CN112062562B - 一种knn基超高击穿电场单晶薄膜材料的制备方法 - Google Patents
一种knn基超高击穿电场单晶薄膜材料的制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 16
- 230000015556 catabolic process Effects 0.000 title claims abstract description 14
- 230000005684 electric field Effects 0.000 title claims abstract description 14
- 239000010409 thin film Substances 0.000 title claims abstract description 13
- 239000013078 crystal Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000010408 film Substances 0.000 claims abstract description 39
- 239000002243 precursor Substances 0.000 claims abstract description 26
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- 229910009112 xH2O Inorganic materials 0.000 claims description 22
- 238000004528 spin coating Methods 0.000 claims description 15
- 229960000583 acetic acid Drugs 0.000 claims description 12
- 239000012362 glacial acetic acid Substances 0.000 claims description 12
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 229910002367 SrTiO Inorganic materials 0.000 abstract description 3
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 229910002371 SrTiO3(110) Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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Abstract
本发明涉及一种KNN基超高击穿电场单晶薄膜材料的制备方法，属于化学工程技术领域。一种KNN基超高击穿电场单晶薄膜材料的制备方法，包括以下步骤：制备KNNS‑LT‑BZ前驱体溶液；所得KNNS‑LT‑BZ前驱体溶液旋涂于不同取向的Nb‑doped SrTiO3衬底上面，得到湿膜；干燥、热解、退火制得一层KNNS‑LT‑BZ薄膜；重复以上制得多层KNNS‑LT‑BZ薄膜。本发明制备方法相对简单，可以通过可以通过多远高熵原理、不同的晶化方式和不同的退火时长控制薄膜的结构和性能，是一种方便快捷的制备技术。
Description
技术领域
本发明涉及一种KNN基超高击穿电场单晶薄膜材料的制备方法，属于化学工程技术领域。
背景技术
随着电子信息技术的发展，对于材料的要求愈来愈高。传统线性电介质材料的介电常数与击穿电场较低，因而储能密度值较低，不能满足实际生产需求，所以需要寻找一种具有超高电场击穿强度的材料。目前，铅基铁电体材料是铁电性能最优异，应用最广泛铁电体材料之一，但在生产和废弃处理过程中，会对环境造成污染。因此研发出具有超高电场击穿强度、铁电性能优异的无铅铁电体材料成为研究的重点。
发明内容
本发明的目的在于提供一种KNN基超高击穿电场单晶薄膜材料的制备方法。
本发明的目的通过如下技术方案实现：
一种KNN基超高击穿电场单晶薄膜材料的制备方法，包括以下步骤：
1)制备KNNS-LT-BZ前驱体溶液，所述KNNS-LT-BZ通式为(NaxK(z-x))(NbySb(z-y))O3-(1-z-c)LiTaO3-cBaZrO3，其中0＜x＜1，0＜y＜1，0＜z＜1，0＜c＜1；
2)将步骤1)所得KNNS-LT-BZ前驱体溶液旋涂于不同取向的Nb-doped SrTiO3衬底上面，所述衬底选自Nb-doped SrTiO3(100)、Nb-doped SrTiO3(110)和Nb-doped SrTiO3(111)中的一种，得到湿膜；
3)将步骤2)所得湿膜干燥、热解、退火制得一层KNNS-LT-BZ薄膜；
4)重复步骤2)和步骤3)制得多层KNNS-LT-BZ薄膜。
优选的是，步骤1)所述的KNNS-LT-BZ前驱体溶液由如下方法制得：将原料CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、Zr(OC3H7)4和C4H6BaO4于120℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)4于室温溶解在冰醋酸和CH3COCH2COCH3的混合液体中，最后所得的两种混合液再次混合于100-150℃搅拌30min，并放置20-30h，得到浓度为0.2-0.3M的KNNS-LT-BZ前驱体溶液。
优选的是，步骤2)所述旋涂包括第一次旋涂和第二次旋涂，所述第一次转速为600-800rpm，旋涂时间为10-20s，第二次旋涂转速为4000-6000rpm，旋涂时间为30-40s。
优选的是，步骤3)所述干燥温度为180-350℃，干燥时间为3-5min；所述热解温度为350-550℃，热解时间为3-5min；退火温度为700-750℃，退火时间为3-8min，退火环境为空气氛围。
优选的是，步骤4)制得12层KNNS-LT-BZ薄膜。
本发明利用KNNS-LT-BZ具有超高电场击穿强度的无铅铁电体材料通过溶胶凝胶合成法在不同取向的Nb-doped SrTiO3衬底上面制备出的KNNS-LT-BZ单晶薄膜材料具有超高电场击穿强度，可以通过不同晶化方式、不同退火时间和不同取向衬底控制薄膜的结构和性能。
附图说明
图1为本发明实施例1、2和3得到的KNNS-LT-BZ单晶薄膜的P-E对比图。
图2为本发明实施例1、2和3得到的KNNS-LT-BZ单晶薄膜的XRD对比图。
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
(1)按照摩尔比0.3:0.6:0.4:0.1:0.1:0.1:0.2:0.2分别称取CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、C4H6BaO4和Zr(OC3H7)4制备KNNS-LT-BZ前驱体溶液；
