CN111302789A - 一种具有三明治结构的脉冲储能介质材料及其制备方法与应用 - Google Patents

一种具有三明治结构的脉冲储能介质材料及其制备方法与应用 Download PDF

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CN111302789A
CN111302789A CN202010185763.3A CN202010185763A CN111302789A CN 111302789 A CN111302789 A CN 111302789A CN 202010185763 A CN202010185763 A CN 202010185763A CN 111302789 A CN111302789 A CN 111302789A
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powder
energy storage
dielectric material
glass
sandwich structure
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CN111302789B (zh
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吕明
李儒强
魏雅妮
赖秋坛
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

本发明公开了一种具有三明治结构的脉冲储能介质材料及其制备方法与应用。本发明采用三明治结构并结合陶瓷与玻璃的材料特性制备高性能的脉冲储能介质材料，其中陶瓷介质为BaxSr1‑xTiO3包裹SiO2的核壳结构粉体，玻璃材料为无碱玻璃AF45，其化学成分为63％SiO2‑12％BaO‑16％B2O3‑9％Al2O3。本发明通过将AF45无碱玻璃浆料旋涂在陶瓷正反面，烧制后得到玻璃‑陶瓷‑玻璃的层状结构材料。经过本发明的介质材料制备工艺简单、技术成熟，适用于工业化生产，其电场强度均在420kV/cm，放电能量密度达到2.50J/cm3以上，储能效率能够达到85％以上，能够表现出优良的脉冲储能性能。

Description

一种具有三明治结构的脉冲储能介质材料及其制备方法与 应用
技术领域
本发明属于脉冲储能陶瓷领域，具体涉及一种具有三明治结构的脉冲储能介质材料及其制备方法与应用。
背景技术
高储能密度电介质具有高能量密度和高效率密度，可用于开发高容量电容器,在脉冲效率技术、效率电子电路、电动汽车、电网效率调节等方向有巨大的应用潜力。与电池和其他能量存储装置相比，陶瓷电容器具有快速充放电和高的温度稳定性的优点。但是，目前现有的大多数无铅储能陶瓷介质材料存在着击穿强度不够高或者极化强度较小，导致储能密度不高，难以满足新技术不断发展的需求。通常情况下，材料的储能密度是指单位体积材料能容纳的电能，目前国际上普遍使用的单位是J/cm3，储能密度可用公式来计算
Figure BDA0002414122800000011
式中J是储能密度，E是电场强度，P极化强度，ε是介电常数。由上式可知，要获得较高的储能密度，提高陶瓷介质材料的电场强度和相对介电常数是有效的途径
