CN117049868A - 一种高熵陶瓷薄膜材料及其制备方法和应用 - Google Patents
一种高熵陶瓷薄膜材料及其制备方法和应用 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 20
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 50
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 16
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 16
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 11
- 239000011572 manganese Substances 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 239000010409 thin film Substances 0.000 claims description 7
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- 239000000203 mixture Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical group O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 5
- 239000003990 capacitor Substances 0.000 claims description 5
- MCFIMQJAFAOJPD-MTOQALJVSA-J hafnium(4+) (Z)-4-oxopent-2-en-2-olate Chemical group [Hf+4].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O MCFIMQJAFAOJPD-MTOQALJVSA-J 0.000 claims description 5
- JLRJWBUSTKIQQH-UHFFFAOYSA-K lanthanum(3+);triacetate Chemical group [La+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JLRJWBUSTKIQQH-UHFFFAOYSA-K 0.000 claims description 5
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical group [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 5
- 229940069446 magnesium acetate Drugs 0.000 claims description 5
- 235000011285 magnesium acetate Nutrition 0.000 claims description 5
- 239000011654 magnesium acetate Substances 0.000 claims description 5
- 229940071125 manganese acetate Drugs 0.000 claims description 5
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical group [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 4
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- 230000002401 inhibitory effect Effects 0.000 claims description 2
