CN110364357A - 一种高储能密度电容器及其制备方法 - Google Patents
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Abstract
本发明公开了一种高储能密度电容器及其制备方法，利用磁控溅射技术和热蒸镀技术制备的Bi2Mg2/3Nb4/3O7基高储能电容器具有无毒、体积小、储能密度大、高储能效率的特点，储能密度高达30J/cm3以上，由于薄膜性能优良，成本低廉，适合工业化生产。
Description
技术领域
本发明属于电容器制造领域，涉及一种高储能密度电容器及其制备方法。
背景技术
目前，高储能元器件在民用和军用领域均发挥着至关重要的作用。如果制备出兼具高功率密度又有高储能密度的理想储能元器件，有望实现二合一功能的全新电源***，将极大减小电源的重量和体积，加快电源***小型化进程，在工业控制、风光发电、交通工具、智能三表、电动工具等民用领域具有极大的应用前景。在高储能元器件中，电介质电容器的功率密度高，且温度稳定性好、安全性高。因此，基于电介质电容材料最有望制备出兼具高功率密度和高储能密度的理想储能元器件。
近年来，对电介质电容材料的研究主要集中在钽酸锶铋(SBT)、钛酸锶钡(BST)、锆钛酸铅(PZT)等几种材料。其中，SBT薄膜具有较好的抗疲劳特性、小的漏电流密度，但是其成膜温度较高，薄膜组分不容易控制，并且介电常数(～110)也较低，难以用来制备高储能密度电容器。BST薄膜具有优良的化学稳定性和热稳定性，并具有高的介电常数(>500)，但是其介电损耗和漏电流都较大，且有一个致命弱点，即BST薄膜的击穿场强较低，这就限制了BST薄膜在高储能密度电容器中的应用。PZT的研究已经比较成熟，研究人员已经研发出储能密度高达30J/cm3的PZT基薄膜电容器。但是由于这类材料含有易挥发的重金属铅，这种高毒性使其很难应用于民用领域，学者们在努力地探寻其它的研究方向，以求获得能够取代PZT的新型高储能材料。
发明内容
为了解决现有技术中存在的问题，本发明提供一种高储能密度电容器及其制备方法，解决现有技术中高储能密度电容器材料含有重金属，不够绿色环保的问题。
本发明的技术方案为：
一种高储能密度电容器，由以下方法制备得到：
(1)将Pt靶材、Bi2Mg2/3Nb4/3O7靶材装入磁控溅射腔体内；
(2)将硅基片放置在磁控溅射腔体的样品台上；
(3)待步骤(2)完成后，将磁控溅射***的本底真空度抽至3.0×10-3Pa以下，使用纯Ar气体溅射Pt层；
(4)待步骤(3)完成后，使用掩膜版覆盖部分Pt层，然后将磁控溅射***的本底真空度抽至1.0×10-3Pa以下，使用Ar和O2混合气体作为溅射气体，溅射功率为50～300W，进行沉积得到Bi2Mg2/3Nb4/3O7层；由此得到结构为Si/Pt/Bi2Mg2/3Nb4/3O7的样品；
(5)待步骤(4)完成后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品放入退火炉中空气退火10min～30min，退火温度为500℃～750℃；
(6)步骤(5)完成后，将Bi2Mg2/3Nb4/3O7层上覆盖金属掩膜版，使用热蒸镀设备制备Au顶电极，最终得到Pt金属底电极/Bi2Mg2/3Nb4/3O7层/Au金属顶电极三层结构的无铅Bi2Mg2/3Nb4/3O7基储能电容器。
所述步骤(1)Pt靶材为任意市售或者自制靶材，纯度为99％以上；Bi2Mg2/3Nb4/3O7靶材为常规的固相烧结法自制而成，靶材的纯度为98％以上；靶材与衬底的距离优选为40mm～150mm。
所述步骤(3)Ar气体纯度在99.99％以上；Pt层厚度为30nm～300nm。
所述步骤(4)Ar和O2的纯度均在99.99％以上，氧氩比为1/50～2/3；溅射总气压0.3～15Pa，Bi2Mg2/3Nb4/3O7层的厚度可以通过调节制备工艺参数或沉积时间控制，厚度为20nm～200nm。
所述步骤(5)将热蒸镀设备的本底真空抽至9.0×10-4Pa以下，将电流控制在80～130A，待Au蒸镀完全后关闭蒸发电源。
一种高储能密度电容器的制备方法，包括以下步骤：
(1)将Pt靶材、Bi2Mg2/3Nb4/3O7靶材装入磁控溅射腔体内；
