CN113416937B - 直流磁控溅射法制备银、石墨/聚四氟乙烯复合电磁屏蔽膜层的方法 - Google Patents
直流磁控溅射法制备银、石墨/聚四氟乙烯复合电磁屏蔽膜层的方法 Download PDFInfo
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Abstract
本申请涉及一种直流磁控溅射法制备银、石墨/聚四氟乙烯复合电磁屏蔽膜层的方法。将Ag颗粒和石墨粉末分散至PTFE中使得靶材具备导电性能,能够应用于直流溅射方法制备,避免了传统绝缘靶材采用射频溅射带来的成膜效率低、设备复杂等缺点。制备得到PTFE膜层能够降低铝蒙皮表面的表面能以达到疏水的目的,此外添加Ag粉末和石墨粉末后的PTFE靶材在溅射过程中Ag和石墨会在PTFE膜中形成Ag纳米颗粒和石墨纳米颗粒,纳米颗粒均匀分散在PTFE膜层中使得最终得到的PTFE表面呈现纳米级疏水结构,进一步提高疏水性能。石墨粉末与Ag粉末经过溅射后以纳米级颗粒的形式分散在PTFE膜层中,会对入射至膜层的电磁波产生反射次数,电磁屏蔽效能增强。
Description
技术领域
本申请涉及一种直流磁控溅射制备膜层的方法,具体为制备银、石墨/聚四氟乙烯复合电磁屏蔽膜层。
背景技术
随着应用环境要求的提高,不仅要求涂层具有耐腐蚀、超疏水等常规性能,同时要求能够保证电磁屏蔽效果,避免宇宙射线,卫星、电视、广播等外部电磁波信号对系统内部工作器件产生干扰或阻制内部的电磁信号泄露到系统外部,对造成信息的泄密。
超疏水涂层是指水接触角大于120°的涂层。已知固体表面与水的润湿性受两个主要因素的影响,即表面化学性质和表面形貌。近年来,使用物理气相沉积 (PVD) 来改性材料的表面性能得到了快速发展。通过PVD方法材料薄膜沉积在基板上。PVD技术中最有前途的技术之一是溅射,它已被广泛用于许多行业的各种材料的改性。
聚四氟乙烯是一种由碳和氟组成的高分子材料,具有很高的机械强度、热稳定性和化学稳定性,以及低介电常数的优良绝缘性能。聚四氟乙烯薄膜由于其优点,已在各个领域得到广泛研究,如窗户或显示器的防污涂层、疏水涂层等。
目前针对聚四氟乙烯的溅射方式以射频溅射为主,这是由于其绝缘性质导致其无法通过中频或直流方式溅射,这限制了聚四氟乙烯薄膜的应用推广。
发明内容
本申请提供一种直流磁控溅射法制备银、石墨/聚四氟乙烯复合电磁屏蔽膜层的方法。
针对铝蒙皮基底首先进行碱性清洗剂超声清洁,去除表面油污等杂质,超声清洗剂采用5%质量浓度的氢氧化钠溶液,超声处理时间5~30分钟;
随后对清洗后的铝蒙皮表面进行等离子体活化处理,活化处理过程在真空腔室中进行,炉内保持0.1~0.5Pa气压,待处理工件表面施加200~250V偏压,离子源电流0.3~0.5A,处理过程中通入高纯氩气产生等离子体,氩气流速10~25sccm,处理时间20~25min,通过等离子体活化处理进一步清洁铝蒙皮表面的同时,能够在基体表面产生活性自由基,能够为后续成膜提供表面能较高的接触面,提高后续成膜与基体的结合性能。
针对活化后的铝蒙皮进行直流溅射沉积Ag、石墨/PTFE复合电磁屏蔽膜层,具体沉积参数为直流偏压400~500V,腔室压力1×10-3~5×10-3Pa,Ar气气流30~50sccm,沉积时间1~3min,溅射采用Ag、石墨、PTFE复合靶材,靶材直径10cm。
具体的靶材制备方法为,将PTFE粉末于370~390℃加热至粘稠状,在搅拌下加入银粉末和石墨粉末,银粉末平均粒径为30~50微米,银粉末添加量占PTFE粉末质量的10~15%,石墨粉末平均粒径为10~15微米,石墨粉末添加量占PTFE粉末质量的10~15%,在持续加热保温下搅拌15~30min,保证银、石墨粉末在PTFE中均匀分散,随后转移至模具中加压排气冷却至室温。
将Ag颗粒和石墨粉末分散至PTFE中使得靶材具备导电性能,能够应用于直流溅射方法制备,避免了传统绝缘靶材采用射频溅射带来的成膜效率低、设备复杂等缺点。制备得到PTFE膜层能够降低铝蒙皮表面的表面能以达到疏水的目的,此外添加Ag粉末后的PTFE靶材在溅射过程中Ag会在PTFE膜中形成Ag纳米颗粒,Ag纳米颗粒均匀分散在PTFE膜层中使得最终得到的PTFE表面呈现纳米级疏水结构,进一步提高疏水性能。石墨粉末与Ag粉末经过溅射后以纳米级颗粒的形式分散在PTFE膜层中,其纳米效应能够引起能级分裂,对不同波长的电磁波均有较高的吸收作用,由于两种纳米颗粒均匀分散在膜层的厚度方向,会对入射至膜层的电磁波产生反射次数,对电磁波消耗增大,电磁屏蔽效能增强,由于二者纳米颗粒形貌存在差异,对电磁波反射更加不规则,能够进一步提高其对电磁波的反射作用。
