CN113739977B - 一种螺栓预紧力测试用带压电传感器智能垫片及其制备方法 - Google Patents
一种螺栓预紧力测试用带压电传感器智能垫片及其制备方法 Download PDFInfo
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Abstract
本发明属于压电涂层材料技术领域，具体涉及一种螺栓预紧力测试用带压电传感器智能垫片及其制备方法，包括垫片及依次设置于垫片表面的垫片加硬层、ZnO压电功能复合层、耐磨导电电极层构成；其中垫片加硬层为CrN陶瓷涂层，ZnO压电功能复合层由诱导结晶层、ZnO压电层及保护层构成，耐磨导电电极层为Cr/CrN多层膜构成。本发明首次将传感器制备于垫片表面，实现在垫片上实现超声检测；传感器采用多层结构，功能上实现使涂层具有比常规压电涂层更好的硬度、耐磨和韧性；具有抗腐蚀、高耐磨和高韧性的特点，可以保证传感器长期稳定的在垫片表面工作，减少腐蚀等导致的失效可能性。
Description
技术领域
本发明属于压电涂层材料技术领域，具体涉及一种螺栓预紧力测试用带压电传感器智能垫片及其制备方法。
背景技术
螺栓连接是对各种螺纹紧固件连接形式的统称，同焊接、铆接、粘接等连接方式相比，螺栓连接具有拆卸方便、互换性强、造价低廉、可重复使用等优点。螺栓连接的可靠性对于机械设备正常运行和保障人身安全至关重要。螺栓连接结构在服役过程中，由于振动、冲击以及外界温度等环境变化，螺栓连接可能会出现断裂和松动等问题，造成螺栓连接失效，进而引发设备故障，严重时造成重大安全事故。有统计表明，全球每年都会因为螺栓连接结构的断裂和松脱引发的事件导致几十亿美元的财产损失。螺栓连接结构的主要失效形式包括螺栓断裂、螺牙脱落、表面疲劳、松动和化学腐蚀等。其中螺栓断裂和松动是最为严重的失效形式。螺栓断裂主要和螺栓材料、强度、螺栓结构、表面状况、载荷和使用环境等因素相关，影响因素复杂，具体失效机理需要针对具体的使用工况进行系统分析。螺栓松动则是目前螺栓连接中普遍存在难以解决的问题。一般螺栓连接松动是指随着设备使用时间的增长，由于外载冲击、长期振动等因素，引起螺栓和螺母产生相对周向位移，造成螺栓夹紧力逐渐下降到一定水平而丧失夹紧功能的现象。螺栓连接松动初期可能并不会影响设备正常运行，但随着松动加剧，可能发展为连接失效，甚至造成整个螺栓连接的失效，引发重大事故，因此研究螺栓连接结构松脱等失效现象对保障装备的安全性具有重要的意义。
螺栓的预紧力是夹紧力的保证，只有高的预紧力才能获得高的夹紧力。螺栓的松脱、预紧等和螺栓的预紧力有密切关系。目前应用最广泛的控制螺栓预紧力方法为扭矩法，根据经验，在拧紧过程中，有50％的扭矩消耗在螺栓端面的摩擦上，有40％消耗在螺纹的摩擦上，仅有10％的扭矩用来产生预紧力。当通过拧紧力矩控制预紧力时，人们希望拧紧力与螺栓预紧力呈线性关系，这样通过控制拧紧力矩的大小就可以计算得到预紧力值。但在实际中，由于受摩擦因数和几何参数偏差的影响，在一定的拧紧力矩下，预紧力变化比较大，所以通过拧紧力矩来控制螺栓预紧力的精度不高，存在较大的误差，最大可达±40％。这也就导致螺栓预紧力的离散度过大，严重影响连接系统的安全性。
除了扭矩法之外，还有光栅法、导波法、颜色法等螺栓预紧力的检测技术。但传统的光纤光栅法需要在螺栓上打孔，严重影响螺栓的安全性，而且只能测出螺栓的整体受力情况，对应力的径向分布无法精确测出。传统的贴片超声法操作简单，但由于压电片和螺栓之间存在粘结用的胶层，厚度不可控，寿命不可靠，容易发生脱落，因此不适合于现场使用。溅射镀膜法可以在螺栓上进行压电薄膜的制备获得传感器也可以监测预紧力的变化，但需要对螺栓进行镀膜，对镀膜设备和成本提出了更高的要求。新的预紧力监测技术的开发具有非常重要的现实意义。
