CN112813396A - 一步磁控溅射沉积无机/有机交替混合结构超高阻隔膜的制备方法 - Google Patents
一步磁控溅射沉积无机/有机交替混合结构超高阻隔膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种一步磁控溅射沉积无机/有机交替混合结构超高阻隔膜的制备方法。尤其是在可弯曲的柔性基体上用无机物旋转靶材和有机物旋转靶材通过R2R一步法制备的超高阻隔膜，通过控制旋转靶材的配比和R2R工艺，制备了具有高阻水性能的柔性透明超高阻隔膜。WVTR：10‑6g/(m2·day)；透光率大于90％。可满足OLED、QLED和薄膜太阳能电池等柔性电子器件的封装要求。
Description
技术领域
本发明涉及一种超高阻隔膜的制备方法，具体涉及一种一步磁控溅射沉积无机/有机交替混合结构超高阻隔膜的制备方法。
背景技术
研究表明空气中水、氧和其它有害物质对OLED、QLED和薄膜太阳能电池等柔性电子器件的寿命影响很大，对柔性电子器件进行有效封装可以大大延长器件寿命。用于电子封装的高阻隔薄膜对透水蒸气率(WVTR)和透氧率(OTR)值要求更低，这种薄膜封装所用材料除了满足极低的气透率，还要求具有高透光性、稳定性，与封装器件有一致的膨胀系数等特点。传统刚性显示器件用特制玻璃进行封装即可满足要求，而柔性电子器件需要使用柔性透明高阻隔电子薄膜进行封装，以保证电子性能和使用寿命。无机薄膜通常比有机薄膜表现出更高的抗水渗透能力且无机单层薄膜制备工艺简单，成本低，相对于有机薄膜性能稳定受环境影响小使用寿命长，常常用于电子封装，不过在沉积过程中会产生多种缺陷，加上薄膜应力容易导致裂纹，受临界厚度制约。有机膜层的引入可以平滑无机层表面，弥补无机层缺陷，阻断无机薄膜缺陷通道，从而避免缺陷在无机薄膜层中的扩展，实现缺陷在厚度方向的近似独立化处理。但是无机-有机混合结构薄膜的制备成本高，不利于成品商品化。因为无机-有机多层膜的沉积通常是通过两种不同的沉积方法的两个步骤来完成的。有机层可以通过等离子体聚合、蒸发和湿涂层技术沉积，而无机层通常通过溅射、化学气相沉积(CVD)、和原子层沉积来沉积。因此，开发一种简单的有机-无机多层沉积工艺，采用一步式R2R加工方法，对高阻隔膜的大批量生产和商业化具有重要意义。
发明内容
发明目的：提供一种一步磁控溅射沉积无机/有机交替混合结构超高阻隔膜的制备方法。尤其是在可弯曲的柔性基体上用无机物旋转靶材和有机物旋转靶材通过R2R一步法制备的超高阻隔膜，通过控制旋转靶材的配比和R2R工艺，制备了具有高阻水性能的柔性透明超高阻隔膜。
技术方案：提供一种一步磁控溅射沉积无机—有机交替混合结构超高阻隔膜的制备方法。在可弯曲的柔性基体上用无机物旋转靶材和有机物旋转靶材通过R2R一步法制备了无机/有机连续多层膜。通过控制旋转靶材的配比和R2R工艺，实现高阻水性和高透明性的超高阻隔膜。用Ca电阻分析仪表征超高阻隔膜的阻隔性；用Agilent Cary-5000光谱仪表征透光性。
步骤1.可弯曲柔性原料卷通过开卷***向R2R***输送基板；
步骤2.基板在R2R***的真空室加热到55～75℃除去表面湿气；然后通过驱动装置进入等离子轰击室，400w的功率暴露于Ar/O2等离子体中，来改善薄膜之间的附着力；
步骤3.在R2R薄膜沉积***腔室1，射频功率10-15KW，Ar流量200-400SCCM，N2流量0-250SCCM，工作压力10mTorr；用无机物旋转靶材在柔性基板上沉积厚度50纳米的无机薄膜1；
