CN111039672B - 一种高功率密度的Sn掺杂高熵钙钛矿氧化物陶瓷材料及其制备方法 - Google Patents
一种高功率密度的Sn掺杂高熵钙钛矿氧化物陶瓷材料及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910052574 oxide ceramic Inorganic materials 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 20
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 20
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000007873 sieving Methods 0.000 claims abstract description 13
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 10
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 10
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
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- 238000000034 method Methods 0.000 claims description 11
- 238000009694 cold isostatic pressing Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000011267 electrode slurry Substances 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- 239000003990 capacitor Substances 0.000 claims description 5
- 229910052573 porcelain Inorganic materials 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052845 zircon Inorganic materials 0.000 claims description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 3
- 238000000748 compression moulding Methods 0.000 claims 1
- 239000011812 mixed powder Substances 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 37
- 238000004146 energy storage Methods 0.000 abstract description 18
- 239000011159 matrix material Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
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- 229910010252 TiO3 Inorganic materials 0.000 description 12
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Abstract
一种高功率密度的Sn掺杂高熵钙钛矿氧化物陶瓷材料。该材料的制备方法为:首先采用了Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2为原料,按化学式(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1‑ x Sn x O3配比取料,对粉体进行湿法球磨混合,干燥后的粉体在900℃下预烧2h,再经过二次球磨、过筛和成型,最终在1250℃温度下烧结2h得到了单相的高熵钙钛矿氧化物陶瓷材料。本发明所制备的高熵陶瓷材料制备工艺简单,制作成本低,通过选择适当的x值,可使放电储能密度达到1.74J/cm3,同时功率密度达51.4MW/cm3,提供了一种新的无铅储能材料基体。
Description
技术领域
本发明涉及弛豫铁电体的技术领域,具体涉及一种(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1- x Sn x O3高功率密度高熵钙钛矿氧化物陶瓷材料、制备方法及其应用。
背景技术
随着脉冲功率技术在混合动力汽车、航空航天及石油钻井等领域的飞速发展,对储能介质电容器提出了“高温化、高能量密度和高可靠性”的要求。然而,储能介质电容器的性能主要取决于所使用的储能介质材料。当传统材料的发展越来越趋近于其极限、无法满足各行业新技术日益增长的需要时,开发新材料变得尤为重要。“高熵”是近年来出现的新的材料设计理论,目前已成为材料研究领域的一大热点。弛豫铁电体由于在理想状态下具有零剩余极化(P r)和高饱和极化(P s),在储能中的应用越来越受到重视。但大多数弛豫铁电体都含有铅,在制备和使用过程中对环境造成了极大的破坏,因此需要开发无铅的弛豫铁电体体系。
发明内容
(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3作为弛豫铁电材料,具有相较于一般铁电材料较低的剩余极化,通过四价离子Sn4+的掺杂对基体储能性能及充放电性能进行进一步改性。一方面,四价Sn离子在(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3的B位取代同价Ti离子,抑制了晶粒生长,降低了晶粒尺寸,增加了高绝缘性晶界的数量,从而增加了晶界势垒高度,利用晶界势垒效应提高材料的击穿强度;另一方面,SnO2本身是具有高绝缘性(禁带宽度为4.5eV)的材料,即绝缘性能介于材料晶粒与晶界之间,因此有为晶粒与晶界之间的电荷传输提供便捷通道、促使电荷由局域态向扩散态转变的理论基础,在一定程度上可抑制界面极化、提高击穿场强,最终改善陶瓷材料的储能性能。