发明内容
本发明的目的之一在于提供一种螺栓预紧力测试用带压电传感器智能垫片，克服现有螺栓预紧力监测需要在螺栓上镀制压电材料的困难，同时也是为了克服压电涂层材料韧性不足，耐磨差的缺点。
本发明的目的之二在于提供一种螺栓预紧力测试用带压电传感器智能垫片的制备方法，制备工艺简便，易于调节。
本发明实现目的之一所采用的方案是：一种螺栓预紧力测试用带压电传感器智能垫片，包括垫片及依次设置于垫片表面的垫片加硬层、ZnO压电功能复合层、耐磨导电电极层构成；其中垫片加硬层为CrN陶瓷涂层，ZnO压电功能复合层由诱导结晶层、ZnO压电层及保护层构成，耐磨导电电极层为Cr/CrN多层膜构成。
优选地，所述ZnO压电功能复合层中，诱导结晶层为Ti诱导结晶层，ZnO压电层为(002)取向的ZnO压电层，保护层为AlCrO保护层构。
优选地，所述Ti诱导结晶层的厚度为0.5-2微米，结晶取向为(002)择优取向。
优选地，所述ZnO压电层的厚度为5-20微米，绝缘电阻大于200MΩ。
优选地，所述AlCrO保护层的厚度为2-5微米，绝缘电阻大于200MΩ。
优选地，所述的垫片加硬层的厚度为2-3微米，硬度为15-20GPa。
优选地，所述耐磨导电电极层的厚度为3-5微米，单层Cr层厚度为3-20纳米，CrN层厚度为5-20纳米，调制周期为8-40纳米，其绝缘电阻小于1000欧姆，硬度10-15GPa。
本发明实现目的之二所采用的方案是：一种所述的螺栓预紧力测试用带压电传感器智能垫片的制备方法，包括以下步骤：
(1)在100-150℃、氩气和氢气环境中，采用弧光放电方法对预处理好的垫片进行等离子刻蚀；
(2)刻蚀结束后，首先通入氮气，采用电弧放电方法烧蚀Cr靶制备垫片加硬层CrN涂层，沉积气压为0.1-1Pa，电流为50-100A，涂层厚度为2-3微米，涂层硬度为15-20GPa；
(3)随后进行ZnO压电功能复合层的制备，首先采用射频磁控溅射法在氩气环境0.3-0.5Pa溅射Ti靶沉积0.5-2微米的Ti结晶诱导层；随后采用射频磁控溅射法在1-3Pa的氧气环境中溅射Zn靶沉积5-20微米的ZnO压电层，在ZnO压电层的基础上采用射频磁控溅射AlCr靶在氧气环境中沉积2-5微米的AlCrO保护层；
(4)最后采用电弧放电法进行Cr/CrN耐磨导电电极层的制备，即得到所述螺栓预紧力测试用带压电传感器智能垫片。
本发明中将CrN和Cr/CrN以及ZnO进行综合利用，利用CrN的硬度对ZnO进行良好的支撑，利用Cr/CrN对ZnO涂层进行良好的保护，使其不但具有导电功能，同时还具有高硬度和高韧性，大幅度提高传感器的耐磨耐冲击性能。此外，为了提高压电涂层和垫片的结合力，本发明还采用离子刻蚀的方法去除表面的污染物，提高涂层和基体之间的附着力，保证传感器在长时使用的过程中也不会发生剥落等情况。克服现有螺栓预紧力监测需要在螺栓上镀制压电材料的困难，同时也是为了克服压电涂层材料韧性不足，耐磨差的缺点。同时避免了现有大部分的压电涂层当经历冲击和变形时将会引起破裂，经常导致涂层失去压电效应的问题。本发明的传感器智能垫片压采用复合材料的设计思路，将高硬度的CrN硬质涂层、ZnO压电复合涂层以及Cr/CrN导电硬质涂层进行复合，实现在垫片上制备出高硬度耐磨耐压的传感器。如果没有CrN加硬层，垫片在受压的过程中将会发生明显的变形引起ZnO压电材料的破裂，导致传感器失去功能。表面如果没有导电的Cr/CrN导电金属陶瓷，则普通电极就会在收到摩擦时产生磨损。此外本发明中多层结构的使用使传感器具有较低的应力，可以在垫片表面长期稳定的工作。