钛酸钡因具有较高的介电常数而引起人们的广泛关注。然而钛酸钡陶瓷材料的介电损耗在高频下较高，其较高的介电损耗值和较差的击穿性能使得制备出的元器件难以满足脉冲储能电容器在实际应用中的需求。钛酸锶在室温下是立方结构，呈现出顺电相，具有较小的介电损耗和较高的耐压强度，并且频率稳定性好，是目前研究最广泛、最具有吸引力的无铅储能介质陶瓷体系之一。但是钛酸锶陶瓷的介电常数较小，在室温下约为300。因此，要拓宽陶瓷介质在储能领域的应用,需要对其进行改性研究。
目前，无铅储能陶瓷介质材料的电场强度、储能密度和储能效率有待提高。
发明内容
为解决现有技术的缺点和不足之处，本发明的首要目的在于提供一种具有三明治结构的脉冲储能介质材料的制备方法。通过设计三明治结构并结合陶瓷材料与玻璃材料的特性，使得该介质材料具有优良的电场强度、储能密度及能量效率。电场强度达到400kV/cm以上，储能密度可达到3.0J/cm3，能量效率可达到86％，同时制备过程中使用的旋涂工艺技术完善，所需要的原材料价格廉价，具有高性能的同时兼具工艺简单等特性。
本发明的另一目的在于提供上述方法制得的一种具有三明治结构的脉冲储能介质材料。
本发明的再一目的在于提供上述一种具有三明治结构的脉冲储能介质材料的应用。
本发明目的通过以下技术方案实现：
一种具有三明治结构的脉冲储能介质材料的制备方法，包括以下步骤：
(1)将BaxSr1-xTiO3粉体分散于乙醇中，加入冰乙酸和聚乙烯吡咯烷酮(PVP)，混合均匀后，加入正硅酸乙酯，调节pH，于30-60℃下搅拌反应12-24小时，得到悬浮液，过滤，干燥，得到BST@SiO2粉体；
其中x表示Ba的摩尔分数，0.2≤x≤0.6；
(2)将BST@SiO2粉体与粘结剂混合均匀，在150-200MPa下成型，排胶，最后在1100-1200℃下烧制成陶瓷块体；
(3)将氧化硅、氧化钡、氧化硼与氧化铝混合，球磨均匀后，过筛，干燥，于1400-1500℃下熔制2-4小时，淬冷，得到熔块；向熔块中加入水后再次球磨，干燥，得到AF45玻璃；其中AF45玻璃的化学组成摩尔含量为63％SiO2-12％BaO-16％B2O3-9％Al2O3；
(4)将AF45玻璃和羧甲基纤维素加入到水中，得到AF45玻璃浆料；将其旋涂在陶瓷块体的正反两面上，干燥后进行烧制，得到玻璃-陶瓷-玻璃的三明治结构材料。
优选的，步骤(1)所述BaxSr1-xTiO3粉体由以下方法制备得到：
将摩尔比为x：(1-x)：1的碳酸钡、碳酸锶和氧化钛混合均匀，加入氯化钠混合均匀并球磨，过筛，干燥，然后在1000-1200℃下烧制2-4小时，过滤，干燥，得到BaxSr1-xTiO3粉体；其中氯化钠占碳酸钡、碳酸锶和氧化钛总质量的5-15倍。
所述球磨以无水乙醇为介质，其中无水乙醇的加入量占碳酸钡、碳酸锶和氧化钛总质量的1-2倍。
所述过滤指用去离子水过滤；所述球磨的条件为：在400-500r/min条件下球磨4-8小时；所述过筛的目数为100-200目；所述干燥的条件均为：80-100℃下干燥12-24小时。
优选的，步骤(1)所述乙醇的质量为BaxSr1-xTiO3粉体的100-200倍；所述冰乙酸的质量为BaxSr1-xTiO3粉体的4-6倍；所述聚乙烯吡咯烷酮的质量为BaxSr1-xTiO3粉体的50-100％；所述正硅酸乙酯的质量为BaxSr1-xTiO3粉体的2-8％。
优选的，步骤(1)所述调节pH指通过氨水将体系的pH调节至9-11。
优选的，步骤(1)所述过滤指用去离子水和乙醇进行过滤；所述干燥的条件为：在80-100℃下干燥12-24小时。
步骤(1)所述BST@SiO2粉体为BaxSr1-xTiO3包裹SiO2的核壳结构粉体。
优选的，步骤(2)所述粘结剂为聚乙烯醇(PVA)；所述粘结剂的质量为BST@SiO2粉体的1-3％。
