2011-10-15射频磁控溅射法制备PZT薄膜工艺及研究

射频磁控溅射法制备PZT薄膜工艺及研究2011-10-15射频磁控溅射法制备PZT薄膜对制备的PZT薄膜能谱分析测PZT薄膜的厚度(Si基底)对制备的PZT薄膜进行退火处理对退火后的样品ESEM表征拉曼分析实验材料及设备：载玻片（1cm×1cm），硅片（0.5cm×0.5cm）PZT靶材：国材科技（ChinaMaterialTechnolpgy）镀膜机：MSP/ED-300c型磁控溅射/热蒸发镀膜机（北京创世威纳科技有限公司）一、射频磁控溅射法制备PZT薄膜Purity:Pb(Zr0.52Ti0.48)O3,实验工艺参数：溅射系统：MSP/ED-300c型薄膜溅射系统溅射靶材：Pb(Zr0.52Ti0.48)O3基片至靶间距：10cm背底真空度：1×10-4Pa溅射气氛：Ar/O2=45/0溅射气压：0.53Pa（实际值1.1Pa）衬底温度：室温溅射功率：160W溅射时间：0.5h，1h，1.5h，2h，2.5h，3h，3.5h实验过程：1、衬底的处理将载玻片（1cm×1cm），硅片（0.5cm×0.5cm）分别放入烧杯中，使硅片正面朝上，以免超声清洗过程中衬底与烧杯底部摩擦刮花。加入适量丙酮浸泡同时进行超声清洗15min，然后用去离子水冲洗，再加入酒精浸泡并超声清洗15min，以除去丙酮及其余杂质。之后经过氮气吹干，烘烤除湿处理。2、用脱脂棉蘸取酒精清洗镀膜机以确保能抽至高真空3、镀膜实验结果：样品编号溅射时间（h）本底真空度(×105Pa)溅射功率（W）溅射气压(Pa)衬底温度（oC）Sample10.58.81601.123.3Sample218.51601.123.5Sample31.58.81601.123.5Sample426.61601.123.3Sample52.58.51601.123.7Sample638.51601.123.3Sample73.58.51601.124.1二、对射频磁控溅射法制备的PZT薄膜能谱分析NanoSEM430Sample1-SiSample2-SiSample3-SiSample4-SiSample5-SiSample6-SiElementLineWeight%Atom%OK21.2669.29TiK5.596.08TiL------ZrL19.4311.11ZrM------PbL------PbM53.7213.52Total100.00100.00ElementLineWeight%Atom%OK14.5059.83TiK7.009.65TiL------ZrL13.589.83ZrM------PbM64.9220.69Total100.00100.00ElementLineWeight%Atom%CK7.3329.66OK14.3643.59TiK7.147.24TiL------ZrL9.485.05ZrM------PbM61.6914.46Total100.00100.00ElementLineWeight%Atom%OK15.2961.29TiK7.7610.39TiL------ZrL11.448.04ZrM------PbM65.5020.27Total100.00100.00ElementLineWeight%Atom%OK14.5959.58TiK8.4511.52TiL------ZrL11.578.28ZrM------PbM65.3920.62Total100.00100.00ElementLineWeight%Atom%OK15.8562.10TiK8.3410.91TiL------ZrL10.547.24ZrM------PbM65.2719.75Total100.00100.00Sample1-SiSample2-SiSample3-SiSample4-SiSample5-SiSample6-Si样品溅射时间（h）ZrAtom%TiAtom%Zr/TiPZT靶材中Zr/TiSample10.511.116.081.830.52/0.481.08Sample219.839.651.02Sample31.55.057.240.70Sample428.0410.390.77Sample52.58.2811.520.72Sample637.2410.910.66在硅基底上所成的膜中Zr元素和Ti元素的原子比：1、随着溅射时间越长，PZT膜中Zr/Ti逐渐下降；2、当溅射时间为1h时，所成PZT膜中Zr/Ti最接近与靶材中的Zr/Ti；Sample1-glassSample2-glassSample3-glassSample4-glassSample5-glassSample6-glassSample1-glassSample2-glassSample3-glassSample4-glassSample5-glassSample6-glassElementLineWeight%Atom%OK19.3659.17NaK1.513.22SiK7.4112.89SiL------TiK6.686.82TiL------ZrL8.544.58ZrM------PbM56.4913.33Total100.00100.00ElementLineWeight%Atom%OK14.8660.28SiK0.771.79SiL------TiK7.119.63TiL------ZrL10.297.32ZrM------PbM66.9720.98Total100.00100.00ElementLineWeight%Atom%OK16.3463.78TiK6.919.01TiL------ZrL10.627.27ZrM------PbM66.1319.94Total100.00100.00ElementLineWeight%Atom%OK15.9062.20TiK7.9310.35TiL------ZrL11.587.94ZrM------PbM64.5919.51Total100.00100.00ElementLineWeight%Atom%OK15.9262.41TiK8.1810.72TiL------ZrL10.106.95ZrM------PbM65.7919.92Total100.00100.00ElementLineWeight%Atom%OK15.8162.36TiK7.8710.38TiL------ZrL10.347.16ZrM------PbM65.9820.10Total100.00100.00样品溅射时间（h）ZrAtom%TiAtom%Zr/TiPZT靶材中Zr/TiSample10.54.586.820.670.52/0.481.08Sample217.329.630.76Sample31.57.279.010.81Sample427.9410.350.77Sample52.56.9510.720.65Sample637.1610.380.69在玻璃基底上所成的膜中Zr元素和Ti元素的原子比：1、随着溅射时间越长，PZT膜中Zr/Ti先上升在下降，在1.5h时Zr/Ti最大；2、当溅射时间为1.5h时，所成PZT膜中Zr/Ti最接近与靶材中的Zr/Ti；三、测PZT薄膜的厚度Sample(1-7)-Si溅射时间与膜厚的关系：样品溅射时间（h）PZT膜的厚度（nm）Sample1-Si0.5145.05Sample2-Si1281.46Sample3-Si1.5524.18Sample4-Si2446.92Sample5-Si2.5708.58Sample6-Si3804.00Sample7-Si3.51329.14四、对制备的PZT薄膜进行退火处理Lilienthal(Germany)NaberthermLHT02/18样品退火温度（oC）保温时间（min）区别Sample165010将样品放于电烤炉中加热至650oCSample265010Sample3（Si）65040先将电烤炉加热至650oC左右，然后将样品放在电烤炉内Sample4（Si）65040Sample5（Si）65040Sample6（Si）65040Sample7（Si）65040五、对退火后的样品ESEM表征Sample1-118Sample2-127Sample3-98Sample4-24Sample5-20Sample6-7Sample7-3膜的厚度与所成裂纹的关系：样品溅射时间（h）PZT膜的厚度（nm）裂纹数Sample1-Si0.5145.05118Sample2-Si1281.46127Sample3-Si1.5524.1898Sample4-Si2446.9224Sample5-Si2.5708.5820Sample6-Si3804.007Sample7-Si3.51329.143六、拉曼分析退火后退火前