本发明的目的在于提供一种高功率密度的Sn掺杂高熵钙钛矿氧化物陶瓷材料及其制备方法,在(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3基体中,通过掺入Sn4+离子以期提高陶瓷材料的击穿强度从而改善其储能性能。
为达成上述所提到的性能,本发明采用如下技术方案:
一种高功率密度的Sn掺杂高熵钙钛矿氧化物陶瓷材料,其化学式为(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3,其中x为Sn离子的掺杂量,0.01≤ x ≤ 0.07,其中x表示摩尔百分比。
一种高功率密度的Sn掺杂高熵钙钛矿氧化物陶瓷材料,包括以下步骤:
(1)按照化学式(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3将分析纯的Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2配制后通过机械球磨混合均匀,然后烘干,过筛,再经预烧,得到块状固体。
(2)将块状固体粉碎后,再次进行球磨,得到产品过筛得到尺寸均匀的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3粉体。
(3)将得到的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3粉体,以每份质量0.35-0.40g进行称量,然后倒入模具当中,施加500-700N竖直方向上的力,将成型好的圆片进行脱模,得到形状完好的样品。
(4)将圆片放置于胶套当中,利用抽真空设备将胶套的空气排出,密封胶套口,放入冷等静压成型。
(5)将得到的样品从胶套中取出后于箱式炉中烧结成瓷,得到(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3高熵陶瓷材料样品。
(6)打磨、清洗步骤(5)中一次烧结好的式样后,在式样的正反两面均匀涂覆银电极浆料,进行热处理,得到Sn4+掺杂的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3具有高功率密度的高熵陶瓷材料。
所述步骤(1)、步骤(2)中球磨时间均为4~6小时。
所述步骤(1)、步骤(2)中混合氧化物与锆球石及去离子水混合、球磨、烘干后形成干料。
所述步骤(1)中预烧条件为:以5℃/min升温至900℃,保温2小时,之后,以5℃/min降温至500℃,随炉冷却到室温。
所述步骤(2)中,将块体粉碎后过200-300目筛得到尺寸均匀的粉体。
所述步骤(4)中,冷等静压成型是,在压机中施加200-250MPa的压力,保压时间为180-300s。
所述步骤(5)中烧结条件为:以5℃/min升到1250℃,保温2小时,之后,以5℃/min降温至500℃,随炉冷却到室温。
所述步骤(6)中热处理的温度为800-850 ℃,保温时间为15-20min。
与现有的技术相比,本发明具有的有益结果:本发明将Sn4+掺杂在(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3基体材料中B位,通过配方设计,验证了四价Sn离子在(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3的B位取代同价Ti离子,抑制了晶粒生长,降低了晶粒尺寸,增加了高绝缘性晶界的数量,从而增加了晶界势垒高度,利用晶界势垒效应提高材料的击穿强度;其次,随着高绝缘性SnO2的掺杂,一定程度抑制了基体材料体系的界面极化,(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3基体材料击穿场强得到提高,储能密度及效率得到了改善;在120 ℃高温工作环境下,依然保持稳定的欠阻尼波形,功率密度亦保持在40MW/cm3以上,适用于高温下脉冲功率电容器应用。通过与之前的类似方法进行改性的材料进行对比,发现本发明所制备的材料储能及充放电性能更加优异。在本发明的样品的制备过程当中,采用了更加先进的冷等静压成型技术,避免了样品的浪费和粘结剂的加入,节省了制作的成本,加快了生产周期并且避免了粘结剂对样品污染的可能性,在后续步骤之中,减少了排除粘结剂的步骤,减少了资源的浪费和制作时间的浪费,除此之外,由于冷等静压成型技术是利用液体进行压力的传递,与传统单项加压的压制相比,冷等静压成型会让样品从各个方向受到压力,并且压力相比较更大,制备的生坯更加的致密,为下一步优异实验结果奠定了基础。
另外,随着人们的环保意识的加强,材料的生产要规避对环境的影响,本发明所采用的原材料中由于不含铅等重金属元素,对环境友好,所以制备过程中不会对环境破坏。本发明所制备的材料致密性良好,无明显的气孔存在,晶粒尺寸均匀,所以本发明能够保证Sn掺杂的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3具有高温下优异的储能及充放电性能。
附图说明
图1为(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3陶瓷材料组分中当x=0.01、0.03、0.05和0.07时,陶瓷材料粉体的XRD图谱;
图2为(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3陶瓷材料组分中当x=0,0.01、0.03、0.05和0.07时,陶瓷材料的极化强度随电场变化图谱(单极电滞回线);
图3(a)(b)分别为(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.97Sn0.03O3陶瓷材料在20-120 kV/cm 和40-120 ℃下的欠阻尼波形图谱。
具体实施方式
下面结合附图及实施例对本发明进行详细说明,但是本发明不局限于以下实施例。
本发明中,制备了Sn掺杂的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3高熵陶瓷材料。
实施例一
该高熵陶瓷材料的化学式为:(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3,其中x表示摩尔百分比,且x=0.01。
上述Sn掺杂(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3高熵陶瓷材料的制备方法,包括以下步骤:
