CN113088942A - 一种手术电极用WS2掺杂Ni-P-PTFE医用复合涂层及其制备方法 - Google Patents
一种手术电极用WS2掺杂Ni-P-PTFE医用复合涂层及其制备方法 Download PDFInfo
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Abstract
一种手术电极用WS2掺杂Ni‑P‑PTFE医用复合涂层及其制备方法，制备步骤为：1)将基体放入丙酮中，采用超声波清洗；2)先采用化学法对基体进行除油，然后再利用盐酸溶液进行酸洗活化；3)通过化学镀在基材上镀一层Ni‑P，作为过渡层；4)通过化学镀在Ni‑P层上镀Ni‑P‑WS2‑PTFE层。该医用复合涂层主要应用于手术电极，能够耐磨减磨，有低摩擦系数的同时起到抗粘连的作用，以此提高手术电极的切割效率与操作精度。
Description
技术领域
本发明属于材料学领域，涉及一种硬质保护涂层，具体来说是一种手术电极用低摩擦、抗粘连WS2掺杂Ni-P-PTFE医用复合涂层及其制备方法。
背景技术
随着社会的进步和科技的发展，人们越来越重视医疗领域的发展前景，在各种医疗手术中，手术刀是必不可少的一项工具。由于时代的进步与技术的发展，高频手术电刀与电凝的出现，大大减少了手术时的大量出血，提高了手术的切割效率。
高频手术电刀在工作时，高频电流通过电极与肌体接触，对组织进行加热，分离和凝固，从而达到止血的目的。可是手术电刀电极表面同时也会产生组织粘附，增加电极与组织之间的摩擦因数，从而降低电刀的切割效率和操作精度。因此为了保证手术电刀工作时，电极表面有着抗粘连以及较低的摩擦，人们通过对电极表面处理来解决这些问题。
众多学者研究表明，Ni-P-PTFE复合涂层摩擦系数较低，具有优秀的润滑减摩性能。同时据大量期刊文献报道，纳米WS2粒子以较低的摩擦系数，抗咬合性而被广泛应用于干摩擦润滑领域，当其复合进入Ni-P基质合金，亦能明显降低Ni-P涂层的摩擦系数。但是此前关于WS2，PTFE双润滑粒子组合掺杂对Ni-P涂层润滑性影响的相关研究极少，在医疗器械领域的应用也极少，本发明提供了一种手术电极用低摩擦、抗粘连WS2掺杂Ni-P-PTFE医用复合涂层及其制备方法，可制备出低摩擦，抗粘连的手术电极用医用复合涂层，同时本发明的方法工艺简单、成本低、沉积速度快、所得Ni-P-WS2-PTFE复合涂层结合强度好，对扩大Ni-P-PTFE涂层在医疗器械领域中的应用具有重要意义。
发明内容
针对现有技术中的上述技术问题，本发明提供了一种手术电极用低摩擦、抗粘连WS2掺杂Ni-P-PTFE医用复合涂层及其制备方法，所述的WS2掺杂Ni-P-PTFE医用复合涂层能够解决现有技术中在医用环境下低摩擦、耐腐蚀和抗粘连的技术问题。
根据本发明的第一方面，提供一种手术电极用低摩擦、抗粘连WS2掺杂Ni-P-PTFE医用复合涂层及其制备方法，其特征在于，所述复合涂层包括形成在基体上的Ni-P过渡层和Ni-P-WS2-PTFE表面层，所述基体为手术用电刀与双极电凝。
具体情况下，所述Ni-P过渡层和所述Ni-P-WS2-PTFE表面层分别通过化学镀工艺沉积而成。
根据本发明的第二方面，还提供上述WS2掺杂Ni-P-PTFE医用复合涂层的制备方法，其特征在于，包括如下步骤：
1)将基体放入丙酮中，采用超声波清洗；
2)采用化学法对基体进行除油，然后再利用盐酸溶液进行酸洗活化；
3)通过化学镀在基体上镀一层Ni-P，作为过渡层；
4)通过化学镀在Ni-P层上镀Ni-P-WS2-PTFE层。
具体情况下，步骤1)中，采用丙酮对基体表面进行超声波清洗；即将基体放入含有丙酮溶液的容器中，浸没，再将容器放置于超声波清洗仪中，功率设置为90W，时间设置为30min，对基材有机除油，获得洁净的基体表面。