具体实施方式
实施例1
针对铝蒙皮基底首先进行碱性清洗剂超声清洁,去除表面油污等杂质,超声清洗剂采用5%质量浓度的氢氧化钠溶液,超声处理时间20分钟;
随后对清洗后的铝蒙皮表面进行等离子体活化处理,活化处理过程在真空腔室中进行,炉内保持0.3Pa气压,待处理工件表面施加220V偏压,离子源电流0.4A,处理过程中通入高纯氩气产生等离子体,氩气流速20sccm,处理时间25min。
针对活化后的铝蒙皮进行直流溅射沉积Ag、石墨/PTFE复合电磁屏蔽膜层,具体沉积参数为直流偏压450V,腔室压力2×10-3Pa,Ar气气流40sccm,沉积时间2min,溅射采用Ag、石墨/PTFE复合靶材,靶材直径10cm。
具体的靶材制备方法为,将PTFE粉末于380℃加热至粘稠状,在搅拌下加入银粉末和石墨粉末,银粉末平均粒径为40微米,银粉末添加量占PTFE粉末质量的12%,石墨粉末平均粒径为15微米,石墨粉末添加量占PTFE粉末质量的13%,在持续加热保温下搅拌20min,随后转移至模具中加压排气冷却至室温。制备得到的涂层进行膜基结合强度和电磁屏蔽性能测试,还对接触角测试采用GB/T24368-2009测试标准进行。
实施例2-5
实施例2-5制备步骤与实施例1相同,具体参数参见表1。
接触角测试采用GB/T24368-2009测试标准进行,可见实施例1-5所获得的涂层接触角测试均大于150°,呈现出超疏水性能。制备得到的涂层进行膜基结合强度测试,实施例1-5结合力均大于30N。实施例1-5得到复合电磁屏蔽膜层在1~40GHz超宽频带的范围内,复合电磁屏蔽膜层的电磁屏蔽效果优于60dB。
表1.实施例1-5处理参数及测试结果
对比例1-4
对比例1-4制备步骤与实施例1相同,具体参数参见表2。对比例1-2在实施例1的基础上调整直流偏压,对比例3-4在实施例1的基础上调整Ar气气流,改变偏压电压及气流会影响靶材中掺杂的Ag粉末和石墨粉末溅射至衬底上的过程,导致最终Ag和石墨在PTFE膜层中的存在状态,若无法以Ag、石墨纳米颗粒的形成存在将无法导致纳米结构的形成,最终使接触角数值变低。在1~40GHz超宽频带的范围内,复合电磁屏蔽膜层的电磁屏蔽效果均低于40dB。
表2.对比例1-4处理参数及测试结果
对比例5
针对铝蒙皮基底首先进行碱性清洗剂超声清洁,去除表面油污等杂质,超声清洗剂采用5%质量浓度的氢氧化钠溶液,超声处理时间20分钟;
随后对清洗后的铝蒙皮表面进行等离子体活化处理,活化处理过程在真空腔室中进行,炉内保持0.3Pa气压,待处理工件表面施加220V偏压,离子源电流0.4A,处理过程中通入高纯氩气产生等离子体,氩气流速20sccm,处理时间25min。
针对活化后的铝蒙皮进行直流溅射沉积Ag、石墨/PTFE复合电磁屏蔽膜层,具体沉积参数为直流偏压450V,腔室压力2×10-3Pa,Ar气气流40sccm,沉积时间2min,溅射采用Ag、石墨/PTFE复合靶材,靶材直径10cm。
具体的靶材制备方法为,将PTFE粉末于380℃加热至粘稠状,在搅拌下加入银粉末,银粉末平均粒径为40微米,银粉末添加量占PTFE粉末质量的8%,石墨粉末平均粒径为15微米,石墨粉末添加量占PTFE粉末质量的8%,在持续加热保温下搅拌20min,随后转移至模具中加压排气冷却至室温。
由于银粉末及石墨粉末添加量较低,导致最终靶材导电性能不足,在直流磁控溅射过程中无法持续溅射成膜。
对比例6
针对铝蒙皮基底首先进行碱性清洗剂超声清洁,去除表面油污等杂质,超声清洗剂采用5%质量浓度的氢氧化钠溶液,超声处理时间20分钟;
随后对清洗后的铝蒙皮表面进行等离子体活化处理,活化处理过程在真空腔室中进行,炉内保持0.3Pa气压,待处理工件表面施加220V偏压,离子源电流0.4A,处理过程中通入高纯氩气产生等离子体,氩气流速20sccm,处理时间25min。