(3)将硅基片放置在磁控溅射腔体的样品台上；
(3)待步骤(2)完成后，将磁控溅射***的本底真空度抽至3.0×10-3Pa以下，使用纯Ar气体溅射Pt层；
(4)待步骤(3)完成后，使用掩膜版覆盖部分Pt层，然后将磁控溅射***的本底真空度抽至1.0×10-3Pa以下，使用Ar和O2混合气体作为溅射气体，溅射功率为50W～300W，进行沉积得到Bi2Mg2/3Nb4/3O7层；由此得到结构为Si/Pt/Bi2Mg2/3Nb4/3O7的样品；
(5)待步骤(4)完成后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品放入退火炉中空气退火10min～30min，退火温度为500℃～750℃；
(6)步骤(5)完成后，将Bi2Mg2/3Nb4/3O7层上覆盖金属掩膜版，使用热蒸镀设备制备Au顶电极，最终得到Pt金属底电极/Bi2Mg2/3Nb4/3O7层/Au金属顶电极三层结构的无铅Bi2Mg2/3Nb4/3O7基储能电容器。
所述步骤(1)Pt靶材为任意市售或者自制靶材，纯度为99％以上；Bi2Mg2/3Nb4/3O7靶材为常规的固相烧结法自制而成，靶材的纯度为98％以上；靶材与衬底的距离优选为40mm～150mm。
所述步骤(3)Ar气体纯度在99.99％以上；Pt层厚度为30nm～300nm。
所述步骤(4)Ar和O2的纯度均在99.99％以上，氧氩比为1/50～2/3；溅射总气压0.3～15Pa，Bi2Mg2/3Nb4/3O7层的厚度可以通过调节制备工艺参数或沉积时间控制，厚度为20nm～200nm。
所述步骤(5)将热蒸镀设备的本底真空抽至9.0×10-4Pa以下，将电流控制在80～130A，待Au蒸镀完全后关闭蒸发电源。
本发明有益效果：本发明利用磁控溅射技术和热蒸镀技术制备的Bi2Mg2/3Nb4/3O7基高储能电容器具有无毒、体积小、储能密度大、高储能效率的特点，储能密度高达30J/cm3以上，由于薄膜性能优良，成本低廉，适合工业化生产。
附图说明
图1为实施例1中制备在硅衬底上的无铅Bi2Mg2/3Nb4/3O7基高储能薄膜电容器的极化强度随外加场强变化的测试曲线图。
具体实施方式
下面结合附图和具体实施例，对本发明的技术方案作进一步详细说明。
实施例1
1.将Pt靶材、Bi2Mg2/3Nb4/3O7靶材装入磁控溅射腔体内，靶材与衬底的距离为100mm。
2.然后，先后用无水乙醇和去离子水超声清洗硅衬底，并用高纯氮气吹干，放入磁控溅射样品台上。
3.步骤2完成后，使用掩膜版覆盖部分Pt层，将磁控溅射***的本底真空度抽至5.0×10-4Pa。通入高纯(99.99％)Ar气体。进行沉积得到100nm的Pt层。
4.步骤3结束后，将磁控溅射***的本底真空度抽至5.0×10-4Pa，通入高纯Ar和O2。溅射功率为120w，氧氩比为3：17，温度为室温。进行沉积得到180nm厚的Bi2Mg2/3Nb4/3O7薄膜。由此得到结构为Si/Pt/Bi2Mg2/3Nb4/3O7的样品。
5.待步骤4完成后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品放入退火炉中在700℃下空气退火10min。
6.步骤5结束后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品转移至热蒸镀设备蒸发室内的样品台上，其上覆盖金属掩膜版，将待蒸发Au放置在蒸发舟内。将热蒸镀设备的本底真空抽至5.0×10-3Pa，将电流从80A逐渐升至110A，待Au蒸镀完全后关闭蒸发电源。
图1为实施例1中制备在硅衬底上的无铅Bi2Mg2/3Nb4/3O7基高储能薄膜电容器的极化强度随外加场强变化的测试曲线图，由图算出薄膜储能密度为36.8J/cm3。
实施例2
1.将Pt靶材、Bi2Mg2/3Nb4/3O7靶材装入磁控溅射腔体内，靶材与衬底的距离为150mm。
2.然后，先后用无水乙醇和去离子水超声清洗硅衬底，并用高纯氮气吹干，放入磁控溅射样品台上。
3.步骤2完成后，使用掩膜版覆盖部分Pt层，将磁控溅射***的本底真空度抽至5.0×10-4Pa。通入高纯(99.99％)Ar气体。进行沉积得到100nm的Pt层。