优选的，步骤(2)所述排胶条件为：500-600℃下保温4-8小时。
优选的，步骤(2)所述烧制的时间为2-4小时。
优选的，步骤(3)所述氧化硅、氧化钡、氧化硼与氧化铝球磨均匀的条件为：以无水乙醇为介质，在400-500r/min条件下球磨4-8小时，其中无水乙醇的重量为氧化硅、氧化钡、氧化硼与氧化铝总质量的1-2倍。
优选的，步骤(3)所述向熔块中加入水后再次球磨的条件为：400-500r/min球磨4-8小时。
优选的，步骤(3)所述过筛的目数为100-200目。
优选的，步骤(3)所述干燥的条件均为：80-100℃下干燥12-24小时。
优选的，步骤(4)所述羧甲基纤维素(CMC)的质量为AF45玻璃的1-2％。
优选的，步骤(4)所述AF45玻璃浆料的密度为1-1.5g/cm3。
优选的，步骤(4)所述旋涂的条件为：转速为100-200rpm，时间为10-30s。
优选的，步骤(4)所述干燥的条件为：80-100℃下干燥12-24小时。
优选的，步骤(4)所述烧制的条件为：800-1000℃下烧制10-30min。
上述方法制得的一种具有三明治结构的脉冲储能介质材料，其陶瓷介质的化学式为BaxSr1-xTiO3，其中x为Ba的摩尔分数，且0.2≤x≤0.6。
所述具有三明治结构的脉冲储能介质材料的电场强度均在420kV/cm以上，放电能量密度达到2.50J/cm3以上，储能效率能够达到85％以上。
上述一种具有三明治结构的脉冲储能介质材料的应用。
与现有技术相比，本发明具有以下优点及有益效果：
本发明通过设计三明治结构并结合陶瓷材料与玻璃材料的特性，将玻璃浆料旋涂于陶瓷块体上，然后对其进行热处理，即可得到具有三明治结构的高能量密度及能量效率的脉冲储能介质材料。本发明的具有三明治结构的高能量密度及能量效率的脉冲储能介质材料的制备工艺简单、性能优异、稳定性好，电场强度均在400kV/cm以上，放电能量密度能够达到3.00J/cm3，储能效率能够达到86％以上，可满足不同应用的需求，无铅无污染，所涉及的价格便宜，技术工艺成熟，适合工业化生产。
附图说明
图1为本发明所述具有三明治结构的脉冲储能介质材料的结构示意图。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
本发明实施例中未注明具体条件者，按照常规条件或者制造商建议的条件进行。所用未注明生产厂商者的原料、试剂等，均为可以通过市售购买获得的常规产品。
实施例1
本实施例的介质材料的化学式为AF45/BaxSr1-xTiO3/AF45，其中x表示Ba的摩尔分数，且x＝0.20。
(1)BST粉体的制备：通过熔盐法，按照BST的化学式对分析纯的碳酸钡、碳酸锶和氧化钛进行配料并混合均匀，加入氯化钠(加入量为碳酸钡、碳酸锶和氧化钛总重量的5倍)，以无水乙醇(加入量为碳酸钡、碳酸锶和氧化钛总重量的1倍)为介质，通过400r/min速率进行球磨4小时，且将浆料过100目的筛网，在80℃下干燥12小时，然后装入刚玉坩埚中于1000℃下烧制2小时，得到粉料后用去离子水过滤，于80℃下干燥12小时后得到纯净的BST(BaxSr1-xTiO3)粉体。