将原料CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、和C4H6BaO4于120℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)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20h，得到浓度为0.2M通式为(NaxK(z-x))(NbySb(z-y))O3-(1-z-c)LiTaO3-cBaZrO3的KNNS-LT-BZ前驱体溶液，其中x＝0.4，y＝0.6，z＝0.7，c＝0.2；
(2)将步骤(1)得到的KNNS-LT-BZ前驱体溶液使用匀胶机以600rpm的转速第一次旋涂10s和4000rpm的转速第二次旋涂30s在Nb-doped SrTiO3(100)衬底上面，得到湿膜；
(3)将步骤(2)制得的湿膜首先在180℃干燥3min，然后在350℃热解3min，最后在700℃于空气氛围中退火3min。得到一层KNNS-LT-BZ薄膜；
(4)重复步骤(2)和步骤(3)12次，得到12层KNNS-LT-BZ薄膜。
实施例2
(1)按照摩尔比0.4:0.65:0.3:0.05:0.1:0.1:0.2:0.2分别称取CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、C4H6BaO4和Zr(OC3H7)4制备KNNS-LT-BZ前驱体溶液；
将原料CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O和C10H25O5Ta于120℃溶解在冰醋酸和去离子水的混合液体中，然后将C4H6BaO4和Zr(OC3H7)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120℃搅拌30min，并放置25h，得到浓度为0.25M的通式为(NaxK(z-x))(NbySb(z-y))O3-(1-z-c)LiTaO3-cBaZrO3的KNNS-LT-BZ前驱体溶液，其中x＝0.3，y＝0.65，z＝0.7，c＝0.2；
(2)将步骤(1)得到的KNNS-LT-BZ前驱体溶液使用匀胶机以700rpm的转速第一次旋涂15s和5000rpm的转速第二次旋涂35s在Nb-doped SrTiO3(110)衬底上面，得到湿膜；
(3)将步骤(2)制得的湿膜首先在200℃干燥4min，然后在400℃热解4min，最后在720℃空气氛围中退火5min。得到一层KNNS-LT-BZ薄膜；
(4)重复步骤(2)和步骤(3)12次，得到12层KNNS-LT-BZ薄膜。
实施例3
(1)按照摩尔比0.3:0.5:0.3:0.1:0.1:0.1:0.3:0.3分别称取CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、C4H6BaO4和Zr(OC3H7)4制备KNNS-LT-BZ前驱体溶液；
将原料CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、和C4H6BaO4于120℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)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150℃搅拌30min，并放置30h，得到浓度为0.3M的通式为(NaxK(z-x))(NbySb(z-y))O3-(1-z-c)LiTaO3-cBaZrO3的KNNS-LT-BZ前驱体溶液，其中x＝0.3，y＝0.5，z＝0.6，c＝0.3；
(2)将步骤(1)得到的KNNS-LT-BZ前驱体溶液使用匀胶机以800rpm的转速第一次旋涂20s和6000rpm的转速第二次旋涂40s在Nb-dopedSrTiO3(111)衬底上面，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750℃于空气氛围中退火8min。得到一层KNNS-LT-BZ薄膜；
(4)重复步骤(2)和步骤(3)12次，得到12层KNNS-LT-BZ薄膜。
Claims (2)
1.一种KNN基超高击穿电场单晶薄膜材料的制备方法，其特征在于，所述方法由以下步骤组成：
(1)按照摩尔比0.3:0.6:0.4:0.1:0.1:0.1:0.2:0.2分别称取CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、C4H6BaO4和Zr(OC3H7)4制备KNNS-LT-BZ前驱体溶液；
将原料CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、和C4H6BaO4于120℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)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20h，得到浓度为0.2M通式为(NaxK(z-x))(NbySb(z-y))O3-(1-z-c)LiTaO3-cBaZrO3的KNNS-LT-BZ前驱体溶液，其中x＝0.4，y＝0.6，z＝0.7，c＝0.2；
(2)将步骤(1)得到的KNNS-LT-BZ前驱体溶液使用匀胶机以600rpm的转速第一次旋涂10s和4000rpm的转速第二次旋涂30s在Nb-dopedSrTiO3(100)衬底上面，得到湿膜；
(3)将步骤(2)制得的湿膜首先在180℃干燥3min，然后在350℃热解3min，最后在700℃于空气氛围中退火3min，得到一层KNNS-LT-BZ薄膜；
(4)重复步骤(2)和步骤(3)12次，得到12层KNNS-LT-BZ薄膜。
2.一种KNN基超高击穿电场单晶薄膜材料的制备方法，其特征在于，所述方法由以下步骤组成：
(1)按照摩尔比0.3:0.5:0.3:0.1:0.1:0.1:0.3:0.3分别称取CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、C4H6BaO4和Zr(OC3H7)4制备KNNS-LT-BZ前驱体溶液；
将原料CH3COOK、C10H25NbO5、CH3COONa·xH2O、C6H9O6Sb、C2H3O2Li·xH2O、C10H25O5Ta、和C4H6BaO4于120℃溶解在冰醋酸和去离子水的混合液体中，然后将Zr(OC3H7)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150℃搅拌30min，并放置30h，得到浓度为0.3M的通式为(NaxK(z-x))(NbySb (z-y))O3-(1-z-c)LiTaO3-cBaZrO3的KNNS-LT-BZ前驱体溶液，其中x＝0.3，y＝0.5，z＝0.6，c＝0.3；
(2)将步骤(1)得到的KNNS-LT-BZ前驱体溶液使用匀胶机以800rpm的转速第一次旋涂20s和6000rpm的转速第二次旋涂40s在Nb-dopedSrTiO3(111)衬底上面，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750℃于空气氛围中退火8min，得到一层KNNS-LT-BZ薄膜；
(4)重复步骤(2)和步骤(3)12次，得到12层KNNS-LT-BZ薄膜。
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