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- 230000015556 catabolic process Effects 0.000 abstract description 15
- 239000010936 titanium Substances 0.000 abstract description 15
- 239000002994 raw material Substances 0.000 abstract description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 2
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- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种高熵陶瓷薄膜材料及其制备方法和应用。该薄膜材料以铋镁钛为基础进行高熵改性,化学式为Bi1‑a‑bLaaSrb(Ti0.5Mg0.5)1‑c‑d‑eMncZrdHfeO3,其中a和b取值均为0‑0.15;c、d和e取值均为0‑0.2,且满足构型熵Sconfig≥1.5R。采用旋涂工艺,通过合适的溶剂配置稳定的前驱体溶液经过老化形成稳定的溶胶,在基板上进行旋涂,并且经过烤胶,最后退火得到稳定的高熵陶瓷薄膜。该薄膜材料具有良好的储能密度与击穿场强,制备方法简单,原料廉价易得,具有广泛的工业前景。
Description
技术领域
本发明属于介电陶瓷薄膜储能材料技术领域,涉及一种高熵陶瓷薄膜材料及其制备方法和应用。
背景技术
储能电介质电容器在先进的电子和电力系统中起着至关重要的作用。然而,一个长期存在的瓶颈是,与电池等电化学储能设备相比,其储能能力相对较小,阻碍了先进设备的小型化、集成化和成本效益。高能量密度、高效率、可靠的电介质的开发工作日益加强介质的能量密度问题取决于其电介质极化(P)在外部应用电场(E)。通过偶极子对外加电场的响应,介质储能电容器可以超高速存储和释放电能,因此被广泛应用于先进的电子和电力系统。然而,电介质储能的主要挑战在于其相对较低的能量密度。虽然已经开发了许多提高储能性能的有效途径,包括畴工程、缺陷控制、界面设计、和非晶/晶粒细化调制,但从本构组成设计开始进一步的性能优化仍然非常需要。最近,自2019年首次尝试以来,一种基于BT基材料的高熵设计被用作储能电容器,受到了越来越多的关注,随后进行了许多类似的研究。然而,能量密度仍然较低,这可能与设计粗糙、机制不明确有关,直到现如今有关高熵储能陶瓷薄膜的报道也仅仅只有一篇。同时高熵陶瓷薄膜的制备工艺也存在一定的困难,比如由于元素种类较多导致无法形成稳定的前驱体溶液。无法形成稳定均匀的薄膜等一系列制备工艺问题都有待改进与完善。
发明内容
本发明的目的在于提出一种高熵陶瓷薄膜材料及其制备方法和应用,该陶瓷薄膜具有良好储能密度,高击穿强度等优点,制备方法简单,热处理温度低,时间短,原料廉价易得,具有广泛的工业应用前景。
为了实现上述技术目的,本发明采用以下技术方案:
提供一种高熵陶瓷薄膜材料,化学式为Bi1-a-bLaaSrb(Ti0.5Mg0.5)1-c-d-eMncZrdHfeO3,其中a和b取值均为0-0.15;c、d和e取值均为0-0.2,且满足构型熵Sconfig≥1.5R。
其中R、N(M)和xi(xj)分别代表理想气体常数、阳离子(阴离子)位置的原子种类和含量。
本发明选择特定元素La、Sr、Mn、Zr、Hf为掺杂元素,当掺杂量达到一定程度,满足构型熵Sconfig≥1.5R时,即为高熵陶瓷,具有良好的储能性能。
本发明还提供了一种高熵陶瓷薄膜的制备方法,包括以下步骤:
1)首先根据化学组成表达式按照化学计量比进行配料,将铋源、镁源、镧源、锶源、锰源、铪源和锆源溶于乙酸和乙二醇甲醚中并用氨水调节pH得到澄清的A溶液;将钛酸四丁酯溶于乙二醇甲醚中,用乙酰丙酮抑制钛酸四丁酯的水解得到B溶液;将A溶液倒入B溶液中与之混合均匀得前驱体溶液,加入pvp进行粘度调节,使前驱体溶液更加均匀稳定,室温下搅拌12-24h;其中A溶液中,乙酸、乙二醇甲醚和氨水的体积比为15:4~8:2~6;B溶液中,乙二醇甲醚和乙酰丙酮的体积比为10~15:1;pvp与前驱体溶液的质量体积比为0.002-0.01g/ml;