(2)BST@SiO2粉体的制备：将(1)中得到的BaxSr1-xTiO3粉体溶解于乙醇(乙醇重量为BaxSr1-xTiO3粉体的100倍)中，超声分散后加入冰乙酸(冰乙酸重量为BaxSr1-xTiO3粉体的4倍)和聚乙烯吡咯烷酮(PVP重量为BaxSr1-xTiO3粉体的50％)，搅拌并超声分散均匀后加入正硅酸乙酯(正硅酸乙酯的重量为BaxSr1-xTiO3粉体的2％)，通过氨水调节pH＝9，最后于30℃的水浴搅拌锅中温和搅拌12小时。然后将获得的悬浮液用去离子水和乙醇过滤，于90℃下干燥12小时后得到BST@SiO2粉体。
将干燥后的BST@SiO2粉体加入粘结剂PVA(PVA重量为BaxSr1-xTiO3粉体的1％)进行造粒，150MPa压力成型，于500℃下保温4小时排胶，最后在1100℃下保温2小时成陶瓷块体。
(3)AF45玻璃材料是通过熔块法将摩尔百分含量为63％SiO2-12％BaO-16％B2O3-9％Al2O3原料以无水乙醇(无水乙醇的重量为氧化硅、氧化钡、氧化硼与氧化铝总质量的1倍)为介质，通过400r/min速率进行球磨4小时，且将浆料过100目的筛网，在80℃下干燥12小时后，置于刚玉坩埚中于1400℃的马弗炉中2小时，淬冷后将玻璃熔块于400r/min下球磨4小时，于80℃下干燥16小时后得到玻璃粉体。
(4)将玻璃粉体加入去离子水与羧甲基纤维素(羧甲基纤维素质量为AF45玻璃的1％)调节密度为1g/cm3的玻璃浆料并以转速为100rpm，保持时间为10s，均匀旋涂于陶瓷块体正反面后，于马弗炉热处理，温度为800℃，保温时间为10min，得到介质材料AF45/BaxSr1-xTiO3/AF45。
(5)将烧结好的样品的两个表面打磨干净并镀金电极，然后在室温和10Hz的频率下测试其铁电性能，并根据储能特性计算其充电能量密度、放电能量密度和储能效率。
本实施例所得具有三明治结构的介质材料的电场强度为425kV/cm，充电能量密度为3.12J/cm3，放电能量密度为2.79J/cm3，储能效率为87％。
本实施例的具有三明治结构的高能量密度及能量效率的脉冲储能介质材料的结构示意图参见图1。
实施例2
本实施例的介质材料的化学式为AF45/BaxSr1-xTiO3/AF45，其中x表示Ba的摩尔分数，且x＝0.30。
(1)BST粉体的制备：通过熔盐法，按照BST的化学式对分析纯的碳酸钡、碳酸锶和氧化钛进行配料并混合均匀，加入氯化钠(加入量为碳酸钡、碳酸锶和氧化钛总重量的15倍)，以无水乙醇(加入量为碳酸钡、碳酸锶和氧化钛总重量的2倍)为介质，在500r/min条件下球磨8小时，且将浆料过200目的筛网，在100℃下干燥24小时，然后装入刚玉坩埚中于1200℃下烧制4小时，得到粉料后用去离子水过滤，于90℃下干燥24小时后得到纯净的BST(BaxSr1-xTiO3)粉体。
(2)BST@SiO2粉体的制备：将(1)中得到的BaxSr1-xTiO3粉体溶解于乙醇(乙醇重量为BaxSr1-xTiO3粉体的200倍)中，超声分散后加入冰乙酸(冰乙酸重量为BaxSr1-xTiO3粉体的6倍)和聚乙烯吡咯烷酮(PVP重量为BaxSr1-xTiO3粉体的100％)，搅拌并超声分散均匀后加入正硅酸乙酯(正硅酸乙酯的重量为BaxSr1-xTiO3粉体的8％)，通过氨水调节PH＝11，最后于60℃的水浴搅拌锅中温和搅拌24小时。然后将获得的悬浮液用去离子水和乙醇过滤，于80℃下干燥12小时后得到BST@SiO2粉体。
将干燥后的BST@SiO2粉体加入粘结剂PVA(PVA重量为BaxSr1-xTiO3粉体的3％)进行造粒，200MPa压力成型，于600℃下保温8小时排胶，最后在1200℃下保温2小时成陶瓷块体。