具体情况下，步骤2)中，化学除油所需的溶液中含有NaOH、Na2CO3、Na3PO4，在所述的溶液中，NaOH的浓度为20g/L，Na2CO3的浓度为30g/L，Na3PO4的浓度为30g/L，溶液加热到70-80℃，然后将基体加入到除油溶液中，除油时间为10-15min，从而使得基体表面的油污被除尽。
具体情况下，步骤2)中，盐酸溶液的体积分数为40-60％，将经过除油的基体浸泡盐酸溶液中进行酸洗活化，溶液温度为常温，浸泡时间为3-5min，使得基体表面的氧化层被除去，得到完全暴露的基材，让基体的表面活性大大增强，利于接下来Ni-P层的沉积。
优选情况下，步骤3)中，Ni-P镀液的pH值是4.8，施镀温度为90℃，沉积时间为20min。
优选情况下，步骤4)中，化学镀Ni-P-WS2-PTFE镀液中的WS2浓度为4.0g/L，PTFE浓度为50ml/L，pH值是4.8，温度为85℃，沉积时间为15min。镀液中添加的WS2优选采用粒径为1μm以下，更优选情况下，采用粒径为100-300nm的WS2，从而为涂层带来纳米尺度效应。
本发明的一种手术电极用低摩擦、抗粘连WS2掺杂Ni-P-PTFE医用复合涂层及其制备方法，是根据化学镀Ni-P-WS2-PTFE复合涂层过程中，镀液中WS2含量随该复合镀液中WS2粒子浓度的增加呈先增加后下降的趋势。镀液中WS2浓度为4.0g/L时，该掺杂量下所得复合涂层WS2粒子含量达极大值。涂层中PTFE含量随着镀液中WS2浓度的增加而一直下降，且涂层中P元素的含量随WS2粒子掺杂量的增加而先下降后增加，以上元素含量均在WS2粒子浓度为4.0g/L时达到最值。同时在化学镀过程中，随复合镀液中WS2粒子掺杂量的增加，复合涂层的Ni(111)衍射峰的强度随之先增加后降低；WS2、PTFE颗粒在涂层中的复合量和分布情况与WS2掺杂量密切相关，当WS2浓度为4.0g/L时，WS2粒子复合量达最大值，且分布最为均匀。在化学镀Ni-P-WS2-PTFE复合涂层过程中，随镀液中WS2粒子掺杂量的增加，涂层的耐磨性随之先增加后下降，在WS2掺杂量为4.0g/L时达到最值；而其摩擦系数随之增加而先下降后增加。
本发明和已有技术相比，其技术进步是显著的。本发明通过在Ni-P-PTFE医用复合涂层中掺杂WS2，对WS2的浓度以及制备工艺参数进行优化，制备出具有低摩擦、优良耐磨性、抗粘连的Ni-P-PTFE医用复合涂层，且将其应用于手术电极上，从而降低手术电极的摩擦系数，提高手术电极的抗组织粘连，以此获得更好的切割效率和操作精度。
附图说明
图1是实施例1-7在化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度分别为0.0g/L、1.0g/L、2.0g/L、3.0g/L、4.0g/L、5.0g/L和6.0g/L时所得到相对应的Ni-P-WS2-PTFE复合涂层的成分；
图2是实施例1-7在化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度分别为0.0g/L、1.0g/L、2.0g/L、3.0g/L、4.0g/L、5.0g/L和6.0g/L时所得到相对应的Ni-P-WS2-PTFE复合涂层的XRD谱图；
图3a是化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度为0.0g/L时，所得的化学镀Ni-P-WS2-PTFE复合涂层SEM图；
图3b是化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度为1.0g/L时，所得的化学镀Ni-P-WS2-PTFE复合涂层SEM图；