步骤4.在R2R薄膜沉积***腔室2，射频功率1-2KW，纯Ar流量350SCCM，工作压力10mTorr；用有机物旋转靶材在无机薄膜1上沉积厚度60纳米的有机薄膜2；
步骤5.在R2R薄膜沉积***腔室3，射频功率10-15KW，Ar流量200-400SCCM，N2流量0-250SCCM，工作压力10mTorr；用无机物旋转靶材在有机薄膜2上沉积厚度50纳米的无机薄膜3；
步骤6.在R2R薄膜沉积***腔室4，射频功率1-2KW，纯Ar流量350SCCM，工作压力10mTorr；用有机物旋转靶材在无机薄膜3上沉积厚度60纳米的有机薄膜4；
步骤7.通过收卷***对沉积的无机—有机连续多层膜的超高阻隔膜重新卷绕成卷；
步骤8.用MOCON水蒸气透过率分析仪和Agilent Cary-5000光谱仪对制备的超高阻隔膜的阻水性能和光透性能表征。
附图说明
图1为本发明卷对卷(R2R)磁控溅射(MS)超高阻隔膜制备示意图。
具体实施方式
步骤1.可弯曲柔性原料卷通过开卷***向R2R***输送基板；
步骤2.基板在R2R***的真空室加热到55～75℃除去表面湿气；然后通过驱动装置进入等离子轰击室，350～450W的功率暴露于Ar/O2等离子体中，来改善薄膜之间的附着力；
步骤3.在R2R薄膜沉积***腔室，射频功率10-15KW，Ar流量200-400SCCM，N2流量0-250SCCM，工作压力10mTorr；用无机物旋转靶材在柔性基板上沉积厚度50纳米的无机薄膜；
步骤4.在R2R薄膜沉积***腔室，射频功率1-2KW，纯Ar流量350SCCM，工作压力10mTorr；用有机物旋转靶材在无机薄膜上沉积厚度60纳米的有机薄膜；
步骤5.在R2R薄膜沉积***腔室，射频功率10-15KW，Ar流量200-400SCCM，N2流量0-250SCCM，工作压力10mTorr；用无机物旋转靶材在有机薄膜上沉积厚度50纳米的无机薄膜；
步骤6.在R2R薄膜沉积***腔室，射频功率1-2KW，纯Ar流量350SCCM，工作压力10mTorr；用有机物旋转靶材在无机薄膜上沉积厚度60纳米的有机薄膜；
步骤7.通过收卷***对沉积的无机—有机连续多层膜的超高阻隔膜重新卷绕成卷；
步骤8.用MOCON水蒸气透过率分析仪和Agilent Cary-5000光谱仪对制备的超高阻隔膜的阻水性能和光透性能表征。
实施例1
(1)可弯曲PET原料卷通过开卷***向R2R***输送PET基板。
(2)PET基板在R2R***的真空室加热到55～75℃除去表面湿气；然后通过驱动装置进入等离子轰击室，400w的功率暴露于Ar/O2等离子体中，来改善薄膜之间的附着力。
(3)在R2R薄膜沉积***腔室1，射频功率12KW，纯Ar流量350SCCM，工作压力10mTorr；用氧化铝旋转靶材在PET基板上沉积厚度50纳米的氧化铝薄膜。
(4)在R2R薄膜沉积***腔室2，射频功率1.0KW，纯Ar流量350SCCM，工作压力10mTorr；用聚四氟乙烯(PTFE)旋转靶材在氧化铝上沉积厚度60纳米的PTFE薄膜。
(5)在R2R薄膜沉积***腔室3，射频功率12KW，纯Ar流量350SCCM，工作压力10mTorr；用氧化铝旋转靶材在PTFE上沉积厚度50纳米的氧化铝薄膜。
(6)在R2R薄膜沉积***腔室4，射频功率1.0KW，纯Ar流量350SCCM，工作压力10mTorr；用聚四氟乙烯(PTFE)旋转靶材在氧化铝上沉积厚度60纳米的PTFE薄膜。
(7)通过收卷***对沉积的氧化铝—聚四氟乙烯连续多层膜的超高阻隔膜重新卷绕成卷。
(8)用Ca电阻水蒸气透过率分析仪和Agilent Cary-5000光谱仪对制备的超高阻隔膜的阻水性能和光透性能表征。
