CN112062553B - 一种超宽温区负电卡效应Pb(ZrxTi1-x)O3基薄膜的制备方法 - Google Patents
一种超宽温区负电卡效应Pb(ZrxTi1-x)O3基薄膜的制备方法 Download PDFInfo
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Abstract
本发明涉及一种通过衬底调控Pb(ZrXTi1‑X)O3薄膜电卡性能的制备方法，属于化学工程技术领域。一种超宽温区负电卡效应Pb(ZrXTi1‑X)O3基薄膜的制备方法，是将Pb(ZrXTi1‑X)O3前驱体溶液旋涂于衬底上制得湿膜；产品干燥、热解，退火制得单层Pb(ZrXTi1‑X)O3薄膜；重复前面步骤，制得多层Pb(ZrXTi1‑X)O3薄膜。本发明的有益效果是：获得具有纯度高、致密性好、平均晶粒尺寸小、电场击穿强度大、可调控温区宽、电卡效应大等优点的薄膜；本发明制备方法相对简单，是一种方便快捷的制备技术。
Description
技术领域
本发明涉及一种通过衬底调控Pb(ZrXTi1-X)O3薄膜电卡性能的制备方法，属于化学工程技术领域。
背景技术
在市场迅猛增长、国际竞争日趋激烈、节能和环保迫切要求的背景之下，现代制冷技术取得了突飞猛进的发展与进步。然而，目前市面上主流的制冷技术是气体压缩制冷，但这一制冷技术对环境污染非常严重；其次作为人类研究已久的磁卡制冷技术，由于其工作物质大多是稀土合金且耗能较大，使用过程中容易吸附水汽或者被氧化从而限制了其进一步的推广与应用；再者就是太阳能吸附式制冷技术，该技术主要是利用吸附剂中制冷剂的物态变化来实现制冷，但相较于其他制冷技术而言，太阳能吸附制冷技术由于其制冷效率过低而难以实现大规模的商业化应用；最后是利用热电材料中的帕尔贴效应实现的热电制冷技术，虽然热电制冷也具备环保、反应快、可控的优点，但同样由于其效率太低、成本也相对较高因而也无法满足商业化的要求。
近几年来，电卡制冷技术由于具有的无噪音、无震动且高效节能的制冷特点备受各国科研人员的广泛关注。电卡制冷主要是利用一种新型的物理效应，即铁电材料的电卡效应(EC)，在绝热条件下对铁电体施加(去除)电场使其发生温度的变化。用铁电材料所制备的固体制冷机无需外加压缩机并且极利于小型化，同时能为小型电子产品如CPU等制冷，使其作为一种新型绿色节能的制冷技术为新形势下多种致冷需求带来了巨大的应用前景，因此发展研究铁电致冷技术在能源资源短缺、环境污染严峻、温室效应突出的今天具有突出的现实意义。
发明内容
本发明的目的在于提供一种超宽温区负电卡效应Pb(ZrXTi1-X)O3基薄膜的制备方法。
本发明的目的通过如下技术方案实现：
一种超宽温区负电卡效应Pb(ZrXTi1-X)O3基薄膜的制备方法，包括以下步骤：
1)将Pb(ZrXTi1-X)O3前驱体溶液旋涂于衬底上制得湿膜，所述 Pb(ZrXTi1-X)O3通式中x＝0.1～0.5；
2)将步骤1)所得产品干燥、热解，退火制得单层Pb(ZrXTi1-X)O3薄膜，所述干燥温度为350-400℃，干燥时间为5-10min；
3)重复步骤1)和步骤2)，制得多层Pb(ZrXTi1-X)O3薄膜。
优选的是，步骤1)所述Pb(ZrXTi1-X)O3前驱体溶液由如下方法制得：将原料Pb(CH3COO)3于110℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)4和Ti(OCH(CH3)2)4于室温溶解在冰醋酸和CH3COCH2COCH3的混合液体中，将所得的两种混合液于60-100℃搅拌30min再次混合，并放置24-30h，得到浓度为0.3M的Pb(ZrXTi1-X)O3前驱体溶液。
优选的是，步骤1)所述旋涂转速为4000-6000rpm，旋涂时间为30-40s。
优选的是，步骤1)所述衬底为p-type GaN。
优选的是，步骤2)所述热解温度为550-600℃，热解时间为5-10min。
优选的是，步骤2)所述退火温度为700-800℃，退火时间为3-5min，退火环境为空气氛围。
优选的是，步骤3)制得8层Pb(ZrXTi1-X)O3薄膜。
本发明的有益效果是：获得具有纯度高、致密性好、平均晶粒尺寸小、电场击穿强度大、可调控温区宽、电卡效应大等优点的薄膜；本发明制备方法相对简单，是一种方便快捷的制备技术。
附图说明
图1为本发明实施例1得到的Pb(ZrxTi1-x)O3薄膜的电卡性能图谱。
具体实施方式
下面结合具体实施例，对本发明作进一步详细的阐述，但本发明的实施方式并不局限于实施例表示的范围。这些实施例仅用于说明本发明，而非用于限制本发明的范围。此外，在阅读本发明的内容后，本领域的技术人员可以对本发明作各种修改，这些等价变化同样落于本发明所附权利要求书所限定的范围。
实施例1
一种超宽温区负电卡效应薄膜的制备方法，具体为Pb(ZrxTi1-x)O3铁电薄膜，其中x＝0.1，即Pb(Zr0.1Ti0.9)O3铁电薄膜，其制备方法包括如下具体步骤：