在涂层的制备过程中，对于垫片材料，由于大部分为金属材料，如果不采用离子刻蚀，涂层表面会存在一定的氧化物。如果采用传统的辉光离子放电清洗，由于能量低，无法去除表面的氧化物，则无法保证传感器长期稳定的附着在垫片表面。而采用高能量密度的电弧放电等离子刻蚀时，去除氧化层，不能真正提高涂层的附着力。当采用离子刻蚀时，可以去除表面各种氧化物，使表面达到一个清洁的状态，这样后续的涂层就可以和垫片表面形成良好的结合，保证涂层的附着力。
本发明中采用弧光放电方法(电弧离子镀技术)制备CrN加硬层主要是考虑其沉积速度快，同时可以获得比较高的硬度。而且在镀CrN涂层之前，还可以作为刻蚀用。在镀Ti结晶诱导层时，采用磁控溅射方法进行制备，主要是利用磁控溅射方法容易控制取向，同时避免电弧离子镀方法时形成的颗粒污染导致后续的ZnO涂层中有缺陷引起传感器在承受电压时引起击穿，导致传感器的过早失效。在ZnO制备结束后，采用射频磁控溅射技术制备AlCrO绝缘层作为保护层，主要是利用AlCrO的高绝缘性和高耐磨性。最后采用Cr/CrN作为电极层主要考虑到Cr具有良好的导电性，而CrN具有良好的硬度，所以两者结合就形成了金属陶瓷，不但具有高硬度，同时还具有高导电性，实现了导电和耐磨的完美结合。
本发明具有以下优点和有益效果：
本发明首次将传感器制备于垫片表面，实现在垫片上实现超声检测；传感器采用多层结构，功能上实现使涂层具有比常规压电涂层更好的硬度、耐磨和韧性；本发明设计了导电耐磨Cr/CrN金属陶瓷涂层充分利用Cr金属的导电性和CrN涂层的高耐磨性能，实现导电耐磨耐压一体化设计；AlCrO保护涂层的使用，不但可以大幅度提高ZnO涂层的耐候性能，延长其在大气环境中的工作时间，同时也使其具有良好的绝缘和耐磨性能；本发明将电弧离子镀技术大功率射频溅射技术应用于传感器的制备中，不但沉积速率快，同时在一个设备中实现了多层涂层材料的制备，大幅度降低传感器的制备成本。
本发明的思路是改变目前测直接测螺栓应力的方法，采用垫片来测量螺栓应力，其原理主要是利用超声波在垫片中的传播收到应力的影响来测量，当预紧力增大时，超声波的声强变低，通过声波声强的降低幅度来表征预紧力的变化。该该种方法的好处就是可以避免不同的螺栓材料对声波的吸收不一样引起的测量的困难和大尺寸螺栓制备传感器的困难。实现同一种垫片用在不同的场合对应力进行监测。
本发明的制备方法所制备带传感器智能垫片具有抗腐蚀、高耐磨和高韧性的特点，可以保证传感器长期稳定的在垫片表面工作，减少腐蚀等导致的失效可能性。同时其采用的电弧离子镀和射频溅射技术为工业上的通用技术，工业生产批量容易实现，加工效率较高，可以大幅度降低厂家的生产成本。
附图说明
图1.为本发明中所采用的涂层制备装置的示意图；
图2.为本发明设计的涂层结构示意图；
图3为本发明的应用示意图；
其中，1.刻蚀靶；2.挡板；3.真空室；4.加热器；5.AlCr靶；6.Zn靶；7.Ti靶；8.工件架；11.垫片基体；12.CrN加硬层；13.Ti结晶诱导层；14.ZnO压电涂层；15.AlCrO涂层；16.Cr/CrN导电耐磨层；21.螺母；22.夹持部件；23.带传感器垫片；24.传感器；25.无传感器垫片；26.螺栓。
具体实施方式
为更好的理解本发明，下面的实施例是对本发明的进一步说明，但本发明的内容不仅仅局限于下面的实施例。
实施例1：在100℃、氩气和氢气环境中，对抛光好的垫片进行等离子刻蚀；刻蚀结束后，首先采用电弧放电方法进行CrN垫片增硬层的制备，沉积气压为0.1Pa，电流为50A，涂层厚度为2微米，涂层硬度为15GPa；随后进行ZnO压电功能复合层的制备，首先在0.3Pa沉积0.5微米的Ti结晶诱导层；随后在1-3Pa沉积5-20微米的ZnO压电层，在压电层的基础上沉积2微米的AlCrO保护层；最后进行耐磨导电Cr/CrN涂层的制备，厚度为3微米，单层Cr层厚度为3纳米，CrN层厚度为7纳米，调制周期为10纳米，其绝缘电阻小于1000欧姆，硬度10GPa；制备结束后获得带传感器的智能垫片。