实施例2
(1)可弯曲PET原料卷通过开卷***向R2R***输送PET基板。
(2)PET基板在R2R***的真空室加热到55～75℃除去表面湿气；然后通过驱动装置进入等离子轰击室，400w的功率暴露于Ar/O2等离子体中，来改善薄膜之间的附着力。
(3)在R2R薄膜沉积***腔室1，射频功率12KW，纯Ar流量350SCCM，工作压力10mTorr；用氧化铝旋转靶材在PET基板上沉积厚度50纳米的氧化铝薄膜。
(4)在R2R薄膜沉积***腔室2，射频功率1.0KW，纯Ar流量350SCCM，工作压力10mTorr；用碳纳米管掺杂聚四氟乙烯(PPFC)旋转靶材在氧化铝上沉积厚度60纳米的PPFC薄膜。
(5)在R2R薄膜沉积***腔室3，射频功率12KW，纯Ar流量350SCCM，工作压力10mTorr；用氧化铝旋转靶材在PPFC上沉积厚度50纳米的氧化铝薄膜。
(6)在R2R薄膜沉积***腔室4，射频功率1.0KW，纯Ar流量350SCCM，工作压力10mTorr；用碳纳米管掺杂聚四氟乙烯(PPFC)旋转靶材在氧化铝上沉积厚度60纳米的PPFC薄膜。
(7)通过收卷***对沉积的Al2O3-PPFC连续多层膜的超高阻隔膜重新卷绕成卷。
(8)用Ca电阻水蒸气透过率分析仪和Agilent Cary-5000光谱仪对制备的超高阻隔膜的阻水性能和光透性能表征。
实施例3
(1)可弯曲PET原料卷通过开卷***向R2R***输送PET基板。
(2)PET基板在R2R***的真空室加热到55～75℃除去表面湿气；然后通过驱动装置进入等离子轰击室，400w的功率暴露于Ar/O2等离子体中，来改善薄膜之间的附着力。
(3)在R2R薄膜沉积***腔室1，射频功率12KW，纯Ar流量350SCCM，工作压力10mTorr；用氧化硅旋转靶材在PET基板上沉积厚度50纳米的SiO2薄膜。
(4)在R2R薄膜沉积***腔室2，射频功率1.0KW，纯Ar流量350SCCM，工作压力10mTorr；聚四氟乙烯(PTFE)旋转靶材在氧化硅上沉积厚度60纳米的PTFE薄膜。
(5)在R2R薄膜沉积***腔室3，射频功率12KW，纯Ar流量350SCCM，工作压力10mTorr；用氧化硅旋转靶材在PTFE上沉积厚度50纳米的SiO2薄膜。
(6)在R2R薄膜沉积***腔室4，射频功率1.0KW，纯Ar流量350SCCM，工作压力10mTorr；聚四氟乙烯(PTFE)旋转靶材在氧化硅上沉积厚度60纳米的PTFE薄膜。
(7)通过收卷***对沉积的氧化硅—PTFE连续多层膜的超高阻隔膜重新卷绕成卷。
(8)用Ca电阻水蒸气透过率分析仪和Agilent Cary-5000光谱仪对制备的超高阻隔膜的阻水性能和光透性能表征。
实施例4
(1)可弯曲PET原料卷通过开卷***向R2R***输送PET基板。
(2)PET基板在R2R***的真空室加热到55～75℃除去表面湿气；然后通过驱动装置进入等离子轰击室，400w的功率暴露于Ar/O2等离子体中，来改善薄膜之间的附着力。
(3)在R2R薄膜沉积***腔室1，射频功率12KW，纯Ar流量350SCCM，工作压力10mTorr；用氧化硅旋转靶材在PET基板上沉积厚度50纳米的SiO2薄膜。
(4)在R2R薄膜沉积***腔室2，射频功率1.0KW，纯Ar流量350SCCM，工作压力10mTorr；碳纳米管掺杂聚四氟乙烯(PPFC)旋转靶材在氧化硅上沉积厚度60纳米的PPFC薄膜。
(5)在R2R薄膜沉积***腔室3，射频功率12KW，纯Ar流量350SCCM，工作压力10mTorr；用氧化硅旋转靶材在PPFC上沉积厚度50纳米的SiO2薄膜。