图3c是化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度为2.0g/L时，所得的化学镀Ni-P-WS2-PTFE复合涂层SEM图；
图3d是化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度为3.0g/L时，所得的化学镀Ni-P-WS2-PTFE复合涂层SEM图；
图3e是化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度为4.0g/L时，所得的化学镀Ni-P-WS2-PTFE复合涂层SEM图；
图3f是化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度为5.0g/L时，所得的化学镀Ni-P-WS2-PTFE复合涂层SEM图；
图3g是化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度为6.0g/L时，所得的化学镀Ni-P-WS2-PTFE复合涂层SEM图；
图4是实施例1-7化学镀过程中Ni-P-WS2-PTFEE镀液中WS2的浓度分别为0.0g/L、1.0g/L、2.0g/L、3.0g/L、4.0g/L、5.0g/L和6.0g/L时所得到相对应的Ni-P-WS2-PTFE复合涂层的硬度和摩擦系数曲线图；
图5是实施例1-7化学镀过程中Ni-P-WS2-PTFE镀液中WS2的浓度分别为0.0g/L、1.0g/L、2.0g/L、3.0g/L、4.0g/L、5.0g/L和6.0g/L时所得到相对应的Ni-P-WS2-PTFE复合涂层在运行载荷为30N，运行时间10min的磨损失重曲线图；
具体实施方式
下面通过具体实施例和附图对本发明作进一步的详细说明，但并不限制本发明。除特殊说明外，各具体实施例中所用试剂均为商业可获得，所用操作条件为现有技术中的常用条件。
本发明所用的制备、表征和测量仪器：
本发明的各实施例中所得的Ni-P-WS2-PTFE复合涂层采用Bruker公司的D8ADVANCE型X射线衍射(XRD)仪分析薄膜的晶相结构；
采用附带有能谱仪(EDS)的QuantaFEG450型场发射环境扫描电子显微镜(美国FEI公司)分析Ni-P-WS2-PTFE复合涂层的成分及微观形貌；
采用美国Agilent公司生产NANO Indenter G200型纳米压痕仪测量Ni-P-WS2-PTFE复合涂层的硬度；
采用兰州中科华凯科技有限公司的HSR-2M往复摩擦磨损仪测量复合涂层的摩擦系数及磨损失重量。
实施例1
一种手术电极用低摩擦、抗粘连WS2掺杂Ni-P-PTFE医用复合涂层及其制备方法，其制备过程包括如下步骤：
(1)将基体放入转装有100mL丙酮的烧杯中，采用超声波清洗10min，功率设置为90W；
(2)接着采用化学法对基体进行除油，除油温度为70-80℃，时间为10-15min，再利用体积分数40-60％的盐酸对基材进行酸洗活化3-5min；
(3)利用化学镀在基体上镀上Ni-P层，作为过渡层，镀液温度为90℃，化学镀过程中镀液的pH值控制在4.8；
(4)接着在Ni-P层上镀Ni-P-PTFE层，镀液温度为80℃，化学镀过程中镀液的pH值控制在4.8。
在上述的化学镀过程中，控制Ni-P镀液温度为90℃，pH值为4.8，施镀20min得到Ni-P层；控制Ni-P-PTFE镀液温度为80℃，pH值为4.8，在Ni-P层上继续施镀15min得到Ni-P-PTFE层，完成后得到Ni-P-PTFE复合涂层。包括基体、Ni-P层和Ni-P-PTFE复合涂层，其自下而上依次为基体、Ni-P层和Ni-P-PTFE复合涂层。
