CN114892143A - 一种细长不锈钢管内壁沉积纳米SiC涂层的方法及装置 - Google Patents
一种细长不锈钢管内壁沉积纳米SiC涂层的方法及装置 Download PDFInfo
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Abstract
一种细长不锈钢管内壁沉积纳米SiC涂层的方法,属于涂层制备技术领域。所述方法为:基于螺旋波等离子体源,先向真空室内通入Ar对细长不锈钢管进行离子轰击,清洗掉表面杂质,然后向真空室内充入Ar和Si(CH3)4的混合气体,该混合气体在螺旋波源作用下被激发电离,在不锈钢管内产生等离子体密度大于1019m‑3的高密度等离子体柱,然后在工件上施加脉冲负偏压,在其内表面沉积纳米SiC薄膜。本发明操作简单、方便、容易实现、易于工业化生产,可以在不需要加热的条件下或者保证不锈钢细长管基体在处理过程中不变形的前提下,制备与基体结合力强、硬度高、耐磨损的SiC涂层的方法,其提高了在恶劣环境下工作的不锈钢细长管的使用寿命。
Description
技术领域
本发明属于涂层制备技术领域,具体涉及一种细长不锈钢管内壁沉积纳米SiC涂层的方法及装置。
背景技术
纳米碳化硅(nano-SiC)涂层由于其具有高硬度、耐腐蚀、耐氧化等优异的性能,在保护涂层领域有着广泛的应用,如切削刀具、热敏打印头等,可以通过纳米SiC涂层增加其使用寿命。SiC涂层可以通过物理气相沉积法(PVD)、化学气相沉积法(CVD)以及等离子体增强化学气相沉积法(PECVD)合成。PECVD具有实验条件简单,制备的膜层纯度高、致密性好、附着力高等优点,是目前SiC涂层的主要制备方式。但是在早期PECVD制备SiC涂层时,使用的SiH4和C2H2混合气体极易爆炸造成危险。而有机硅烷具有良好的稳定性,目前通常采用Si(CH3)4作为PECVD合成SiC涂层的前驱体。然而,这种方法的问题在于处理过程中基板的温度相对较高,通常在500℃以上,这会引起基板组成和结构上的变化。另外,SiC涂层和基板材料也会由于不同的热膨胀系数在膜基结合处产生应力,最终引起缺陷。
对于大长径比的细长管来说,如核燃料包壳等,采用等离子体的手段对其内表面进行改性一直以来都是一项重大的挑战。细长管内表面等离子体沉积的SiC涂层通常性能较差,与基体结合力不强,所以在细长管内表面沉积SiC涂层的技术还有待改进。
发明内容
本发明的目的是为了解决细长管内SiC涂层与基体结合不牢固的问题,提供一种细长不锈钢管内壁沉积纳米SiC涂层的方法及装置。
为实现上述目的,本发明采取的技术方案如下:
一种细长不锈钢管内壁沉积纳米SiC涂层的方法,所述方法为:基于螺旋波等离子体源,先向真空室内通入Ar对细长不锈钢管进行离子轰击,清洗掉表面杂质,然后向真空室内充入Ar和Si(CH3)4的混合气体,该混合气体在螺旋波源作用下被激发电离,在不锈钢管内产生等离子体密度大于1019m-3的高密度等离子体柱,然后在工件上施加脉冲负偏压,在其内表面沉积纳米SiC薄膜。
进一步地,所述细长不锈钢管的长径比为50~100:1。
进一步地,所述离子轰击具体为:对其进行Ar+轰击处理,处理时真空室内的压力为1×10-2Pa,射频电源的功率为3.5kW,在不锈钢管上施加直流负偏压-Vc=200V,磁场强度为2000Gs,Ar的流量为50sccm,轰击处理时间为15min。
进一步地,所述混合气体中,Ar作为载体气体,流量为30sccm,Si(CH3)4的流量为50sccm。
进一步地,所述负偏压的范围为0V~-600V,可以在不同偏压幅值下实现细长不锈钢管内表面SiC涂层的沉积。
进一步地,所述负偏压的范围为-400V,沉积的SiC涂层的性能是最优异。
进一步地,沉积SiC涂层时,真空室内的真空度为0.1Pa,射频电源的功率为3.5Kw,磁场强度为2000Gs,沉积SiC涂层时采用脉冲偏压,幅值为-V=400V,频率10kHz,占空比20%,沉积时间10min。