(6)在R2R薄膜沉积***腔室4，射频功率1KW，纯Ar流量350SCCM，工作压力10mTorr；碳纳米管掺杂聚四氟乙烯(PPFC)旋转靶材在氧化硅上沉积厚度60纳米的PPFC薄膜。
(7)通过收卷***对沉积的SiO2—PPFC连续多层膜的超高阻隔膜重新卷绕成卷。
(8)用Ca电阻水蒸气透过率分析仪和Agilent Cary-5000光谱仪对制备的超高阻隔膜的阻水性能和光透性能表征。
实施例5
(1)可弯曲PET原料卷通过开卷***向R2R***输送PET基板。
(2)PET基板在R2R***的真空室加热到55～75℃除去表面湿气；然后通过驱动装置进入等离子轰击室，400w的功率暴露于Ar/O2等离子体中，来改善薄膜之间的附着力。
(3)在R2R薄膜沉积***腔室1，射频功率10KW，Ar流量200SCCM，N2流量200SCCM，工作压力10mTorr；用硅旋转靶材在PET基板上沉积厚度50纳米的SiNx薄膜。
(4)在R2R薄膜沉积***腔室2，射频功率1.5KW，纯Ar流量350SCCM，工作压力10mTorr；碳纳米管掺杂聚四氟乙烯(PPFC)旋转靶材在SiNx上沉积厚度60纳米的PPFC薄膜。
(5)在R2R薄膜沉积***腔室3，射频功率10KW，Ar流量300SCCM，N2流量150SCCM，工作压力10mTorr；用硅旋转靶材在PPFC上沉积厚度50纳米的SiNx薄膜。
(6)在R2R薄膜沉积***腔室4，射频功率1.5KW，纯Ar流量350SCCM，工作压力10mTorr；碳纳米管掺杂聚四氟乙烯(PPFC)旋转靶材在SiNx上沉积厚度60纳米的PPFC薄膜。
(7)通过收卷***对沉积的SiNx—PPFC连续多层膜的超高阻隔膜重新卷绕成卷。
(8)用Ca电阻水蒸气透过率分析仪和Agilent Cary-5000光谱仪对制备的超高阻隔膜的阻水性能和光透性能表征。
| 发明实施 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
| WVTR(g/(m<sup>2</sup>·day)) | ≤10<sup>-5</sup> | ≤10<sup>-5</sup> | ≤10<sup>-6</sup> | ≤10<sup>-4</sup> | ≤10<sup>-4</sup> |
| 透光率(％) | 91 | 92 | 92 | 89 | 90 |
上述实施例仅用于说明本发明，根据上述实施例，可以更好地理解本发明，而不用于限制本发明的范围。此外，本领域科研技术人员在阅读本发明后，以等同替换或变量等对本发明进行各种修改，同样属于本发明权利要求书所限定的范围。
Claims (4)
1.一种一步磁控溅射沉积无机/有机交替混合结构超高阻隔膜的制备方法，其特征在于：在可弯曲的柔性原料卷上用无机物旋转靶材和有机物旋转靶材通过R2R一步法制备超高阻隔膜，通过控制旋转靶材的配比和R2R工艺，制备具有高阻水性能的柔性透明超高阻隔膜。
2.根据权利要求1所述的一步磁控溅射沉积无机/有机交替混合结构超高阻隔膜的制备方法，其特征在于：无机物旋转靶材为氧化铝、氧化硅、氧化钛、氮化硅或氮氧化铝中的一种或一种以上；有机物旋转靶材为聚四氟乙烯、碳纳米管掺杂聚四氟乙烯、石墨烯掺杂聚四氟乙烯、聚甲基丙烯酸甲酯或聚酰亚胺中的一种或一种以上；柔性原料卷为PET、PI、PES、PDMS或柔性玻璃中的一种或一种以上；
步骤如下：
步骤1.可弯曲柔性原料卷通过开卷***向R2R***输送基板；