实施例2
一种在基体上化学镀Ni-P、Ni-P-WS2-PTFE复合涂层的制备方法，只是制备过程的步骤(4)中化学镀过程中Ni-P-PTFE镀液中加入WS2粒子，WS2的浓度为1.0g/L，镀液温度为85℃，化学镀过程中镀液的pH值控制在4.8。
其它同实施例1。
实施例3
一种在基体上化学镀Ni-P、Ni-P-WS2-PTFE复合涂层的制备方法，只是制备过程的步骤(3)中化学镀过程中Ni-P-PTFE镀液中加入WS2粒子，WS2的浓度为2.0g/L，镀液温度为85℃，化学镀过程中镀液的pH值控制在4.8。
其它同实施例1。
实施例4
一种在基体上化学镀Ni-P、Ni-P-WS2-PTFE复合涂层的制备方法，只是制备过程的步骤(3)中化学镀过程中Ni-P-PTFE镀液中加入WS2粒子，WS2的浓度为3.0g/L，镀液温度为85℃，化学镀过程中镀液的pH值控制在4.8。
其它同实施例1。
实施例5
一种在基体上化学镀Ni-P、Ni-P-WS2-PTFE复合涂层的制备方法，只是制备过程的步骤(3)中化学镀过程中Ni-P-PTFE镀液中加入WS2粒子，WS2的浓度为4.0g/L，镀液温度为85℃，化学镀过程中镀液的pH值控制在4.8。
其它同实施例1。
实施例6
一种在基体上化学镀Ni-P、Ni-P-WS2-PTFE复合涂层的制备方法，只是制备过程的步骤(3)中化学镀过程中Ni-P-PTFE镀液中加入WS2粒子，WS2的浓度为5.0g/L，镀液温度为85℃，化学镀过程中镀液的pH值控制在4.8。
其它同实施例1。
实施例7
一种在基体上化学镀Ni-P、Ni-P-WS2-PTFE复合涂层的制备方法，只是制备过程的步骤(3)中化学镀过程中Ni-P-PTFE镀液中加入WS2粒子，WS2的浓度为6.0g/L，镀液温度为85℃，化学镀过程中镀液的pH值控制在4.8。
其它同实施例1。
分别对实施例1-7即化学镀过程中，即Ni-P-WS2-PTFE镀液中WS2的浓度分别为0.0g/L、1.0g/L、2.0g/L、3.0g/L、4.0g/L、5.0g/L和6.0g/L时所得到相对应的Ni-P-WS2-PTFE复合涂层的成分进行测定，结果如图1所示。从图1可以看出，复合涂层中W(代表WS2)含量随化学镀Ni-P-PTFE复合镀液中WS2浓度的增加呈先增加后下降的趋势。镀液中WS2浓度在0-4.0g/L之间时，所得复合涂层中W的含量随着镀液中WS2浓度的增加而增加，当复合镀液中WS2粒子浓度为4.0g/L时，此浓度下所得复合涂层中WS2粒子含量达最大值。复合涂层中F(代表PTFE)含量变化亦如图1所示，易知涂层中F含量随复合镀液中WS2浓度的增加呈一直下降的趋势。此外，由图1还可知，涂层中P元素含量呈先下降后增加的趋势。
分别对实施例1-7即化学镀过程中，即Ni-P-WS2-PTFE镀液中WS2的浓度分别为0.0g/L、1.0g/L、2.0g/L、3.0g/L、4.0g/L、5.0g/L和6.0g/L时所得到相对应的Ni-P-WS2-PTFE复合涂层的XRD图谱进行测定，结果如图2所示。从图2可以看出，不同WS2掺杂量下所得复合涂层的X射线衍射图谱形状基本相同，所有掺杂量下所得复合涂层均在2θ＝45°附近出现馒头包状Ni(111)晶面的衍射峰；除WS2掺杂量为5.0、6.0g/L以外，其余掺杂量下所得涂层均在2θ＝18.4°的位置出现PTFE的衍射峰。各掺杂量下所得Ni-P-WS2-PTFE复合涂层的PTFE衍射峰强度随WS2粒子浓度提高几乎不发生变化；Ni(111)衍射峰的强度随着镀液中WS2粒子浓度增加呈先增加后下降的趋势，当复合镀液中WS2粒子浓度为4.0g/L时，Ni(111)衍射峰的强度达最大值。
