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Article(id=1210577664499380245, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210577662121209865, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2024.08.008, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1692720000000, receivedDateStr=2023-08-23, revisedDate=1699891200000, revisedDateStr=2023-11-14, acceptedDate=null, acceptedDateStr=null, onlineDate=1766553806662, onlineDateStr=2025-12-24, pubDate=1724083200000, pubDateStr=2024-08-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1766553806662, onlineIssueDateStr=2025-12-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1766553806662, creator=13701087609, updateTime=1766553806662, updator=13701087609, issue=Issue{id=1210577662121209865, tenantId=1146029695717560320, journalId=1149653034449285133, year='2024', volume='57', issue='8', pageStart='1', pageEnd='147', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1766553806095, creator=13701087609, updateTime=1766563971278, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1210620298043454173, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210577662121209865, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1210620298043454174, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1210577662121209865, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=66, endPage=72, ext={EN=ArticleExt(id=1210577664851701790, articleId=1210577664499380245, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Investigation on effect of low temperature plasma jet treatment on performance of silicone rubber material, columnId=1190369198472794288, journalTitle=Insulating Materials, columnName=Insulation Technology, runingTitle=null, highlight=null, articleAbstract=

In order to solve the problem of printing contamination on the surface of silicone rubber cables, the application of low temperature plasma jet in surface treatment of silicone rubber was proposed in this paper. Ar plasma jet was generated with needle-ring structure electrode driven by AC power source, and the surface of silicone rubber cables was dynamically treated at different moving speeds. The influence of processing speed on the hydrophobicity, surface voltage, and breakdown strength of silicone rubber cable was systematically studied. The changes in surface physical morphology and chemical composition of silicone rubber were detected by SEM and EDS. The results show that static jet treatment can cause an increase of the material surface temperature, while dynamic treatment can significantly reduce the temperature rise. The water contact angle and flashover voltage of silicone rubber slightly decrease after treatment. With the increase of processing speeds, the hydrophobic and electrical insulation performance gradually recover. Under the speed of 5 mm/s, the anti-ink adhesion of silicone rubber surface is significantly improved. It can be concluded that the degree of cross-linking polymerization on the surface of silicone rubber increases after the plasma jet treatment, and the diffusion movement of interface molecules at the interface is hindered, which decrease the anti-ink adhesion of the silicone rubber surface.

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为解决硅橡胶电缆表面印字污染问题，本文提出利用低温等离子体射流对硅橡胶进行表面处理。以交流电源激励针-环结构电极产生氩气等离子体射流，对不同移动速度下的硅橡胶电缆表面进行动态处理，系统研究处理速度对硅橡胶电缆憎水性、沿面耐压和击穿性能的影响，通过SEM和EDS检测硅橡胶表面物理形貌和化学成分变化。结果表明：射流静态处理会导致材料表面温度升高，而动态处理可以显著降低温升。处理后硅橡胶的水接触角和闪络电压均有小幅度下降。随着处理速度增大，硅橡胶的憎水性和电气绝缘性能逐渐恢复。5 mm/s处理条件下，硅橡胶表面抗油墨粘接性显著提高。结合物化特性结果可知，等离子体射流处理后硅橡胶表面交联聚合程度提高，界面分子扩散运动受到阻碍，进而降低了硅橡胶表面自黏性能。

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伍雪峰（1972-），男（汉族），江苏九江人，高级工程师，主要从事电力系统方面的研究。

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伍雪峰（1972-），男（汉族），江苏九江人，高级工程师，主要从事电力系统方面的研究。

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伍雪峰（1972-），男（汉族），江苏九江人，高级工程师，主要从事电力系统方面的研究。

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元素种类处理条件
面扫未处理面扫处理后点测白点处点测无白点
C20242722
O28273630
Si52493749
), ArticleFig(id=1218111685752176662, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1210577664499380245, language=CN, label=表1, caption=

等离子体射流处理前后硅橡胶表面的C、O、Si三元素含量变化

, figureFileSmall=null, figureFileBig=null, tableContent=
元素种类处理条件
面扫未处理面扫处理后点测白点处点测无白点
C20242722
O28273630
Si52493749
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低温等离子体射流处理对硅橡胶材料性能的影响研究
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伍雪峰 , 段家振 , 史如新 , 刘洪涛 , 何轶聪 , 任显铭
绝缘材料 | 绝缘技术 2024,57(8): 66-72
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绝缘材料 | 绝缘技术 2024, 57(8): 66-72
低温等离子体射流处理对硅橡胶材料性能的影响研究
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伍雪峰, 段家振, 史如新, 刘洪涛, 何轶聪, 任显铭
作者信息
  • 国家电网常州供电公司，江苏 常州 213004