步骤2.基板在R2R***的真空室加热到55～75℃除去表面湿气；然后通过驱动装置进入等离子轰击室，350～450w的功率暴露于Ar/O2等离子体中，来改善薄膜之间的附着力；
步骤3.在R2R薄膜沉积***腔室1，射频功率10-15KW,Ar流量200-400SCCM，N2流量0-250SCCM，工作压力10mTorr；用无机物旋转靶材在柔性基板上沉积厚度50纳米的无机薄膜1；
步骤4.在R2R薄膜沉积***腔室2，射频功率1-2KW，纯Ar流量350SCCM，工作压力10mTorr；用有机物旋转靶材在无机薄膜1上沉积厚度60纳米的有机薄膜2；
步骤5.在R2R薄膜沉积***腔室3，射频功率10-15KW，Ar流量200-400SCCM，N2流量0-250SCCM，工作压力10mTorr；用无机物旋转靶材在有机薄膜2上沉积厚度50纳米的无机薄膜3；
步骤6.在R2R薄膜沉积***腔室4，射频功率1-2KW，纯Ar流量350SCCM，工作压力10mTorr；用有机物旋转靶材在无机薄膜3上沉积厚度60纳米的有机薄膜4；
步骤7.通过收卷***对沉积的无机-有机连续多层膜的超高阻隔膜重新卷绕成卷；
步骤8.用MOCON水蒸气透过率分析仪和Agilent Cary-5000光谱仪对制备的超高阻隔膜的阻水性能和光透性能表征。
3.根据权利要求2所述的一步磁控溅射沉积无机/有机交替混合结构超高阻隔膜的制备方法，其特征在于：超高阻隔膜包括至少两个无机层；用的无机物旋转靶材还包括各种掺杂的复合无机旋转靶材。
4.根据权利要求2所述的一步磁控溅射沉积无机/有机交替混合结构超高阻隔膜的制备方法，其特征在于：超高阻隔膜包括至少两个有机层；有机旋转靶材还包括各种掺杂的复合有机旋转靶材。
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| US20030203210A1 (en) * | 2002-04-30 | 2003-10-30 | Vitex Systems, Inc. | Barrier coatings and methods of making same |
| US20040195960A1 (en) * | 2001-08-20 | 2004-10-07 | Grzegorz Czeremuszkin | Coatings with low permeation of gases and vapors |
| WO2017039342A1 (ko) * | 2015-09-01 | 2017-03-09 | 한국화학연구원 | 탄화불소 박막을 포함하는 배리어 필름 및 이의 제조방법 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040195960A1 (en) * | 2001-08-20 | 2004-10-07 | Grzegorz Czeremuszkin | Coatings with low permeation of gases and vapors |
| US20030203210A1 (en) * | 2002-04-30 | 2003-10-30 | Vitex Systems, Inc. | Barrier coatings and methods of making same |
| WO2017039342A1 (ko) * | 2015-09-01 | 2017-03-09 | 한국화학연구원 | 탄화불소 박막을 포함하는 배리어 필름 및 이의 제조방법 |
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