分别对实施例1-7即化学镀过程中，即Ni-P-WS2-PTFE镀液中WS2的浓度分别为0.0g/L、1.0g/L、2.0g/L、3.0g/L、4.0g/L、5.0g/L和6.0g/L时所得到相对应的Ni-P-WS2-PTFE复合涂层的硬度与摩擦系数进行测定，结果如图4所示。当复合镀液中WS2粒子浓度在0-4.0g/L之间时，该系列复合涂层的硬度和摩擦系数变化不大；当镀液中WS2粒子浓度进一步增加时，镀液稳定性较低，此时复合进入涂层中WS2、PTFE复合粒子明显减少，因此，在此掺杂量范围内所得涂层硬度值随之大幅增加。
分别对实施例1-7即化学镀过程中，即Ni-P-WS2-PTFE镀液中WS2的浓度分别为0.0g/L、1.0g/L、2.0g/L、3.0g/L、4.0g/L、5.0g/L和6.0g/L时所得到相对应的Ni-P-WS2-PTFE复合涂层的涂层耐摩性进行测定，由图5可知，该浓度梯度下所得复合涂层的耐磨性随镀液中WS2粒子浓度增加呈先增加后降低的趋势，当镀液中WS2粒子浓度为4.0g/L时，所得复合涂层呈现最优异的耐磨性。
由以上实例，实现了通过控制Ni-P-WS2-PTFE镀液中WS2的浓度，最终获得WS2含量不同的Ni-P-WS2-PTFE复合涂层，通过对比不同WS2浓度掺杂对化学镀Ni-P-PTFE复合涂层的微观结构和力学性能的影响，明确了Ni-P-PTFE复合涂层的最优掺杂量为4.0g/L。在此掺杂量下制备的Ni-P-WS2-PTFE复合涂层结构致密，涂层硬度较高，且摩擦系数此时仍保持在较低水平，相对Ni-P-PTFE复合涂层其的耐磨性得到显著提升。
Claims (6)
1.一种手术电极用WS2掺杂Ni-P-PTFE医用复合涂层及其制备方法，其特征在于，所述复合涂层包括形成在基体上的Ni-P过渡层和Ni-P-WS2-PTFE表面层，所述基体为手术用电刀与双极电凝。
2.如权利要求1所述的WS2掺杂Ni-P-PTFE医用复合涂层，其特征在于，所述Ni-P过渡层和所述Ni-P-WS2-PTFE表面层分别通过化学镀工艺沉积而成。
3.如权利要求1-2之一所述的WS2掺杂Ni-P-PTFE医用复合涂层的制备方法，其特征在于，包括如下步骤：
1)将基体放入丙酮中，采用超声波清洗；
2)采用化学法对基体进行除油，然后再利用盐酸溶液进行酸洗活化；
3)通过化学镀在基体上镀一层Ni-P，作为过渡层；
4)通过化学镀在Ni-P层上镀Ni-P-WS2-PTFE层。
4.如权利要求3所述的WS2掺杂Ni-P-PTFE医用复合涂层的制备方法，其特征在于：步骤1)中，采用丙酮对基体表面进行超声波清洗；即将基体放入含有丙酮溶液的容器中，浸没，再将容器放置于超声波清洗仪中，功率设置为90W，时间设置为30min，对基材有机除油，获得洁净的基体表面。
5.如权利要求3所述的WS2掺杂Ni-P-PTFE医用复合涂层的制备方法，其特征在于：步骤2)中，化学除油所需的溶液中含有NaOH、Na2CO3、Na3PO4，在所述的溶液中，NaOH的浓度为20g/L，Na2CO3的浓度为30g/L，Na3PO4的浓度为30g/L，溶液加热到70-80℃，然后将基体加入到除油溶液中，除油时间为10-15min，从而使得基体表面的油污被除尽。
6.如权利要求3所述的WS2掺杂Ni-P-PTFE医用复合涂层的制备方法，其特征在于：步骤2)中，盐酸溶液的体积分数为40-60％，将经过除油的基体浸泡盐酸溶液中进行酸洗活化，溶液温度为常温，浸泡时间为3-5min，使得基体表面的氧化层被除去，得到完全暴露的基材。
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