求1至6中任一项所述的超厚DLC涂层的制备方法，其特征在于，所述超厚DLC涂层采用真空PVD法制备，具体制备步骤包括：
S1、提供基底材料，进行清洗、干燥，得到干燥后的基底材料；
S2、将所述干燥后的基底材料置于PVD真空镀膜机的腔体内，密闭抽真空至5.0*10-3Pa时，加热到200-300℃，并继续抽真空；
S3、当压力达到1.0*10-3Pa以下时，开始制备所述调制结构，沉积所述软质层，并在所述软质层上沉积所述硬质层；
S4、重复步骤S3，以达到目标厚度。
8.如权利要求7所述的超厚DLC涂层的制备方法，其特征在于，所述步骤S3中采用磁控溅射或者阴极电弧工艺沉积所述软质层。
9.如权利要求7所述的超厚DLC涂层的制备方法，其特征在于，所述步骤S3中的调制结构的制备过程包括：通入工艺气体至0.05Pa，开启靶源，在所述基底材料上施加300-1000V的偏压,将电流调整到10-15A，沉积时间设为5-10min，沉积厚度为0.05-0.10μm的所述软质层；通入烃类含碳气体，开启离子源电源，在所述基底材料上施加300-1000V的偏压,电流调节到1-5A，沉积时间设为10-30min，沉积厚度为0.10-0.80μm的所述硬质层。
10.如权利要求7所述的超厚DLC涂层的制备方法，其特征在于，所述步骤S3中的调制结构的制备过程包括：通入工艺气体至0.05Pa，开启靶源，在所述基底材料上施加300-1000V的偏压,将电流调整到60-80A，沉积时间设为5-10min，沉积厚度为0.50-0.80μm的所述软质层；通入烃类含碳气体，开启离子电源，在所述基底材料上施加300-1000V的偏压,电流调节到1-5A，沉积时间设为30-60min，沉积厚度为1.00-2.00μm的所述硬质层。
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| CN111153599A (zh) * | 2019-12-27 | 2020-05-15 | 季华实验室 | 纳米结构dlc薄膜、增硬玻璃、制备装备及制备方法 |
| CN112941475A (zh) * | 2021-01-26 | 2021-06-11 | 苏州涂冠镀膜科技有限公司 | 用于水处理过程的去除浮油的dlc薄膜及制备方法 |
| CN113215537A (zh) * | 2021-04-21 | 2021-08-06 | 合肥波林新材料股份有限公司 | 一种连杆用防护涂层的制备方法及其应用 |
| CN113278921A (zh) * | 2021-04-30 | 2021-08-20 | 广东工业大学 | 一种高厚度曲面dlc制品及其制备方法和应用 |
| CN113278921B (zh) * | 2021-04-30 | 2022-04-01 | 广东工业大学 | 一种高厚度曲面dlc制品及其制备方法和应用 |
| NL2031516A (en) | 2021-04-30 | 2022-11-09 | Univ Guangdong Technology | High-thickness curved dlc product and preparation method and application thereof |
| CN114959617A (zh) * | 2022-06-28 | 2022-08-30 | 西安工程大学 | Ag/WS2-DLC涂层及其制备方法 |
| CN114959617B (zh) * | 2022-06-28 | 2024-01-26 | 西安工程大学 | Ag/WS2-DLC涂层及其制备方法 |
| CN115821206A (zh) * | 2022-12-08 | 2023-03-21 | 中国科学院宁波材料技术与工程研究所 | 一种异质多层结构的超厚碳基复合涂层及其制法与应用 |
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