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[求助] AAO制备 磷酸电解液

我想制备大孔(超过100nm)孔径的AAO模板,制备过程中,首先AL片退火,我直接在空气气氛中放在电阻炉里退火的,然后是升温时间200min,到450度,然后450度保温3小时,这时候Al片有些地方黑黑的 ,请问你们退火是怎样的?
然后抛光后,用磷酸电解液,0.3mol/L,才50V电压,几分钟就烧断了,后来我用玻璃棒搅拌后,还是20几分钟的时候断了,看到文献上说,氧化几个小时 ,十几个小时的,都是怎么办到的呀,你们是怎么做的呀,膜都做不出来,后面我没法进行我的实验内容了呀,拜托拜托
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