实施例2：在150℃、氩气和氢气环境中，对抛光好的垫片进行等离子刻蚀；刻蚀结束后，首先采用电弧放电方法进行CrN垫片增硬层的制备，沉积气压为1Pa，电流为100A，涂层厚度为3微米，涂层硬度为20GPa；随后进行ZnO压电功能复合层的制备，首先在0.5Pa沉积2微米的Ti结晶诱导层；随后在3Pa沉积20微米的ZnO压电层，在压电层的基础上沉积5微米的AlCrO保护层；最后进行耐磨导电Cr/CrN涂层的制备，厚度为5微米，单层Cr层厚度为10纳米，CrN层厚度为10纳米，调制周期为20纳米，其绝缘电阻小于1000欧姆，硬度15GPa；制备结束后获得带传感器的智能垫片。
实施例3：在120℃、氩气和氢气环境中，对抛光好的垫片进行等离子刻蚀；刻蚀结束后，首先采用电弧放电方法进行CrN垫片增硬层的制备，沉积气压为0.5Pa，电流为80A，涂层厚度为2.5微米，涂层硬度为16GPa；随后进行ZnO压电功能复合层的制备，首先在0.4Pa沉积1微米的Ti结晶诱导层；随后在3Pa沉积15微米的ZnO压电层，在压电层的基础上沉积2微米的AlCrO保护层；最后进行耐磨导电Cr/CrN涂层的制备，厚度为4微米，单层Cr层厚度为4纳米，CrN层厚度为16纳米，调制周期为20纳米，其绝缘电阻小于1000欧姆，硬度12GPa；制备结束后获得带传感器的智能垫片。
实施例4：在130℃、氩气和氢气环境中，对抛光好的垫片进行等离子刻蚀；刻蚀结束后，首先采用电弧放电方法进行CrN垫片增硬层的制备，沉积气压为0.5Pa，电流为100A，涂层厚度为3微米，涂层硬度为20GPa；随后进行ZnO压电功能复合层的制备，首先在0.4Pa沉积1微米的Ti结晶诱导层；随后在2Pa沉积10微米的ZnO压电层，在压电层的基础上沉积3微米的AlCrO保护层；最后进行耐磨导电Cr/CrN涂层的制备，厚度为5微米，单层Cr层厚度为5纳米，CrN层厚度为5纳米，调制周期为10纳米，其绝缘电阻小于1000欧姆，硬度15GPa；制备结束后获得带传感器的智能垫片。
实施例5：在140℃、氩气和氢气环境中，对抛光好的垫片进行等离子刻蚀；刻蚀结束后，首先采用电弧放电方法进行CrN垫片增硬层的制备，沉积气压为0.5Pa，电流为80A，涂层厚度为2微米，涂层硬度为15GPa；随后进行ZnO压电功能复合层的制备，首先在0.4Pa沉积2微米的Ti结晶诱导层；随后在2.5Pa沉积20微米的ZnO压电层，在压电层的基础上沉积4微米的AlCrO保护层；最后进行耐磨导电Cr/CrN涂层的制备，厚度为4微米，单层Cr层厚度为10纳米，CrN层厚度为10纳米，调制周期为20纳米，其绝缘电阻小于1000欧姆，硬度10-15GPa；制备结束后获得带传感器的智能垫片。
实施例6：在140℃、氩气和氢气环境中，对抛光好的垫片进行等离子刻蚀；刻蚀结束后，首先采用电弧放电方法进行CrN垫片增硬层的制备，沉积气压为1Pa，电流为90A，涂层厚度为2.5微米，涂层硬度为16GPa；随后进行ZnO压电功能复合层的制备，首先在0.3Pa沉积1.5微米的Ti结晶诱导层；随后在3Pa沉积14微米的ZnO压电层，在压电层的基础上沉积3微米的AlCrO保护层；最后进行耐磨导电Cr/CrN涂层的制备，厚度为5微米，单层Cr层厚度为10纳米，CrN层厚度为10纳米，调制周期为20纳米，其绝缘电阻小于1000欧姆，硬度15GPa；制备结束后获得带传感器的智能垫片。