    • 伍雪峰（1972-），男（汉族），江苏九江人，高级工程师，主要从事电力系统方面的研究。

Investigation on effect of low temperature plasma jet treatment on performance of silicone rubber material
Xuefeng WU, Jiazhen DUAN, Ruxin SHI, Hongtao LIU, Yicong HE, Xianming REN
Affiliations
  • State Grid Changzhou Power Supply Company, Changzhou 213004, China
出版时间: 2024-08-20 doi: 10.16790/j.cnki.1009-9239.im.2024.08.008
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摘要
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为解决硅橡胶电缆表面印字污染问题，本文提出利用低温等离子体射流对硅橡胶进行表面处理。以交流电源激励针-环结构电极产生氩气等离子体射流，对不同移动速度下的硅橡胶电缆表面进行动态处理，系统研究处理速度对硅橡胶电缆憎水性、沿面耐压和击穿性能的影响，通过SEM和EDS检测硅橡胶表面物理形貌和化学成分变化。结果表明：射流静态处理会导致材料表面温度升高，而动态处理可以显著降低温升。处理后硅橡胶的水接触角和闪络电压均有小幅度下降。随着处理速度增大，硅橡胶的憎水性和电气绝缘性能逐渐恢复。5 mm/s处理条件下，硅橡胶表面抗油墨粘接性显著提高。结合物化特性结果可知，等离子体射流处理后硅橡胶表面交联聚合程度提高，界面分子扩散运动受到阻碍，进而降低了硅橡胶表面自黏性能。

低温等离子体射流  /  表面改性  /  硅橡胶电缆

In order to solve the problem of printing contamination on the surface of silicone rubber cables, the application of low temperature plasma jet in surface treatment of silicone rubber was proposed in this paper. Ar plasma jet was generated with needle-ring structure electrode driven by AC power source, and the surface of silicone rubber cables was dynamically treated at different moving speeds. The influence of processing speed on the hydrophobicity, surface voltage, and breakdown strength of silicone rubber cable was systematically studied. The changes in surface physical morphology and chemical composition of silicone rubber were detected by SEM and EDS. The results show that static jet treatment can cause an increase of the material surface temperature, while dynamic treatment can significantly reduce the temperature rise. The water contact angle and flashover voltage of silicone rubber slightly decrease after treatment. With the increase of processing speeds, the hydrophobic and electrical insulation performance gradually recover. Under the speed of 5 mm/s, the anti-ink adhesion of silicone rubber surface is significantly improved. It can be concluded that the degree of cross-linking polymerization on the surface of silicone rubber increases after the plasma jet treatment, and the diffusion movement of interface molecules at the interface is hindered, which decrease the anti-ink adhesion of the silicone rubber surface.