(3)AF45玻璃材料是通过熔块法将摩尔百分含量为63％SiO2-12％BaO-16％B2O3-9％Al2O3原料以无水乙醇(无水乙醇的重量为氧化硅、氧化钡、氧化硼与氧化铝总质量的1.5倍)为介质，在500r/min条件下球磨8小时，且将浆料过200目的筛网，在100℃下干燥24小时后，置于刚玉坩埚中于1500℃的马弗炉中4小时，淬冷后将玻璃熔块以500r/min球磨8小时，于100℃下干燥24小时后得到玻璃粉体。
(4)将玻璃粉体加入去离子水与羧甲基纤维素(羧甲基纤维素质量为AF45玻璃的1％)调节密度为1.5g/cm3的玻璃浆料并以转速为200rpm，保持时间为30s，均匀旋涂于陶瓷块体正反面后，于马弗炉热处理，温度为1000℃，保温时间为30min，得到介质材料AF45/BaxSr1-xTiO3/AF45。
(5)将烧结好的样品的两个表面打磨干净并镀金电极，然后在室温和10Hz的频率下测试其铁电性能，并根据储能特性计算其充电能量密度、放电能量密度和储能效率。
本实施例所得具有三明治结构的介质材料的电场强度为435kV/cm，充电能量密度为3.00J/cm3，放电能量密度为2.73J/cm3，储能效率为88％。
本实施例的具有三明治结构的高能量密度及能量效率的脉冲储能介质材料的结构示意图参见图1。
实施例3
本实施例的介质材料的化学式为AF45/BaxSr1-xTiO3/AF45，其中x表示Ba的摩尔分数，且x＝0.60。
(1)BST粉体的制备：通过熔盐法，按照BST的化学式对分析纯的碳酸钡、碳酸锶和氧化钛进行配料并混合均匀，加入氯化钠(加入量为碳酸钡、碳酸锶和氧化钛总重量的9倍)，以无水乙醇(加入量为碳酸钡、碳酸锶和氧化钛总重量的1.5倍)为介质，在450r/min条件下球磨5小时，且将浆料过150目的筛网，在85℃下干燥20小时，然后装入刚玉坩埚中于1120℃下烧制3小时，得到粉料后用去离子水过滤，于85℃下干燥18小时后得到纯净的BST(BaxSr1-xTiO3)粉体。
(2)BST@SiO2粉体的制备：将(1)中得到的BaxSr1-xTiO3粉体溶解于乙醇(乙醇重量为BaxSr1-xTiO3粉体的150倍)中，超声分散后加入冰乙酸(冰乙酸重量为BaxSr1-xTiO3粉体的5倍)和聚乙烯吡咯烷酮(PVP重量为BaxSr1-xTiO3粉体的75％)，搅拌并超声分散均匀后加入正硅酸乙酯(正硅酸乙酯的重量为BaxSr1-xTiO3粉体的6％)，通过氨水调节PH＝9.5，最后于45℃的水浴搅拌锅中温和搅拌20小时。然后将获得的悬浮液用去离子水和乙醇过滤，于100℃下干燥18小时后得到BST@SiO2粉体。
将干燥后的BST@SiO2粉体加入粘结剂PVA(PVA重量为BaxSr1-xTiO3粉体的1.5％)进行造粒，150MPa压力成型，于550℃下保温6小时排胶，最后在1120℃下保温3小时成陶瓷块体。
(3)AF45玻璃材料是通过熔块法将摩尔百分含量为63％SiO2-12％BaO-16％B2O3-9％Al2O3原料以无水乙醇(无水乙醇的重量为氧化硅、氧化钡、氧化硼与氧化铝总质量的1.5倍)为介质，在450r/min条件下球磨5小时，且将浆料过150目的筛网，在85℃下干燥20小时后，置于刚玉坩埚中于1450℃的马弗炉中3小时，淬冷后将玻璃熔块以450r/min球磨6小时，于85℃下干燥14小时后备用。
(4)将玻璃粉体加入去离子水与羧甲基纤维素(羧甲基纤维素质量为AF45玻璃的1％)调节密度为1.2g/cm3玻璃浆料并以转速为160rpm，保持时间为15s，均匀旋涂于陶瓷块体正反面后，于马弗炉热处理，温度为920℃，保温时间为15min，得到介质材料AF45/BaxSr1-xTiO3/AF45。