(1)按照摩尔比1:0.1:0.9分别称取Pb(CH3COO)3、Zr(OC3H7)4、 Ti(OCH(CH3)2)4，将原料Pb(CH3COO)3于110℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)4、Ti(OCH(CH3)2)4于室温溶解在冰醋酸和 CH3COCH2COCH3的混合液体中，最后将前面两种混合液再次混合于60℃搅拌30min，并放置24h，得到浓度为0.3M的Pb(Zr0.1Ti0.9)O3前驱体溶液；
(2)将步骤(1)得到的Pb(Zr0.1Ti0.9)O3前驱体溶液使用匀胶机以4000rpm 的转速旋涂30s在p-type GaN衬底上，得到湿膜；
(3)将步骤(2)制得的湿膜首先在350℃干燥5min，然后在550℃热解5min，最后在700℃于空气氛围中退火3min。得到一层Pb(Zr0.1Ti0.9)O3薄膜；
(4)重复步骤(2)和步骤(3)8次，得到8层Pb(Zr0.1Ti0.9)O3薄膜。
实施例2
一种超宽温区负电卡效应薄膜的制备方法，具体为Pb(ZrxTi1-x)O3铁电薄膜，其中x＝0.3，即Pb(Zr0.3Ti0.7)O3铁电薄膜，其制备方法包括如下具体步骤：
(1)按照摩尔比1:0.3:0.7分别称取Pb(CH3COO)3、Zr(OC3H7)4、 Ti(OCH(CH3)2)4，将原料Pb(CH3COO)3于110℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)4、Ti(OCH(CH3)2)4于室温溶解在冰醋酸和 CH3COCH2COCH3的混合液体中，最后将前面两种混合液再次混合于70℃搅拌30min，并放置25h，得到浓度为0.3M的Pb(Zr0.3Ti0.7)O3前驱体溶液；
(2)将步骤(1)得到的Pb(Zr0.3Ti0.7)O3前驱体溶液使用匀胶机以5000rpm 的转速旋涂35s在p-type GaN衬底上，得到湿膜；
(3)将步骤(2)制得的湿膜首先在360℃干燥8min，然后在580℃热解8min，最后在750℃于空气氛围中退火4min。得到一层Pb(Zr0.3Ti0.7)O3薄膜；
(4)重复步骤(2)和步骤(3)8次，得到8层Pb(Zr0.3Ti0.7)O3薄膜。
实施例3
一种超宽温区负电卡效应薄膜的制备方法，具体为Pb(ZrxTi1-x)O3铁电薄膜，其中x＝0.5，即Pb(Zr0.5Ti0.5)O3铁电薄膜，其制备方法包括如下具体步骤：
(1)按照摩尔比1:0.5:0.5分别称取Pb(CH3COO)3、Zr(OC3H7)4、 Ti(OCH(CH3)2)4，将原料Pb(CH3COO)3于110℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)4、Ti(OCH(CH3)2)4于室温溶解在冰醋酸和 CH3COCH2COCH3的混合液体中，最后将前面两种混合液再次混合于100℃搅拌30min，并放置30h，得到浓度为0.3M的Pb(Zr0.5Ti0.5)O3前驱体溶液；
(2)将步骤(1)得到的Pb(Zr0.5Ti0.5)O3前驱体溶液使用匀胶机以6000rpm 的转速旋涂40s在p-type GaN衬底上，得到湿膜；
(3)将步骤(2)制得的湿膜首先在400℃干燥10min，然后在600℃热解10min，最后在800℃于空气氛围中退火5min。得到一层Pb(Zr0.5Ti0.5)O3薄膜；
(4)重复步骤(2)和步骤(3)8次，得到8层Pb(Zr0.5Ti0.5)O3薄膜。
本发明制备方法简单，所制得的薄膜性能良好，满足使用要求。
Claims (2)
1.一种超宽温区负电卡效应Pb(ZrXTi1-X)O3基薄膜的制备方法，其特征在于，所述方法包括以下步骤：
1)将Pb(ZrXTi1-X)O3前驱体溶液旋涂于衬底上制得湿膜，所述Pb(ZrXTi1-X)O3通式中x＝0.1～0.5；
2)将步骤1)所得产品干燥、热解，退火制得单层Pb(ZrXTi1-X)O3薄膜，所述干燥温度为350-400℃，干燥时间为5-10min；
3)重复步骤1)和步骤2)，制得多层Pb(ZrXTi1-X)O3薄膜；
步骤1)所述Pb(ZrXTi1-X)O3前驱体溶液由如下方法制得：将原料Pb(CH3COO)3于110℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)4和Ti(OCH(CH3)2)4于室温溶解在冰醋酸和CH3COCH2COCH3的混合液体中，将所得的两种混合液于60-100℃搅拌30min再次混合，并放置24-30h，得到浓度为0.3M的Pb(ZrXTi1-X)O3前驱体溶液；
步骤1)所述衬底为p-type GaN；
步骤2)所述热解温度为550-600℃，热解时间为5-10min；
步骤2)所述退火温度为700-800℃，退火时间为3-5min，退火环境为空气氛围；
步骤3)制得8层Pb(ZrXTi1-X)O3薄膜。
2.根据权利要求1所述的超宽温区负电卡效应Pb(ZrXTi1-X)O3基薄膜的制备方法，其特征在于，步骤1)所述旋涂转速为4000-6000rpm，旋涂时间为30-40s。
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