low temperature plasma jet  /  surface modification  /  silicon rubber cable
伍雪峰, 段家振, 史如新, 刘洪涛, 何轶聪, 任显铭. 低温等离子体射流处理对硅橡胶材料性能的影响研究. 绝缘材料, 2024 , 57 (8) : 66 -72 . DOI: 10.16790/j.cnki.1009-9239.im.2024.08.008
Xuefeng WU, Jiazhen DUAN, Ruxin SHI, Hongtao LIU, Yicong HE, Xianming REN. Investigation on effect of low temperature plasma jet treatment on performance of silicone rubber material[J]. Insulating Materials, 2024 , 57 (8) : 66 -72 . DOI: 10.16790/j.cnki.1009-9239.im.2024.08.008
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0 引言
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硅橡胶因其良好的耐候性和绝缘性，常被用于电缆的制备[1-4]。由于电缆应用场景的多样性，通常需要通过表面处理以调节其表面性能。例如，为了便于区分型号和生产商，需要在电缆表面印刷文字，但由于硅橡胶本身具有自黏性，在堆积收卷存储的过程中会与接触的硅橡胶表面互相粘结，进而在表面形成污渍，既影响辨识电缆信息，又会对电缆绝缘性能造成影响[5-6]。目前，解决硅橡胶材料表面性能问题的方法主要有化学法和物理法，其中化学法主要通过引入功能基团对硅橡胶表面进行修饰[6]，但该方法存在工艺复杂、产生挥发性有机物等问题；物理法主要通过清洗、喷涂等方式改变表面特性，但在处理效率和时效性等方面仍存在问题。
低温等离子表面改性技术因其处理条件简单、能耗低、效率高、无污染等优点受到人们的广泛关注[7]。近年来，国内外利用低温等离子体技术对绝缘材料进行表面处理以提高表面性能的研究已经取得了一些进展。如LI S等[8]以He为工作气体驱动等离子体射流阵列，对污染后的硅橡胶样片进行处理，可提高其表面疏水性能；GUAN H L等[9]利用等离子体技术进行硅橡胶表面处理，并通过控制等离子体处理时间，提高了硅橡胶在常压空气下的直流闪络电压；K KRAWCZYK等[10]通过等离子体技术改善硅橡胶表面的亲水性。综合现有研究发现，利用等离子体技术能够提高硅橡胶表面的不同性能，但处理过程中材料表面的物理形貌和化学成分会发生变化，其润湿性、沿面耐压和电气强度均会随之改变。此外，现有硅橡胶改性研究大都固定等离子体与硅橡胶的相对位置，而实际应用中等离子体处理作为电缆加工工艺环节之一，通常将等离子体源固定，电缆处于连续运动状态。因此，需要系统研究在动态处理过程中，等离子体对硅橡胶的润湿性、油墨粘接性、沿面耐压和电气强度等综合性能的影响规律。
目前，低温等离子体表面处理应用中，主要有介质阻挡放电和大气压等离子体射流两种方式。其中，大气压等离子体射流由于其产生位置与改性区域的空间分离，适合于电缆表面处理[11-12]。因此，本文利用交流电源激励氩气放电产生低温等离子体射流，对硅橡胶表面进行改性处理，并研究不同处理速度条件下硅橡胶综合性能的变化规律，为等离子体射流在硅橡胶电缆表面改性应用提供实验依据。
1 实验系统及研究方法
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1.1 等离子体射流处理硅橡胶实验系统
本研究搭建的实验系统如图1所示。等离子体射流电极采用针-环结构，由石英管（内径为2 mm，外径为4 mm，长度为180 mm）、高压电极和地电极组成。其中高压电极为一根空心钢管（外径为1.5 mm，内径为0.8 mm），顶端距石英管口40 mm。地电极为10 mm宽的铜箔，其下端距石英管口10 mm。工作气体采用99.999%高纯度氩气，流速为 1 L/min，使用交流电源激励产生等离子体。放电电压和电流分别由高压探头（Tektronix P6139A型）和电流线圈（Pearson 4100型）测得，通过示波器（Tektronix TDS-3054c型）进行数据采集。采用光纤光谱仪（Ocean Optics HR4000CG型）测量发射光谱，探头距离射流体羽30 mm。放电图像采用Cannon相机进行拍摄，曝光时间为1/4 s。
1.2 硅橡胶试样处理
实验用硅橡胶购自中天电缆科技有限公司，样片尺寸为10 mm×10 mm，厚度为1 mm。为了保证射流放电的稳定性并实现良好的改性效果，通过前期实验，确定电源电压为9 kV，频率为5 kHz，处理距离为10 mm。考虑电缆生产加工过程的在线处理需求，采用动态方式进行硅橡胶表面改性：固定射流反应器，将硅橡胶样片置于水平位移平台，控制电机使其带动平台以恒定速度运动。硅橡胶材料作为电缆材料时，工作温度通常不超过80℃，过高的处理温度会产生显著的老化效应，甚至可能烧蚀硅橡胶。为考察等离子体处理对硅橡胶的热效应，使用FOTRIC型热成像仪检测硅橡胶的表面温度。