2)将步骤1)所得的前驱体溶液静置老化,经过充分的水解与缩聚过程形成稳定澄清的溶胶凝胶;
3)利用旋涂工艺将步骤2)所得的溶胶凝胶在基板上进行旋涂,并进行烤胶处理使其初步形成均匀薄膜;
4)将步骤3)得到的薄膜进行退火热处理,即得稳定均匀致密的高熵陶瓷薄膜。
按上述方案,所述步骤1)中,前驱体溶液中溶质浓度为0.05~0.2mol/L。
按上述方案,所述步骤1)中,铋源为五水硝酸铋,镁源为乙酸镁,镧源为乙酸镧,锶源为乙酸锶,锰源为乙酸锰,铪源为乙酰丙酮铪,锆源为正丙醇锆。
按上述方案,所述步骤2)中,静置时间为12-24h。
按上述方案,所述步骤3)中,基板为Pt/Ti/SiO2/Si。
按上述方案,所述步骤3)中,将基板吸附于匀胶机中,将步骤2)所得溶胶凝胶滴于基板之上,进行旋涂。
按上述方案,所述步骤3)中,旋涂工艺:首先在转速为500-1000rmp下旋涂10-30s进行预旋涂,之后在4000-6000rmp下旋涂30-45s进行正式旋涂。
按上述方案,所述步骤3)中,所述烤胶处理工艺为,分别在200℃、300℃和450℃保温5-10分钟。
按上述方案,所述步骤3)重复四到六次。
按上述方案,所述步骤4)中,退火温度为500-700℃,退火时间为120-300s。
提供一种上述高熵陶瓷薄膜材料在制备储能电容器方面的应用。
本发明的有益效果如下:
1.本发明提供了一种高熵陶瓷薄膜材料,以铋镁钛(Bi(Mg1/2Ti1/2)O3,简记为BMT)为基础体系,通过掺杂特定种类与含量的La、Sr、Mn、Zr、Hf元素从而达到一个较高的熵值,具有高熵效果,实现较高的击穿场强以及良好的储能密度。
2.本发明提供了一种高熵陶瓷薄膜材料的制备方法,通过选择合适比例的乙酸、乙二醇甲醚和氨水配置金属源溶液,加入氨水调控合适的酸碱度,再配合合适比例的乙二醇甲醚和乙酰丙酮配置钛酸四丁酯溶液,将两者混合后通过合适用量的PVP进行粘度调节,可以得到更加稳定的溶胶凝胶,旋涂时有利于得到分散均匀的薄膜,并通过掺杂元素的调控,得到具有高熵效应的高熵陶瓷薄膜,制备方法简单,条件温和,具有工业化应用前景。
附图说明
图1为本发明实施例中高熵陶瓷薄膜的制备方法流程图。
图2为实施例1在较大击穿场强下测得的PE曲线。
图3为实施例2在较大击穿场强下测得的PE曲线。
图4为实施例3在较大击穿场强下测得的PE曲线。
图5为实施例1所得产物的XRD图谱。
图6为实施例2所得产物的XRD图谱。
图7为实施例3所得产物的XRD图谱。
图8为对比例1所得产物的XRD图谱。
图9为对比例1在最大击穿场强下测得的PE曲线。
图10为对比例2在最大击穿场强下测得的PE曲线。
图11为对比例3在最大击穿场强下测得的PE曲线。
具体实施方式
下面详细描述本发明的实施例,下面的实施例是示例性的,旨在于更好的解释本发明,不能理解为对本发明的限制。
实施例1
提供一种高熵陶瓷薄膜,其化学组成表达式为Bi1-a-bLaaSrb(Ti0.5Mg0.5)1-c-d- eMncZrdHfeO3,a=0.1,b=0,c=d=e=0.1其制备方法包括以下步骤:
(1)按照陶瓷薄膜的化学计量比称取一定的溶质原料。其中将五水硝酸铋、乙酸镧、乙酸锶、乙酸镁、乙酸锰、乙酰丙酮铪、正丙醇锆溶于15mL乙酸和5mL乙二醇甲醚并用5ml氨水进行酸碱度调节得到混合液A;将钛酸四丁酯溶于23mL乙二醇甲醚并滴加2mL乙酰丙酮抑制钛酸四丁酯水解得到混合溶液B,待A溶液搅拌至澄清混合均匀后,将A溶液倒入B溶液中与之混合均匀得前驱体溶液,溶质浓度为0.2mol/L,再加入0.25g聚乙烯吡咯烷酮(pvp)室温下搅拌24h左右。
(2)静置老化步骤(1)中的前驱体溶液24h得到澄清的,具有丁达尔效应的前驱体溶液。
(3)将步骤(2)所得前驱体溶液采用直径为2微米左右的过滤器进行过滤,然后用注射器吸取步骤(2)中的10mL左右前驱体液进行旋涂工艺。
(4)将Pt/Ti/SiO2/Si基板吸附于匀胶机中,将溶液滴于基板之上,首先在转速为500rmp下旋涂10s进行预旋涂,之后在4500rmp下旋涂30s进行正式旋涂,将正式旋涂之后的基片放置加热台进行烤胶处理,200℃-300℃-450℃,时间均为6分钟。