4.步骤3结束后，将磁控溅射***的本底真空度抽至5.0×10-4Pa，通入高纯Ar和O2。溅射功率为300W，氧氩比为3：17，温度为室温。进行沉积得到200nm厚的Bi2Mg2/3Nb4/3O7薄膜。由此得到结构为Si/Pt/Bi2Mg2/3Nb4/3O7的样品。
5.待步骤4完成后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品放入退火炉中在750℃下空气退火10min。
6.步骤5结束后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品转移至热蒸镀设备蒸发室内的样品台上，其上覆盖金属掩膜版，将待蒸发Au放置在蒸发舟内。将热蒸镀设备的本底真空抽至5.0×10-3Pa，将电流从80A逐渐升至110A，待Au蒸镀完全后关闭蒸发电源。
实施例2中制备在硅衬底上的无铅Bi2Mg2/3Nb4/3O7基高储能薄膜电容器的储能密度约为35.5J/cm3。
实施例3
1.将Pt靶材、Bi2Mg2/3Nb4/3O7靶材装入磁控溅射腔体内，靶材与衬底的距离为100mm。
2.然后，先后用无水乙醇和去离子水超声清洗硅衬底，并用高纯氮气吹干，放入磁控溅射样品台上。
3.步骤2完成后，使用掩膜版覆盖部分Pt层，将磁控溅射***的本底真空度抽至5.0×10-4Pa。通入高纯(99.99％)Ar气体。进行沉积得到30nm的Pt层。
4.步骤3结束后，将磁控溅射***的本底真空度抽至5.0×10-4Pa，通入高纯Ar和O2。溅射功率为50W，氧氩比为1：9，温度为室温。进行沉积得到20nm厚的Bi2Mg2/3Nb4/3O7薄膜。由此得到结构为Si/Pt/Bi2Mg2/3Nb4/3O7的样品。
5.待步骤4完成后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品放入退火炉中在600℃下空气退火15min。
6.步骤5结束后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品转移至热蒸镀设备蒸发室内的样品台上，其上覆盖金属掩膜版，将待蒸发Au放置在蒸发舟内。将热蒸镀设备的本底真空抽至5.0×10-3Pa，将电流从80A逐渐升至110A，待Au蒸镀完全后关闭蒸发电源。
实施例3中制备在硅衬底上的无铅Bi2Mg2/3Nb4/3O7基高储能薄膜电容器的储能密度约为30.4J/cm3。
实施例4
1.将Pt靶材、Bi2Mg2/3Nb4/3O7靶材装入磁控溅射腔体内，靶材与衬底的距离为40mm。
2.然后，先后用无水乙醇和去离子水超声清洗硅衬底，并用高纯氮气吹干，放入磁控溅射样品台上。
3.步骤2完成后，使用掩膜版覆盖部分Pt层，将磁控溅射***的本底真空度抽至5.0×10-4Pa。通入高纯(99.99％)Ar气体。进行沉积得到300nm的Pt层。
4.步骤3结束后，将磁控溅射***的本底真空度抽至5.0×10-4Pa，通入高纯Ar和O2。溅射功率为200W，氧氩比为1：4，温度为室温。进行沉积得到150nm厚的Bi2Mg2/3Nb4/3O7薄膜。由此得到结构为Si/Pt/Bi2Mg2/3Nb4/3O7的样品。
5.待步骤4完成后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品放入退火炉中在500℃下空气退火30min。
6.步骤5结束后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品转移至热蒸镀设备蒸发室内的样品台上，其上覆盖金属掩膜版，将待蒸发Au放置在蒸发舟内。将热蒸镀设备的本底真空抽至5.0×10-3Pa，将电流从80A逐渐升至110A，待Au蒸镀完全后关闭蒸发电源。
实施例4中制备在硅衬底上的无铅Bi2Mg2/3Nb4/3O7基高储能薄膜电容器的储能密度约为33.2J/cm3。
本发明并不局限于实施例中所描述的技术，它的描述是说明性的，并非限制性的。本发明的权限由权利要求所限定，基于本技术领域人员依据本发明所能够变化、重组等方法得到的与本发明相关的技术，都在本发明的保护范围之内。
Claims (10)
1.一种高储能密度电容器，其特征在于，由以下方法制备得到：
(1)将Pt靶材、Bi2Mg2/3Nb4/3O7靶材装入磁控溅射腔体内；