1.3 硅橡胶性能检测方法
改性前后表面憎水性的变化由水接触角测量仪（ZJ-CAZ2型）表征，实验时将1.5 μL蒸馏水滴在材料表面，每个样片测量3次取平均值。为考察硅橡胶表面抗油墨粘接性，将带有印字的硅橡胶用射流进行处理，处理后使用10 kg砝码将其与无印字未处理样片挤压以模拟电缆堆积收卷，静置24 h后观察表面是否发生印字渗透。采用Oxford Ultim Max 65型扫描电子显微镜（SEM），与其配备的X射线能谱仪（EDS）结合，检测处理前后的硅橡胶表面物化特性。通过傅里叶红外光谱仪（FTIR，Thermo Scientific Nicolet iS 50型）分析样品的化学成分。为考察等离子体处理对硅橡胶绝缘性能影响，分别对处理前后的闪络电压、表面电荷消散过程和电气强度进行测量。采用高压直流电源激励测量闪络电压，在指型电极两端施加电压，以0.5 kV/s的速度调高输出电压，直到发生闪络。利用表面电荷测试系统进行正极性电晕充电，记录表面电荷衰减过程[13-16]。测试条件：充电电压为3 kV，针尖与样品上表面垂直间距为5 mm，在充电5 min后迅速将样品移动至Kelvin静电探头（Trek-6000B型）下进行测试，探头距样品上表面2 mm。采用球-球电极测试样品电气强度，以0.5 kV/s的速度升压，直到发生击穿，将击穿电压除以样品厚度获得电气强度。每个样品测试8次，采用双参数威布尔模型分析。
2 放电特性诊断结果
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图2给出了硅橡胶等离子体射流放电特性诊断结果。其中图2(a)为电学特性结果，从图2(a)可以看出，正、负半周期的放电均产生了多个电流脉冲，说明介质管内放电模式为丝状放电。放电脉冲电流峰值平均约50 mA，且正、负半周呈现显著的不对称性，这是由针环电极结构形成的非对称电场导致[17]。图2(b)为光学特性结果，由图2(b)中的发光图像可见，射流体羽呈暗紫色，长度约为11 mm。体羽由管口向周围空气延伸过程中逐渐收缩，这是由于放电产生的高能粒子在传输过程中不断发生碰撞、解离等反应，粒子能量逐渐衰减[18]。根据发射光谱测试结果，等离子体中含有丰富的Ar激发态粒子，这是由于该放电以Ar作为工作气体，Ar原子与自由电子碰撞频率高，致使其光谱强度最高[19-20]。高能电子、激发态Ar与空气中氮气分子发生非弹性碰撞，引发电离和激发反应，生成大量化学活性粒子及自由基，根据图2(b)中光谱检测结果可知，生成的粒子主要为N2(C3Пu→B3Пg)。此外，光谱中检测到OH自由基，这是空气中微量的水参与反应所致[19]。
不同状态条件下，射流体羽作用在硅橡胶表面导致其温度变化的结果如图3所示。Ar1为硅橡胶表面的温度，Ar2为等离子体反应器的温度。从图3(a)可以看出，在静态条件下，随着处理时间的增加，硅橡胶表面温度显著增加。在处理60 s时，最高温度由原来的27.9℃（图3(b)）达到78.6℃（图3(c)），接近硅橡胶表面最高工作温度。因此，在静态条件下，采用射流处理时间应控制在60 s以内。在动态条件下（样品移动速度为1 mm/s），随着处理时间增加，硅橡胶表面温度缓慢增加随之趋于稳定，稳定温度在33～34℃。该结果表明，动态处理能够显著降低等离子体处理过程中硅橡胶的表面温升。
3 改性效果
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3.1 表面水接触角
等离子体射流处理前后硅橡胶的表面水接触角测量结果如图4所示。从图4可以看出，未处理的硅橡胶水接触角为113°。当样品移动速度为 1 mm/s时，射流处理后表面水接触角为94.1°，相较于未处理时降低了16.7%。随着移动速度增加，表面水接触角逐渐增大，当样品移动速度为5 mm/s时，水接触角为107.2°，相较于未处理时降低5.1%。由此说明，射流处理会导致硅橡胶表面憎水性变差，这是由于等离子体射流产生的高能粒子轰击硅橡胶表面，会改变材料表面分子的化学结构。结合图7的FTIR检测结果，处理后非极性基团Si-CH3减少，因此憎水性降低。虽然硅橡胶表面水接触角相较于未处理时有所降低，但在高速处理下水接触角仍可达到107°，呈现出较好的憎水性能。此外，提高处理速度能够有效抑制憎水性的降低，为了保证硅橡胶电缆的憎水性，应该在满足处理要求的前提下，增大处理速度。
3.2 表面抗油墨粘接性能
图5所示为射流处理前后硅橡胶表面抗油墨粘接性能测试结果，样品移动速度为5 mm/s。根据图5(a)可知，未处理的硅橡胶表面经过重物压24 h后，其油墨印已经染到与之接触的硅橡胶上，形成白色印字痕迹。经过等离子体射流处理后，如图5(b)所示，硅橡胶的印染问题得到解决，硅橡胶表面无明显印字痕迹，原始印字硅橡胶无字迹损失。
3.3 表面物理形貌和化学成分
图6给出了等离子体射流处理前后硅橡胶表面SEM图像，表1为对应的EDS检测结果。由图6(a)可知，未经处理的硅橡胶表面整体平整，表面纹路分布均匀，为硅橡胶制作过程中所留下的痕迹，长度为1～2 μm[21-22]。由图6(b)可见，处理后硅橡胶表面出现白色斑点。根据表1所示的EDS检测结果，未处理硅橡胶表面主要包含Si、O、C三种元素，含量比约为5∶3∶2。射流处理后表面形成的斑点位置的Si含量较其他位置低12%，而O和C的含量均有所上升。等离子体射流处理前后硅橡胶表面的FTIR检测结果如图7所示。由图7可见，处理前后的表面化学基团种类没有变化，这与EDS检测结果具有一致性。上述表面物化特性检测的结果表明，等离子体处理硅橡胶并未在其表面引入新的化学基团，但会提升主链的交联程度，硅橡胶界面分子链段扩散运动受到阻碍，进而降低了硅橡胶表面自黏性能。
