基于响应面法的原子层沉积高阻隔膜研究  

Atomic Layer Deposition of High Barrier Films Based on Response Surface Method

作　　者：赵丽丽[1] 林晶[1] 于贵文[1] 董静[1] ZHAO Li-li;LIN Jing;YU Gui-wen;DONG Jing(Packaging Science and Printing Technology Engineering Laboratory,Harbin University of Commerce,Harbin 150028,China)

机构地区：[1]哈尔滨商业大学包装科学与工程技术实验室,哈尔滨150028

出　　处：《包装工程》2022年第23期167-173,共7页Packaging Engineering

基　　金：哈尔滨商业大学青年创新人才计划(18XN032);黑龙江高校科技成果(TSTAU-R2018009)。

摘　　要：目的研究分析等离子辅助原子层沉积技术(ALD)技术在PET表面上沉积超薄Al_(2)O_(3)阻隔层的工艺优化。方法采用单因素结合响应面设计试验法,对Al_(2)O_(3)/PET薄膜的沉积速率(GPC)进行优化,通过AFM分析得到薄膜的生长模式和表面粗糙度,最后用水蒸气透过率表征薄膜的阻隔性能。结果最大GPC的沉积参数:TMA脉冲时间为0.17 s、吹扫时间为11 s、O_(2)的脉冲时间为0.35 s、吹扫时间为10 s、沉积速率为0.215 nm/cycle;薄膜以层状生长模式生长,表面粗糙度均方根(RMS)为0.58 nm;沉积500个循环后薄膜的水透过率从7.456 g∙d/m2降低到0.319 g∙d/m2。结论通过响应面法优化了ALD制备工艺参数,Al_(2)O_(3)在PET表面沉积100 nm左右时,水蒸气阻隔性提高了25倍。The work aims to study and analyze the process optimization of deposition of ultra-thin Al_(2)O_(3)barrier layer on PET surface by plasma-assisted atomic layer deposition(ALD).The deposition rate(GPC)of Al_(2)O_(3)/PET film was optimized by single factor combined with response surface design method.The growth mode and surface roughness of the film were obtained by AFM analysis.Finally,the barrier property of the film was characterized by water vapor transmission rate.According to the experimental results,the deposition parameters of the largest GPC were:TMA pulse time 0.17 s,purge time 11 s,O2 pulse time 0.35 s,purge time 10 s,deposition rate 0.215 nm/cycle;the film grew in a layered growth mode with a rough surface.The root mean square(RMS)was 0.58 nm;the water permeability decreased from 7.456 g∙d/m2 of the original film to 0.319 g∙d/m2 after 500 cycles of deposition.The preparation parameters of ALD are optimized by response surface methodology,and the water vapor barrier was increased by 25 times when Al_(2)O_(3)is de-posited on PET surface at about 100 nm.

关 键 词：原子层沉积 Box-Behnken响应面法 Al_(2)O_(3)/PET高阻隔膜 

分 类 号：O484.5[理学—固体物理]