(1)按照化学式(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3(x=0.01)将分析纯的Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2配制后通过球磨混合均匀,然后烘干、过筛,再经预烧,得到块状固体;
(2)将块状固体粉碎后,再次进行球磨,产品过筛得到尺寸均匀的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.99Sn0.01O3粉体;
(3)将得到的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.99Sn0.01O3粉体,以每份质量0.35-0.40g进行称量,然后倒入模具当中,施加600N的力,将成型好的圆片进行脱模,得到形状完好的样品;
(4)将圆片放置于胶套当中,利用抽真空设备将胶套的空气排出,密封胶套口,放入冷等静压成型,在200Mpa的压力下保压300s;
(5)将得到的样品从胶套中取出后于箱式炉中1250℃烧结2小时成瓷,得到(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.99Sn0.01O3线性电介质陶瓷材料样品;
(6)打磨、清洗步骤(5)中一次烧结好的式样后,在式样的正反两面均匀涂覆银电极浆料,在750℃进行热处理25min,得到(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.99Sn0.01O3高熵陶瓷材料。
参照图1,图1中x=0.01曲线为本实施例制备样品的XRD曲线,由图1可以看出高熵陶瓷材料(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.99Sn0.01O3组分中x=0.01时,合成了纯相的陶瓷。
参照图2,图2中x=0.01曲线为本实施例制备样品的电滞回线,由图2可以看出线性电介质陶瓷材料(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3组分中x=0.01时,储能密度为1.375J/cm3,储能效率为85.6%以上。
实施例二
该高熵陶瓷材料的化学式为:(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3,其中x表示摩尔百分比,且x=0.03。
上述Sn掺杂(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3高熵陶瓷材料的制备方法,包括以下步骤:
(1)按照化学式(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3(x=0.03)将分析纯的Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2配制后通过球磨混合均匀,然后烘干、过筛,再经预烧,得到块状固体;
(2)将块状固体粉碎后,再次进行球磨,产品过筛得到尺寸均匀的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.97Sn0.03O3粉体;
(3)将得到的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.97Sn0.03O3粉体,以每份质量0.35-0.40g进行称量,然后倒入模具当中,施加600N的力,将成型好的圆片进行脱模,得到形状完好的样品;
(4)将圆片放置于胶套当中,利用抽真空设备将胶套的空气排出,密封胶套口,放入冷等静压成型,在200Mpa的压力下保压300s;
(5)将得到的样品从胶套中取出后于箱式炉中1250℃烧结2小时成瓷,得到(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.97Sn0.03O3线性电介质陶瓷材料样品;
(6)打磨、清洗步骤(5)中一次烧结好的式样后,在式样的正反两面均匀涂覆银电极浆料,在750℃进行热处理25min,得到(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.97Sn0.03O3高熵陶瓷材料。
参照图1,图1中x=0.03曲线为本实施例制备样品的XRD曲线,由图1可以看出高熵陶瓷材料(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.97Sn0.03O3组分中x=0.03时,合成了纯相的陶瓷。
参照图2,图2中x=0.03曲线为本实施例制备样品的电滞回线,由图2可以看出线性电介质陶瓷材料(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3组分中x=0.03时,储能密度为1.742J/cm3,储能效率为85.9%以上。
参照图3,由图3(a)中可以看出(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.97Sn0.03O3高熵陶瓷材料在120kV/cm的电场下电流密度为857.1A/cm2,功率密度为51.4 MW/cm3;由图3(b)中可以看出(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.97Sn0.03O3高熵陶瓷材料在40-120℃范围内仍保持很好的欠阻尼波形,即具有良好的温度稳定性。
实施例三
该高熵陶瓷材料的化学式为:(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3,其中x表示摩尔百分比,且x=0.05。
上述Sn掺杂(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3高熵陶瓷材料的制备方法,包括以下步骤:
(1)按照化学式(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3(x=0.05)将分析纯的Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2配制后通过球磨混合均匀,然后烘干、过筛,再经预烧,得到块状固体;
(2)将块状固体粉碎后,再次进行球磨,产品过筛得到尺寸均匀的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.95Sn0.05O3粉体;