(2)将硅基片放置在磁控溅射腔体的样品台上；
(3)待步骤(2)完成后，将磁控溅射***的本底真空度抽至3.0×10-3Pa以下，使用纯Ar气体溅射Pt层；
(4)待步骤(3)完成后，使用掩膜版覆盖部分Pt层，然后将磁控溅射***的本底真空度抽至1.0×10-3Pa以下，使用Ar和O2混合气体作为溅射气体，溅射功率为50～300W，进行沉积得到Bi2Mg2/3Nb4/3O7层；由此得到结构为Si/Pt/Bi2Mg2/3Nb4/3O7的样品；
(5)待步骤(4)完成后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品放入退火炉中空气退火10min～30min，退火温度为500℃～750℃；
(6)步骤(5)完成后，将Bi2Mg2/3Nb4/3O7层上覆盖金属掩膜版，使用热蒸镀设备制备Au顶电极，最终得到Pt金属底电极/Bi2Mg2/3Nb4/3O7层/Au金属顶电极三层结构的无铅Bi2Mg2/ 3Nb4/3O7基储能电容器。
2.根据权利要求1所述高储能密度电容器，其特征在于，所述步骤(1)Pt靶材为任意市售或者自制靶材，纯度为99％以上；Bi2Mg2/3Nb4/3O7靶材为常规的固相烧结法自制而成，靶材的纯度为98％以上；靶材与衬底的距离优选为40mm～150mm。
3.根据权利要求1所述高储能密度电容器，其特征在于，所述步骤(3)Ar气体纯度在99.99％以上；Pt层厚度为30nm～300nm。
4.根据权利要求1所述高储能密度电容器，其特征在于，所述步骤(4)Ar和O2的纯度均在99.99％以上，氧氩比为1/50～2/3；溅射总气压0.3～15Pa，Bi2Mg2/3Nb4/3O7层的厚度可以通过调节制备工艺参数或沉积时间控制，厚度为20nm～200nm。
5.根据权利要求1所述高储能密度电容器，其特征在于，所述步骤(5)将热蒸镀设备的本底真空抽至9.0×10-4Pa以下，将电流控制在80～130A，待Au蒸镀完全后关闭蒸发电源。
6.一种高储能密度电容器的制备方法，其特征在于，包括以下步骤：
(1)将Pt靶材、Bi2Mg2/3Nb4/3O7靶材装入磁控溅射腔体内；
(3)将硅基片放置在磁控溅射腔体的样品台上；
(3)待步骤(2)完成后，将磁控溅射***的本底真空度抽至3.0×10-3Pa以下，使用纯Ar气体溅射Pt层；
(4)待步骤(3)完成后，使用掩膜版覆盖部分Pt层，然后将磁控溅射***的本底真空度抽至1.0×10-3Pa以下，使用Ar和O2混合气体作为溅射气体，溅射功率为50～300W，进行沉积得到Bi2Mg2/3Nb4/3O7层；由此得到结构为Si/Pt/Bi2Mg2/3Nb4/3O7的样品；
(5)待步骤(4)完成后，将Si/Pt/Bi2Mg2/3Nb4/3O7样品放入退火炉中空气退火10min～30min，退火温度为500℃～750℃；
(6)步骤(5)完成后，将Bi2Mg2/3Nb4/3O7层上覆盖金属掩膜版，使用热蒸镀设备制备Au顶电极，最终得到Pt金属底电极/Bi2Mg2/3Nb4/3O7层/Au金属顶电极三层结构的无铅Bi2Mg2/ 3Nb4/3O7基储能电容器。
7.根据权利要求6所述高储能密度电容器的制备方法，其特征在于，所述步骤(1)Pt靶材为任意市售或者自制靶材，纯度为99％以上；Bi2Mg2/3Nb4/3O7靶材为常规的固相烧结法自制而成，靶材的纯度为98％以上；靶材与衬底的距离优选为40mm～150mm。
8.根据权利要求6所述高储能密度电容器的制备方法，其特征在于，所述步骤(3)Ar气体纯度在99.99％以上；Pt层厚度为30nm～300nm。
9.根据权利要求6所述高储能密度电容器的制备方法，其特征在于，所述步骤(4)Ar和O2的纯度均在99.99％以上，氧氩比为1/50～2/3；溅射总气压0.3～15Pa，Bi2Mg2/3Nb4/3O7层的厚度可以通过调节制备工艺参数或沉积时间控制，厚度为20nm～200nm。
10.根据权利要求6所述高储能密度电容器的制备方法，其特征在于，所述步骤(5)将热蒸镀设备的本底真空抽至9.0×10-4Pa以下，将电流控制在80～130A，待Au蒸镀完全后关闭蒸发电源。
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