(5)将烧结好的样品的两个表面打磨干净并镀金电极，然后在室温和10Hz的频率下测试其铁电性能，并根据储能特性计算其充电能量密度、放电能量密度和储能效率。
本实施例所得具有三明治结构的介质材料的电场强度为420kV/cm，充电能量密度为2.78J/cm3，放电能量密度为2.50J/cm3，储能效率为85％。
本实施例的具有三明治结构的高能量密度及能量效率的脉冲储能介质材料的结构示意图参见图1。
实施例4
本实施例的介质材料的化学式为AF45/BaxSr1-xTiO3/AF45，其中x表示Ba的摩尔分数，且x＝0.40。
(1)BST粉体的制备：通过熔盐法，按照BST的化学式对分析纯的碳酸钡、碳酸锶和氧化钛进行配料并混合均匀，加入氯化钠(加入量为碳酸钡、碳酸锶和氧化钛总重量的10倍)，以无水乙醇(加入量为碳酸钡、碳酸锶和氧化钛总重量的1.6倍)为介质，在500r/min条件下球磨5小时，且将浆料过180目的筛网，在80℃下干燥24小时，然后装入刚玉坩埚中于1050℃下烧制2.5小时，得到粉料后用去离子水过滤，于95℃下干燥20小时后得到纯净的BST(BaxSr1-xTiO3)粉体。
(2)BST@SiO2粉体的制备：将(1)中得到的BaxSr1-xTiO3粉体溶解于乙醇(乙醇重量为BaxSr1-xTiO3粉体的150倍)中，超声分散后加入冰乙酸(冰乙酸重量为BaxSr1-xTiO3粉体的5倍)和聚乙烯吡咯烷酮(PVP重量为BaxSr1-xTiO3粉体的60％)，搅拌并超声分散均匀后加入正硅酸乙酯(正硅酸乙酯的重量为BaxSr1-xTiO3粉体的4％)，通过氨水调节PH＝10，最后于45℃的水浴搅拌锅中温和搅拌18小时。然后将获得的悬浮液用去离子水和乙醇过滤，于95℃下干燥17小时后得到BST@SiO2粉体。
将干燥后的BST@SiO2粉体加入粘结剂PVA(PVA重量为BaxSr1-xTiO3粉体的2.5％)进行造粒，200MPa压力成型，于600℃下保温5小时排胶，最后在1150℃下烧制保温3小时得到陶瓷块体。
(3)AF45玻璃材料是通过熔块法将摩尔百分含量为63％SiO2-12％BaO-16％B2O3-9％Al2O3原料以无水乙醇(无水乙醇的重量为氧化硅、氧化钡、氧化硼与氧化铝总质量的1.4倍)为介质，在500r/min条件下球磨5小时，且将浆料过180目的筛网，在80℃下干燥24小时后，置于刚玉坩埚中于1480℃的马弗炉中2.5小时，淬冷后将玻璃熔块以450r/min球磨6小时，于95℃下干燥20小时后备用。
(4)将玻璃粉体加入去离子水与羧甲基纤维素(羧甲基纤维素质量为AF45玻璃的1％)调节密度为1.2g/cm3的玻璃浆料并以转速为180rpm，保持时间为20s，均匀旋涂于陶瓷块体正反面后，于马弗炉热处理，温度为900℃，保温时间为15min，得到介质材料AF45/BaxSr1-xTiO3/AF45。
(5)将烧结好的样品的两个表面打磨干净并镀金电极，然后在室温和10Hz的频率下测试其铁电性能，并根据储能特性计算其充电能量密度、放电能量密度和储能效率。
本实施例所得具有三明治结构的介质材料的电场强度为450kV/cm，充电能量密度为3.21J/cm3，放电能量密度为2.83J/cm3，储能效率为89％。
本实施例的具有三明治结构的高能量密度及能量效率的脉冲储能介质材料的结构示意图参见图1。
对比例1
本对比例的介质材料的化学式为BaxSr1-xTiO3，其中x表示Ba的摩尔分数，且x＝0.4。
