使用SEM和EDS能谱对薄膜前处理锆化膜形貌和元素组成进行了表征,并分析了薄膜前处理控制变量对锆成膜量的影响。结果表明,锆系薄膜主要由Zr和Si元素组成,其中Zr和Si的质量分数分别为2%和0.2%;锆成膜量随着温度的升高而增加,锆成膜量在30~35℃区间随温度的变化幅度较其他温度区间大;随着处理液锆浓度的提高,锆成膜量也随之增加,当锆浓度由0.2 mg/L提高到0.4 mg/L时,锆成膜增加量相对最多,增加量为10 mg/m2;提高处理液的pH也能够促进锆成膜,当pH在4.5~4.8区间时,锆成膜量随pH的变化最为明显;锆成膜量随着处理时间的延长逐渐增加,且成膜速度呈现出先快后慢的趋势;而随着薄膜处理液游离氟的提高,锆成膜量呈现下降的趋势,在15~25 mg/L区间,锆成膜量受游离氟变化的影响最大。

he morphology and elemental composition of the zirconium films prepared by thin film pretreatment were analyzed by SEM and EDS,and the influence of the control variables of thin film pretreatment on the amount of zirconium film formation was analyzed.The results showed that the zirconiumbased thin films were mainly composed of Zr and Si elements,and the weight percentages of Zr and Si were2%and 0.2%.The amount of zirconium film formation increased with the increase of temperature,and the variation of the amount of zirconium film formation with temperature in the range of 30~35℃was larger than that in other temperature ranges.When the concentration of zirconium in the treatment solution increased,the amount of zirconium film formation also increased.When the concentration of zirconium increased from 0.2 mg/L to 0.4 mg/L,the increase in zirconium film formation was relatively the largest,with an increase of 10 mg/m~2.Increasing the pH of the treatment solution could also promote zirconium film formation,and when the pH was in the range of 4.5~4.8,the change of zirconium film formation with pH was the most obvious.The amount of zirconium film formation increased gradually with the prolongation of the treatment time,and the film formation speed showed a trend of fast at first and then slow.With the increase of free fluorine in the film treatment solution,the zirconium film formation showed a downward trend,in the range of 15~25 mg/L,the amount of zirconium film was most affected by the change of free fluorine.