针对活化后的铝蒙皮进行直流溅射沉积Ag、石墨/PTFE复合电磁屏蔽膜层,具体沉积参数为直流偏压450V,腔室压力2×10-3Pa,Ar气气流40sccm,沉积时间2min,溅射采用Ag、石墨/PTFE复合靶材,靶材直径10cm。
具体的靶材制备方法为,将PTFE粉末于380℃加热至粘稠状,在搅拌下加入银粉末,银粉末平均粒径为40微米,银粉末添加量占PTFE粉末质量的18%,石墨粉末平均粒径为15微米,石墨粉末添加量占PTFE粉末质量的18%,在持续加热保温下搅拌20min,随后转移至模具中加压排气冷却至室温。
由于银粉末和石墨粉末添加量较高,导致最终溅射得到的PTFE膜层中Ag颗粒及石墨颗粒形成二次颗粒,颗粒尺寸较大,无法导致纳米结构的形成,最终使接触角数值为135°。此外由于颗粒较大使得导电性颗粒分布较集中,膜层导电性能不足,在1-40GHz超宽频带的范围内,复合电磁屏蔽膜层的电磁屏蔽效果均低于45dB。
对比例7
针对铝蒙皮基底首先进行碱性清洗剂超声清洁,去除表面油污等杂质,超声清洗剂采用5%质量浓度的氢氧化钠溶液,超声处理时间20分钟;
随后对清洗后的铝蒙皮表面进行等离子体活化处理,活化处理过程在真空腔室中进行,炉内保持0.3Pa气压,待处理工件表面施加220V偏压,离子源电流0.4A,处理过程中通入高纯氩气产生等离子体,氩气流速20sccm,处理时间25min。
针对活化后的铝蒙皮进行直流溅射沉积Ag、石墨/PTFE复合电磁屏蔽膜层,具体沉积参数为直流偏压450V,腔室压力2×10-3Pa,Ar气气流40sccm,沉积时间2min,溅射采用Ag、石墨/PTFE复合靶材,靶材直径10cm。
具体的靶材制备方法为,将PTFE粉末于380℃加热至粘稠状,在搅拌下加入银粉末和石墨粉末,银粉末平均粒径为40微米,银粉末添加量占PTFE粉末质量的15%,在持续加热保温下搅拌20min,随后转移至模具中加压排气冷却至室温。
由于仅添加一种粉末,导致最后膜层中对电磁波反射作用减弱,在1~40GHz超宽频带的范围内,复合电磁屏蔽膜层的电磁屏蔽效果均低于50dB。
对比例8
针对铝蒙皮基底首先进行碱性清洗剂超声清洁,去除表面油污等杂质,超声清洗剂采用5%质量浓度的氢氧化钠溶液,超声处理时间20分钟;
针对铝蒙皮进行直流溅射沉积Ag/PTFE复合电磁屏蔽膜层,具体沉积参数为直流偏压450V,腔室压力2×10-3Pa,Ar气气流40sccm,沉积时间2min,溅射采用Ag、石墨/PTFE复合靶材,靶材直径10cm。
具体的靶材制备方法为,将PTFE粉末于380℃加热至粘稠状,在搅拌下加入银粉末,银粉末平均粒径为40微米,银粉末添加量占PTFE粉末质量的12%,石墨粉末平均粒径为15微米,石墨粉末添加量占PTFE粉末质量的12%,在持续加热保温下搅拌20min,随后转移至模具中加压排气冷却至室温。制备得到的涂层还进行膜基结合强度测试,结合力为27N,可见未进行等离子体活化处理膜基结合强度会出现降低。
Claims (2)
1.一种直流磁控溅射法制备银、石墨/聚四氟乙烯复合电磁屏蔽膜层的方法,其特征在于,首先针对铝蒙皮基底进行碱性清洗剂超声清洁和等离子体活化处理,随后采用Ag、石墨/PTFE复合靶材直流溅射沉积膜层,具体沉积参数为直流偏压400~500V,腔室压力1×10-3~5×10-3Pa,Ar气气流30~50sccm,沉积时间1~3min;具体的靶材制备方法为,将PTFE粉末于370~390℃加热至粘稠状,在搅拌下加入银粉末和石墨粉末,银粉末平均粒径为30~50微米,银粉末添加量占PTFE粉末质量的10~15%,石墨粉末平均粒径为10~15微米,石墨粉末添加量占PTFE粉末质量的10~15%,在持续加热保温下搅拌15~30min,随后转移至模具中加压排气冷却至室温;所述等离子体活化处理过程在真空腔室中进行,炉内保持0.1~0.5Pa气压,待处理工件表面施加200~250V偏压,离子源电流0.3~0.5A,处理过程中通入高纯氩气产生等离子体,氩气流速10~25sccm,处理时间20~25min。
2.根据权利要求1所述的直流磁控溅射法制备银、石墨/聚四氟乙烯复合电磁屏蔽膜层的方法,其特征在于,针对铝蒙皮基底首先进行碱性清洗剂超声清洁,去除表面油污,超声清洗剂采用5%质量浓度的氢氧化钠溶液,超声处理时间5~30分钟。
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