(1)BST粉体的制备：通过熔盐法，按照BST的化学式对分析纯的碳酸钡、碳酸锶和氧化钛进行配料并混合均匀，加入氯化钠(加入量为碳酸钡、碳酸锶和氧化钛总重量的10倍)，以无水乙醇(加入量为碳酸钡、碳酸锶和氧化钛总重量的1.6倍)为介质，在500r/min条件下球磨5小时，且将浆料过180目的筛网，在80℃下干燥24小时，然后装入刚玉坩埚中于1050℃下烧制2.5小时，得到粉料后用去离子水过滤，于95℃下干燥20小时后得到纯净的BST(BaxSr1-xTiO3)粉体。
(2)BST@SiO2粉体的制备：将(1)中得到的BaxSr1-xTiO3粉体溶解于乙醇(乙醇重量为BaxSr1-xTiO3粉体的150倍)中，超声分散后加入冰乙酸(冰乙酸重量为BaxSr1-xTiO3粉体的5倍)和聚乙烯吡咯烷酮(PVP重量为BaxSr1-xTiO3粉体的60％)，搅拌并超声分散均匀后加入正硅酸乙酯(正硅酸乙酯的重量为BaxSr1-xTiO3粉体的4％)，通过氨水调节PH＝10，最后于45℃的水浴搅拌锅中温和搅拌18小时。然后将获得的悬浮液用去离子水和乙醇过滤，于95℃下干燥17小时后得到BST@SiO2粉体。
将干燥后的BST@SiO2粉体加入粘结剂PVA(PVA重量为BaxSr1-xTiO3粉体的2.5％)进行造粒，200MPa压力成型，于600℃下保温5小时排胶，最后在1150℃下保温3小时得到陶瓷块体。
(3)将烧结好的样品的两个表面打磨干净并镀金电极，然后在室温和10Hz的频率下测试其铁电性能，并根据储能特性计算其充电能量密度、放电能量密度和储能效率。
本实施例所得具有三明治结构的介质材料的电场强度为320kV/cm，充电能量密度为2.10J/cm3，放电能量密度为2.32J/cm3，储能效率为81％。
对比例2
本对比例的介质材料的化学式为BaxSr1-xTiO3，其中x表示Ba的摩尔分数，且x＝0.4。
(1)BST粉体的制备：通过熔盐法，按照BST的化学式对分析纯的碳酸钡、碳酸锶和氧化钛进行配料并混合均匀，加入氯化钠(加入量为碳酸钡、碳酸锶和氧化钛总重量的10倍)，以无水乙醇(加入量为碳酸钡、碳酸锶和氧化钛总重量的1.6倍)为介质，在500r/min条件下球磨5小时，且将浆料过180目的筛网，在80℃下干燥24小时，然后装入刚玉坩埚中于1050℃下烧制2.5小时，得到粉料后用去离子水过滤，于95℃下干燥20小时后得到纯净的BST(BaxSr1-xTiO3)粉体。
(2)将干燥后的BST粉体加入粘结剂PVA(PVA重量为BaxSr1-xTiO3粉体的2.5％)进行造粒，200MPa压力成型，于600℃下保温5小时排胶，最后在1150℃下保温3小时得到陶瓷块体。
(3)将烧结好的样品的两个表面打磨干净并镀金电极，然后在室温和10Hz的频率下测试其铁电性能，并根据储能特性计算其充电能量密度、放电能量密度和储能效率。
本实施例所得具有三明治结构的介质材料的电场强度为280kV/cm，充电能量密度为1.79J/cm3，放电能量密度为1.65J/cm3，储能效率为85％。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

1.一种具有三明治结构的脉冲储能介质材料的制备方法，其特征在于，包括以下步骤：
(1)将BaxSr1-xTiO3粉体分散于乙醇中，加入冰乙酸和聚乙烯吡咯烷酮，混合均匀后，加入正硅酸乙酯，调节pH，于30-60℃下搅拌反应12-24小时，得到悬浮液，过滤，干燥，得到BST@SiO2粉体；