(5)将步骤(4)重复四次后,对得到的薄膜进行退火处理,退火温度为600℃,退火时间为120s,得到厚度约为160nm的高熵陶瓷薄膜。
对实施例1的熵值进行计算,构型熵Sconfig=1.75R。
将实施例1所制备的薄膜进行X射线衍射测试(XRD),分析薄膜晶体结构,图谱如图5所示,出现了较为明显的焦绿石相。稳定的焦绿石相具有较小的剩余极化,降低能量损失,PE曲线呈线性。
将实施例1所制备的高熵陶瓷薄膜利用磁控溅射制备顶电极,测试铁电性能如图2所示,具有较高的击穿场强,约为4200kv/cm。
实施例2
提供一种高熵陶瓷薄膜,其化学组成表达式为Bi1-a-bLaaSrb(Ti0.5Mg0.5)1-c-d- eMncZrdHfeO3,a=0.1,b=0.05,c=d=e=0.1其制备方法包括以下步骤:
(1)按照陶瓷薄膜的化学计量比称取一定的溶质原料,将五水硝酸铋、乙酸镧、乙酸锶、乙酸镁、乙酸锰、乙酰丙酮铪、正丙醇锆溶于15mL乙酸和5mL乙二醇甲醚并用5ml氨水进行酸碱度调节得到混合液A;将钛酸四丁酯溶于23mL乙二醇甲醚并滴加2mL乙酰丙酮抑制钛酸四丁酯水解得到混合溶液B,待A溶液搅拌至澄清混合均匀后,将A溶液倒入B溶液中与之混合均匀得前驱体溶液,溶质浓度为0.2mol/L,再加入0.25g pvp室温下搅拌24h左右。
(2)静置老化步骤一中的前驱体溶液24h得到澄清的,具有丁达尔效应的前驱体溶液。
(3)将步骤(2)所得前驱体溶液采用直径为2微米左右的过滤器进行过滤,然后用注射器吸取步骤二中的10ML左右前驱体液进行旋涂工艺。
(4)将Pt/Ti/SiO2/Si基板吸附于匀胶机中,将溶液滴于基板之上,首先在转速为500rmp下旋涂10s进行预旋涂,之后在4500rmp下旋涂30s进行正式旋涂,将正式旋涂之后的基片放置加热台进行烤胶处理,200℃-300℃-450℃,时间均为6分钟。
(5)将步骤(4)重复四次后,对得到的薄膜进行退火处理,退火温度为600℃,退火时间为120s,得到厚度约为160nm的高熵陶瓷薄膜。
对实施例2的熵值进行计算,构型熵Sconfig=1.94R。
将实施例2所制备的薄膜进行X射线衍射测试(XRD),分析薄膜晶体结构,图谱如图6所示,出现了较为明显的焦绿石相。
将实施例2所制备的高熵陶瓷薄膜利用磁控溅射制备顶电极,测试铁电性能如图3所示,具有较高的击穿场强,约为4700kv/cm。
实施例3
提供一种高熵陶瓷薄膜,其化学组成表达式为Bi1-a-bLaaSrb(Ti0.5Mg0.5)1-c-d- eMncZrdHfeO3,a=0.05,b=0.05,c=d=e=0.13其制备方法包括以下步骤:
(1)按照陶瓷薄膜的化学计量比称取一定的溶质原料,将五水硝酸铋、乙酸镧、乙酸锶、乙酸镁、乙酸锰、乙酰丙酮铪、正丙醇锆溶于15mL乙酸和5mL乙二醇甲醚并用5ml氨水进行酸碱度调节得到混合液A;将钛酸四丁酯溶于23mL乙二醇甲醚并滴加2mL乙酰丙酮抑制钛酸四丁酯水解得到混合溶液B,待A溶液搅拌至澄清混合均匀后,将A溶液倒入B溶液中与之混合均匀得前驱体溶液,溶质浓度为0.2mol/L,再加入0.25g pvp室温下搅拌24h左右。
(2)静置老化步骤一中的前驱体溶液24h得到澄清的,具有丁达尔效应的前驱体溶液。
(3)将步骤(2)所得前驱体溶液采用直径为2微米左右的过滤器进行过滤,然后用注射器吸取步骤二中的10mL左右前驱体液进行旋涂工艺。
(4)将Pt/Ti/SiO2/Si基板吸附于匀胶机中,将溶液滴于基板之上,首先在转速为500rmp下旋涂10s进行预旋涂,之后在4500rmp下旋涂30s进行正式旋涂,将正式旋涂之后的基片放置加热台进行烤胶处理,200℃-300℃-450℃,时间均为5-10分钟。
(5)将步骤(4)重复四次后,对得到的薄膜进行退火处理,退火温度为600℃,退火时间为120s,得到厚度约为160nm的高熵陶瓷薄膜。
对实施例3的熵值进行计算,构型熵Sconfig=1.91R。
将实施例3所制备的薄膜进行X射线衍射测试(XRD),分析薄膜晶体结构,图谱如图7所示,出现了较为明显的焦绿石相。