一种上述细长不锈钢管内壁沉积纳米SiC涂层所使用的装置,所述装置包括螺旋波半波长水冷天线、磁体、不锈钢管、分子泵、真空室、OES诊断系统、朗缪尔探针和脉冲电压源;
所述磁体位于真空室外,用于产生稳态的轴向磁场;
所述螺旋波半波长水冷天线位于真空室的等离子体源区域,不锈钢管位于真空室的加工区,真空室的末端设有OES诊断系统和朗缪尔探针,用于诊断处理过程中的等离子体参数,所述分子泵用于为真空室提供真空环境,所述脉冲电压源为不锈钢管施加脉冲负偏压。
本发明相对于现有技术的有益效果为:本发明是一种基于螺旋波等离子体的增强化学气相沉积方法(HWP-PECVD),操作简单、方便、容易实现、易于工业化生产,可以在不需要加热的条件下或者保证不锈钢细长管基体在处理过程中不变形的前提下,制备与基体结合力强(约为14MPa)、硬度高(36.8GPa)、耐磨损的SiC涂层的方法,其提高了在恶劣环境(如核包壳和化工管道等)下工作的不锈钢细长管的使用寿命。
附图说明
图1为316L不锈钢细长管螺旋波等离子体PECVD沉积SiC装置示意图;
图2为脉冲偏压为-400V时316L不锈钢管内表面沉积SiC涂层横截面扫描电镜图;
图3为不同脉冲偏压幅值下316L不锈钢管内表面沉积SiC涂层的沉积速率;
图4为脉冲偏压为-400V时316L不锈钢管内表面沉积SiC涂层原子力显微镜图;
图5为不同脉冲偏压幅值下316L不锈钢管内表面SiC涂层的XRD图;
图6为不同脉冲偏压幅值下316L不锈钢管内表面SiC涂层的硬度。
具体实施方式
下面结合附图和实施例对本发明的技术方案作进一步的说明,但并不局限于此,凡是对本发明技术方案进行修正或等同替换,而不脱离本发明技术方案的精神范围,均应涵盖在本发明的保护范围之中。
实施例1:
本实施例在内径10mm,长500mm的316L不锈钢管内表面沉积了28.2μm厚的SiC涂层,对其表面以及横截面的微观形貌采用SEM和AFM进行了表征,如图2和图4所示。其具体的实施方案如下:
本实施例所用的装置为发明人自研,其组成部分之间的位置及连接关系如图1所示,主要部分为真空室5内等离子体源区域的一个螺旋波半波长水冷天线1,模式为m=+1,以及放置在真空室外的磁体2。天线上施加有13.5MHz的射频电源。天线通过耦合外部电源的功率以激发螺旋波;真空室外的磁体用于产生稳态的轴向磁场。不锈钢管3通过支撑平台固定在真空室的加工区,等离子体诊断区用于诊断处理过程中的等离子体参数,包括一个朗缪尔探针7和OES诊断系统6。朗缪尔探针通过密封法兰固定在真空室腔体上,其工作部分位于不锈钢管端口处。在进行放电之前,需要通过分子泵4将真空室内的真空度抽至1.0×10-5Pa,通过脉冲电压源8在不锈钢管工件上施加不同幅值的脉冲负偏压实现SiC涂层的沉积。
在对316L不锈钢管进行处理之前,需要对其进行Ar+轰击处理,处理时真空室内的压力为1×10-2Pa,射频电源的功率为3.5kW,在不锈钢管上施加直流负偏压-Vc=200V,磁场强度为2000Gs,Ar的流量为50sccm,轰击处理时间为15min。
在进行管内沉积SiC涂层时,仍然以前述的Ar流量,即50sccm,向真空室内充气,以维持放电。同时通过质量流量计向真空室内通入Ar和Si(CH3)4的混合气体。此处的Ar作为载体气体,流量为30sccm,Si(CH3)4的流量为50sccm。真空室内的真空度为0.1Pa,射频电源的功率为3.5Kw,磁场强度为2000Gs。沉积SiC涂层时采用脉冲偏压,幅值为-V=400V,频率10kHz,占空比20%,沉积时间10min。
在整个处理过程中,细长不锈钢管的温度不会超过150℃,最大程度上避免了高温带来的形变和相变。