图1所示为本发明所用的装置，装置的真空室3由炉壁围成，真空室3的尺寸为500x500x500 mm。真空室3的四个角是加热器4，加热功率25千瓦，提高加热效率。4个靶分4列安装在炉壁上，分别安装一个刻蚀靶1，一个镀膜AlCr靶5、一个Zn靶6和一个Ti靶7，样品装在工件架8上。刻蚀靶1前面安装有挡板2，主要是为了阻挡金属离子。本系统多靶的布局使真空室3中等离子体密度大幅度增加，工件完全浸没在等离子体中。使涂层沉积速率、硬度、附着力得到较大的提高。由于对靶结构进行了优化，磁场分布更均匀，使磁控溅射靶面刻蚀均匀，提高了涂层的均匀性。
图2为本发明设计的涂层结构示意图，从图中可以看出，由下至上依次为垫片基体11、CrN加硬层12、Ti结晶诱导层13、ZnO压电涂层14、AlCrO涂层15、Cr/CrN导电耐磨层16，涂层结构上存在成分梯度和硬度梯度，降低了涂层的应力，增加了涂层的韧性，可沉积较厚的和耐磨耐压的压电涂层。
图3为本发明智能垫片应用于螺栓连接时的结构示意图，通过智能垫片的应用可以实时监测螺栓的预紧力。其中包括螺母21、夹持部件22、带传感器垫片23、传感器24、无传感器垫片25、螺栓26，其中带传感器垫片23、传感器24组成本发明的带压电传感器智能垫片。
以上所述是本发明的优选实施方式而已，当然不能以此来限定本发明之权利范围，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和变动，这些改进和变动也视为本发明的保护范围。
Claims (5)
1.一种螺栓预紧力测试用带压电传感器智能垫片的制备方法，其特征在于：
所述螺栓预紧力测试用带压电传感器智能垫片包括垫片及依次设置于垫片表面的垫片加硬层、ZnO压电功能复合层、耐磨导电电极层；其中，垫片加硬层为CrN陶瓷涂层，ZnO压电功能复合层由诱导结晶层、ZnO压电层及保护层构成，耐磨导电电极层由Cr/CrN导电耐磨层构成；
所述制备方法包括以下步骤：
（1）在100-150℃、氩气和氢气环境中，采用弧光放电方法对预处理好的垫片进行等离子刻蚀；
（2）刻蚀结束后，首先通入氮气，采用电弧放电方法烧蚀Cr靶制备垫片加硬层CrN涂层，沉积气压为0.1-1Pa，电流为50-100A，涂层厚度为2-3微米，涂层硬度为15-20GPa；
（3）随后进行ZnO压电功能复合层的制备，首先采用射频磁控溅射法在0.3-0.5Pa的氩气环境中溅射Ti靶沉积0.5-2微米的Ti诱导结晶层；随后采用射频磁控溅射法在1-3Pa的氧气环境中溅射Zn靶沉积5-20微米的ZnO压电层，在ZnO压电层的基础上采用射频磁控溅射法在氧气环境中溅射AlCr靶沉积2-5微米的AlCrO保护层；
（4）最后采用电弧放电法进行Cr/CrN耐磨导电电极层的制备，即得到所述螺栓预紧力测试用带压电传感器智能垫片。
2.根据权利要求1所述的螺栓预紧力测试用带压电传感器智能垫片的制备方法，其特征在于：所述Ti诱导结晶层的结晶取向为（002）择优取向。
3. 根据权利要求1所述的螺栓预紧力测试用带压电传感器智能垫片的制备方法，其特征在于：所述ZnO压电层的绝缘电阻大于200 MΩ。
4.根据权利要求1所述的螺栓预紧力测试用带压电传感器智能垫片的制备方法，其特征在于：所述AlCrO保护层的绝缘电阻大于200MΩ。
5.根据权利要求1所述的螺栓预紧力测试用带压电传感器智能垫片的制备方法，其特征在于：所述耐磨导电电极层的厚度为3-5微米，单层Cr层厚度为3-20纳米，CrN层厚度为5-20纳米，调制周期为8-40纳米，其绝缘电阻小于1000欧姆，硬度为10-15GPa。
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