其中x表示Ba的摩尔分数，0.2≤x≤0.6；
(2)将BST@SiO2粉体与粘结剂混合均匀，在150-200MPa下成型，排胶，最后在1100-1200℃下烧制成陶瓷块体；
(3)将氧化硅、氧化钡、氧化硼与氧化铝混合，球磨均匀后，过筛，干燥，于1400-1500℃下熔制2-4小时，淬冷，得到熔块；向熔块中加入水后再次球磨，干燥，得到AF45玻璃；其中AF45玻璃的化学组成摩尔含量为63％SiO2-12％BaO-16％B2O3-9％Al2O3；
(4)将AF45玻璃和羧甲基纤维素加入到水中，得到AF45玻璃浆料；将其旋涂在陶瓷块体的正反两面上，干燥后进行烧制，得到玻璃-陶瓷-玻璃的三明治结构材料。
2.根据权利要求1所述一种具有三明治结构的脉冲储能介质材料的制备方法，其特征在于，步骤(1)所述乙醇的质量为BaxSr1-xTiO3粉体的100-200倍；所述冰乙酸的质量为BaxSr1-xTiO3粉体的4-6倍；所述聚乙烯吡咯烷酮的质量为BaxSr1-xTiO3粉体的50-100％；所述正硅酸乙酯的质量为BaxSr1-xTiO3粉体的2-8％。
3.根据权利要求1或2所述一种具有三明治结构的脉冲储能介质材料的制备方法，其特征在于，步骤(4)所述烧制的条件为：800-1000℃下烧制10-30min。
4.根据权利要求1或2所述一种具有三明治结构的脉冲储能介质材料的制备方法，其特征在于，步骤(1)所述调节pH指通过氨水将体系的pH调节至9-11；步骤(2)所述烧制的时间为2-4小时。
5.根据权利要求1或2所述一种具有三明治结构的脉冲储能介质材料的制备方法，其特征在于，步骤(2)所述粘结剂为PVA；所述粘结剂的质量为BST@SiO2粉体的1-3％；所述排胶条件为：500-600℃下保温4-8小时。
6.根据权利要求1或2所述一种具有三明治结构的脉冲储能介质材料的制备方法，其特征在于，步骤(1)所述BaxSr1-xTiO3粉体由以下方法制备得到：
将摩尔比为x：(1-x)：1的碳酸钡、碳酸锶和氧化钛混合均匀，加入氯化钠混合均匀并球磨，过筛，干燥，然后在1000-1200℃下烧制2-4小时，过滤，干燥，得到BaxSr1-xTiO3粉体；其中氯化钠占碳酸钡、碳酸锶和氧化钛总质量的5-15倍；
所述球磨以无水乙醇为介质，其中无水乙醇的加入量占碳酸钡、碳酸锶和氧化钛总质量的1-2倍；所述球磨的条件为：在400-500r/min条件下球磨4-8小时；所述过筛的目数为100-200目。
7.根据权利要求1或2所述一种具有三明治结构的脉冲储能介质材料的制备方法，其特征在于，步骤(4)所述AF45玻璃浆料中AF45玻璃的密度为1-1.5g/cm3；所述旋涂的条件为：转速为100-200rpm，持续时间为10-30s；所述羧甲基纤维素的质量为AF45玻璃的1-2％。
8.根据权利要求1或2所述一种具有三明治结构的脉冲储能介质材料的制备方法，其特征在于，步骤(3)所述氧化硅、氧化钡、氧化硼与氧化铝球磨均匀的条件为：以无水乙醇为介质，在400-500r/min条件下球磨4-8小时，其中无水乙醇的重量为氧化硅、氧化钡、氧化硼与氧化铝总质量的1-2倍；所述向熔块中加入水后再次球磨的条件为：400-500r/min球磨4-8小时；所述过筛的目数为100-200目。
9.权利要求1～8任一项所述方法制得的一种具有三明治结构的脉冲储能介质材料。
10.权利要求9所述一种具有三明治结构的脉冲储能介质材料的应用。
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