本发明基于不同的脉冲偏压幅值,在直径10mm,长500mm的316L不锈钢管内表面沉积了SiC涂层。在400V的脉冲偏压幅值下,试样的截面扫描电镜和表面扫描电镜结果(图2)显示涂层均匀且致密,与基体之间的界面没有缝隙和缺陷,不同脉冲偏压幅值对应的SiC涂层的沉积速率如图3所示。在400V的脉冲偏压幅值下沉积的SiC涂层的原子力显微镜结果(图4)显示,涂层表面具有良好的均匀性和表面平整度,这也与扫描电镜的结果相一致。由试样的XRD结果(图5)可以看出,在2θ为36.5°处显著的显示出3C-SiC(111)峰,表明涂层的成分确实为SiC。另外由Rietveld细化方法计算可以得到SiC涂层的纳米晶粒的平均尺寸为11.81nm,这也是涂层具有高硬度的主要原因之一。采用维氏压头的纳米压痕测试仪对SiC涂层的机械硬度进行测试,结果如图6所示,其中脉冲偏压幅值为400V时SiC涂层的硬度为36.8GPa,是316L不锈钢基体硬度的19倍,具有优良的机械性能。
实施例2:
本实施例与实施例1不同的是,沉积SiC涂层时脉冲偏压幅值为-V=200V,结果为在内径10mm,长500mm的316L不锈钢管内表面沉积了厚度为21.3μm的SiC涂层。相对实施例1,较小的脉冲偏压幅值时SiC涂层的沉积速率有所下降的根本原因。
实施例3:
本实施例与实施例1不同的是,沉积SiC涂层时脉冲偏压幅值为-V=600V,结果为在内径10mm,长500mm的316L不锈钢管内表面沉积了厚度为3.54μm的SiC涂层。相对实施例1和实施例2,SiC涂层的沉积速率在较大的脉冲偏压幅值条件下有所下降的原因是发生了刻蚀。
Claims (8)
1.一种细长不锈钢管内壁沉积纳米SiC涂层的方法,其特征在于:所述方法为:基于螺旋波等离子体源,先向真空室内通入Ar对细长不锈钢管进行离子轰击,清洗掉表面杂质,然后向真空室内充入Ar和Si(CH3)4的混合气体,该混合气体在螺旋波源作用下被激发电离,在不锈钢管内产生等离子体密度大于1019m-3的高密度等离子体柱,然后在工件上施加脉冲负偏压,在其内表面沉积纳米SiC薄膜。
2.根据权利要求1所述的一种细长不锈钢管内壁沉积纳米SiC涂层的方法,其特征在于:所述细长不锈钢管的长径比为50~100:1。
3.根据权利要求1所述的一种细长不锈钢管内壁沉积纳米SiC涂层的方法,其特征在于:所述离子轰击具体为:对其进行Ar+轰击处理,处理时真空室内的压力为1×10-2Pa,射频电源的功率为3.5kW,在不锈钢管上施加直流负偏压-Vc=200V,磁场强度为2000Gs,Ar的流量为50sccm,轰击处理时间为15min。
4.根据权利要求1所述的一种细长不锈钢管内壁沉积纳米SiC涂层的方法,其特征在于:所述混合气体中,Ar作为载体气体,流量为30sccm,Si(CH3)4的流量为50sccm。
5.根据权利要求1所述的一种细长不锈钢管内壁沉积纳米SiC涂层的方法,其特征在于:所述负偏压的范围为0V~-600V。
6.根据权利要求5所述的一种细长不锈钢管内壁沉积纳米SiC涂层的方法,其特征在于:所述负偏压的范围为-400V。
7.根据权利要求1所述的一种细长不锈钢管内壁沉积纳米SiC涂层的方法,其特征在于:沉积SiC涂层时,真空室内的真空度为0.1Pa,射频电源的功率为3.5Kw,磁场强度为2000Gs,沉积SiC涂层时采用脉冲偏压,幅值为-V=400V,频率10kHz,占空比20%,沉积时间10min。
8.一种权利要求1~7任一项细长不锈钢管内壁沉积纳米SiC涂层所使用的装置,其特征在于:所述装置包括螺旋波半波长水冷天线、磁体、不锈钢管、分子泵、真空室、OES诊断系统、朗缪尔探针和脉冲电压源;
所述磁体位于真空室外,用于产生稳态的轴向磁场;
所述螺旋波半波长水冷天线位于真空室的等离子体源区域,不锈钢管位于真空室的加工区,真空室的末端设有OES诊断系统和朗缪尔探针,用于诊断处理过程中的等离子体参数,所述分子泵用于为真空室提供真空环境,所述脉冲电压源为不锈钢管施加脉冲负偏压。
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