3.4 电气性能
图8所示为不同样品移动速度下射流处理后的硅橡胶电气性能测试结果。图8(a)为闪络电压测试结果，根据图8(a)所示，未处理硅橡胶表面闪络电压为8.8 kV。在1 mm/s速度处理下，闪络电压降低至7.4 kV，较未处理时减少15.9%；当处理速度达到4 mm/s时，闪络电压升高到9.1 kV，较未处理时提高3.4%。结果表明，低速处理会导致沿面耐压性能下降，当速度增加到4～5 mm/s时，其处理后的沿面耐压性能可达到未处理水平，甚至略有增加。图8(b)所示为不同样品移动速度下射流处理后硅橡胶的表面电荷消散过程曲线。由图8(b)可见，随着速度的增加，电荷消散速率变快，但相仍比未处理时的慢。当速度增加到4～5 mm/s时，处理后的硅橡胶
可达到原始硅橡胶电荷消散速率，并且当速度为 4 mm/s时，处理后电荷消散速率高于未处理试样的速率，这与沿面耐压性能测试结果具有一致性。由图8(b)计算得到的陷阱电荷密度结果如图8(c)所示。从图8(c)可以看出，在1 mm/s处理条件下，硅橡胶表面陷阱能级升高到0.963 eV，说明处理后硅橡胶表面束缚电子能力增强，易发生表面电荷积聚、表面电场畸变增强、沿面耐压降低。随着处理速度的增加，陷阱能级逐渐变浅。当处理速度为 4 mm/s时，其陷阱能级由未处理时的0.947 eV降低到0.907 eV。更浅的陷阱使得载流子更容易沿着表面去深陷阱化，加速电荷消散，减弱表面电场畸变，提升闪络电压。图8(d)为5 mm/s处理速度下硅橡胶电气强度的测试结果。由图8(d)可知，未处理硅橡胶的电气强度为34.6 kV/mm，射流处理后的硅橡胶电气强度为35.0 kV/mm，与未处理时相差不大，说明高速处理条件下，射流表面处理基本不会影响硅橡胶本体绝缘性能。
4 结论
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（1）在静态处理条件下，等离子体射流处理硅橡胶会导致其温度升高，且随处理时间增加温升增大，静态射流处理1 min时最高温度达到78.6℃，接近硅橡胶耐受温度。在样品移动速度为1 mm/s的动态条件下，硅橡胶表面温度可稳定温度在33～34℃。因此，在实际应用中，需要采用动态处理方法以降低等离子体处理过程中硅橡胶的表面温升。
（2）在5 mm/s动态处理条件下，硅橡胶表面形成Si元素含量较低的白点并且表面交联聚合程度提高，使得抗油墨粘接性能提升，有效解决了硅橡胶电缆印字污染问题。
（3）在低速处理条件下，硅橡胶憎水性以及沿面耐压性能均有所下降，在1 mm/s射流处理后，水接触角降低16.7%，闪络电压降低15.9%。随着处理速度增加，两者的下降程度减弱。当速度升高至5 mm/s时，水接触角较未处理时仅降低了5.1%，沿面耐压和电气强度基本可达到未处理水平。因此，利用射流进行硅橡胶表面改性，需要适当提高处理速度以保证憎水性和绝缘性。
基金
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  • 国网江苏省电力有限公司科技项目(J2022079)
文献
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2024年第57卷第8期
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doi: 10.16790/j.cnki.1009-9239.im.2024.08.008
  • 接收时间：2023-08-23
  • 首发时间：2025-12-24
  • 出版时间：2024-08-20
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  • 收稿日期：2023-08-23
  • 修回日期：2023-11-14
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国网江苏省电力有限公司科技项目(J2022079)
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    国家电网常州供电公司，江苏 常州 213004
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2种不同金属材料的力学参数
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
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红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
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