将实施例3所制备的高熵陶瓷薄膜利用磁控溅射制备顶电极,测试铁电性能如图4所示,具有较高的击穿场强,约为3800kv/cm。
对比例1
一种陶瓷薄膜材料,表达式为Bi(Mg0.5Ti0.5)O3;对其熵值进行计算,构型熵Sconfig=0.69R。
其制备方法同实施例1,其区别在于该陶瓷薄膜材料未达到高熵。
将对比例1所制备的高熵陶瓷薄膜利用磁控溅射制备顶电极,测试铁电性能如图9所示,击穿场强较低,约为1000kv/cm。对对比例1中制备出的样品进行XRD表征,如图8可以看出具有明显的钙钛矿相结构。
对比例2
一种陶瓷薄膜材料,表达式为Bi0.9Ca0.1La0.1Sr0.1Na0.1(Mg0.5Ti0.5)O3;对其熵值进行计算,构型熵Sconfig=1.92R。
其制备方法同实施例1,其区别为该陶瓷薄膜材料中选择的掺杂元素不同。
将对比例2所制备的高熵陶瓷薄膜利用磁控溅射制备顶电极,测试铁电性能如图10所示,击穿场强较低,约为1500kv/cm。说明并非达到高熵即可提高性能,还需要本发明选择的特定的掺杂元素。
对比例3
一种陶瓷薄膜材料,表达式为Bi0.94La0.03Sr0.03(Mg0.5Ti0.5)0.8Mn0.1Zr0.1O3;对其熵值进行计算,构型熵Sconfig=1.46R。
其制备方法同实施例1,其区别为该陶瓷薄膜材料掺杂元素掺量不足,未达到高熵。
将对比例3所制备的高熵陶瓷薄膜利用磁控溅射制备顶电极,测试铁电性能如图11所示,击穿场强较低,约为1800kv/cm。
应当理解的是,对本领域普通技术人员来说,可以根据上述说明加以改进或变换,而所有这些改进和变换都应属于本发明所附权利要求的保护范围。
Claims (10)
1.一种高熵陶瓷薄膜材料,其特征在于,化学式为Bi1-a-bLaaSrb(Ti0.5Mg0.5)1-c-d- eMncZrdHfeO3,其中a和b取值均为0-0.15;c、d和e取值均为0-0.2,且满足构型熵Sconfig≥1.5R。
2.一种权利要求1所述的高熵陶瓷薄膜的制备方法,其特征在于,包括以下步骤:
1)首先根据化学组成表达式按照化学计量比进行配料,将铋源、镁源、镧源、锶源、锰源、铪源和锆源溶于乙酸和乙二醇甲醚中并用氨水调节pH得到澄清的A溶液;将钛酸四丁酯溶于乙二醇甲醚中,用乙酰丙酮抑制钛酸四丁酯的水解得到B溶液;将A溶液倒入B溶液中与之混合均匀得前驱体溶液,加入pvp进行粘度调节,室温下搅拌12-24h;其中A溶液中,乙酸、乙二醇甲醚和氨水的体积比为15:4~8:2~6;B溶液中,乙二醇甲醚和乙酰丙酮的体积比为10~15:1;pvp与前驱体溶液的质量体积比为0.002-0.01g/ml;
2)将步骤1)所得的前驱体溶液静置老化,经过充分的水解与缩聚过程形成稳定澄清的溶胶凝胶;
3)利用旋涂工艺将步骤2)所得的溶胶凝胶在基板上进行旋涂,并进行烤胶处理使其初步形成均匀薄膜;
4)将步骤3)得到的薄膜进行退火热处理,即得稳定均匀致密的高熵陶瓷薄膜。
3.根据权利要求2所述的制备方法,其特征在于,所述步骤1)中,前驱体溶液中溶质浓度为0.05~0.2mol/L。
4.根据权利要求2所述的制备方法,其特征在于,所述步骤1)中,铋源为五水硝酸铋,镁源为乙酸镁,镧源为乙酸镧,锶源为乙酸锶,锰源为乙酸锰,铪源为乙酰丙酮铪,锆源为正丙醇锆。
5.根据权利要求2所述的制备方法,其特征在于,所述步骤2)中,静置时间为12-24h。
6.根据权利要求2所述的制备方法,其特征在于,所述步骤3)中,旋涂工艺:首先在转速为500-1000rmp下旋涂10-30s进行预旋涂,之后在4000-6000rmp下旋涂30-45s进行正式旋涂。
7.根据权利要求2所述的制备方法,其特征在于,所述步骤3)中,所述烤胶处理工艺为,分别在200℃、300℃和450℃保温5-10分钟。
8.根据权利要求2所述的制备方法,其特征在于,所述步骤3)中旋涂、烤胶工艺重复四到六次。
9.根据权利要求2所述的制备方法,其特征在于,所述步骤4)中,退火温度为500-700℃,退火时间为120-300s。
10.一种权利要求1所述的高熵陶瓷薄膜材料在制备储能电容器方面的应用。
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