(3)将得到的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.95Sn0.05O3粉体,以每份质量0.35-0.40g进行称量,然后倒入模具当中,施加600N的力,将成型好的圆片进行脱模,得到形状完好的样品;
(4)将圆片放置于胶套当中,利用抽真空设备将胶套的空气排出,密封胶套口,放入冷等静压成型,在200Mpa的压力下保压300s;
(5)将得到的样品从胶套中取出后于箱式炉中1250℃烧结2小时成瓷,得到(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.95Sn0.05O3线性电介质陶瓷材料样品;
(6)打磨、清洗步骤(5)中一次烧结好的式样后,在式样的正反两面均匀涂覆银电极浆料,在750℃进行热处理25min,得到(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.95Sn0.05O3高熵陶瓷材料。
参照图1,图1中x=0.05曲线为本实施例制备样品的XRD曲线,由图1可以看出高熵陶瓷材料(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.95Sn0.05O3组分中x=0.05时,合成了纯相的陶瓷。
参照图2,图2中x=0.05曲线为本实施例制备样品的电滞回线,由图2可以看出线性电介质陶瓷材料(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3组分中x=0.05时,储能密度为1.621J/cm3,储能效率为92.5%以上。
实施例四
该高熵陶瓷材料的化学式为:(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3,其中x表示摩尔百分比,且x=0.07。
上述Sn掺杂(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)TiO3高熵陶瓷材料的制备方法,包括以下步骤:
(1)按照化学式(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3(x=0.07)将分析纯的Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2配制后通过球磨混合均匀,然后烘干、过筛,再经预烧,得到块状固体;
(2)将块状固体粉碎后,再次进行球磨,产品过筛得到尺寸均匀的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.93Sn0.07O3粉体;
(3)将得到的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.93Sn0.07O3粉体,以每份质量0.35-0.40g进行称量,然后倒入模具当中,施加600N的力,将成型好的圆片进行脱模,得到形状完好的样品;
(4)将圆片放置于胶套当中,利用抽真空设备将胶套的空气排出,密封胶套口,放入冷等静压成型,在200Mpa的压力下保压300s;
(5)将得到的样品从胶套中取出后于箱式炉中1250℃烧结2小时成瓷,得到(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.93Sn0.07O3线性电介质陶瓷材料样品;
(6)打磨、清洗步骤(5)中一次烧结好的式样后,在式样的正反两面均匀涂覆银电极浆料,在750℃进行热处理25min,得到(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.93Sn0.07O3高熵陶瓷材料。
参照图1,图1中x=0.07曲线为本实施例制备样品的XRD曲线,由图1可以看出高熵陶瓷材料(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti0.93Sn0.07O3组分中x=0.07时,合成了纯相的陶瓷。
Claims (7)
1.一种高功率密度的Sn掺杂高熵钙钛矿氧化物陶瓷材料的制备方法,其特征在于,包括如下步骤:
按照化学式(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3、x=0.03将分析纯的Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2配制后,对粉体进行球磨、预烧、过筛、成型,将成型的陶瓷坯体在1250℃温度下烧结,得到一种高功率密度的Sn掺杂高熵钙钛矿氧化物陶瓷材料;
所述成型采用冷等静压成型,压强200-250MPa。
2.如权利要求1所述的方法,其特征在于,包括至少两次球磨,Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2混合后进行第一次球磨,然后在900℃进行预烧,得到块状固体;将块状固体再次球磨,然后过筛。
3.如权利要求1所述的方法,其特征在于,包括如下步骤:
1)按照化学式(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3、x=0.03将分析纯的Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2配制后通过球磨混合均匀,然后烘干、过筛,再经预烧,得到块状固体;
2)将块状固体粉碎后,再次进行球磨,产品过筛得到尺寸均匀的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3粉体;
3)将得到的(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3粉体倒入模具当中压制成型,将成型好的坯体进行脱模,得到形状完好的坯体;
4)将步骤3)制备的坯体冷等静压成型;
5)将步骤4)得到的坯体烧结成瓷,得到具有高功率密度的电介质(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3陶瓷。
4.如权利要求1所述的方法,其特征在于,Na2CO3、Bi2O3、BaCO3、SrCO3、CaCO3、TiO2和SnO2混合粉体在去离子水中以锆球石进行球磨,球磨时间为4~6小时。
5.权利要求1~4任一项所述方法制备的材料,其特征在于,化学式为(Na0.2Bi0.2Ba0.2Sr0.2Ca0.2)Ti1-x Sn x O3,x=0.03。
6.一种电容器,包括电极和介电层,其特征在于,所述介电层为权利要求5所述材料。
7.权利要求6所述电容器的制备方法,其特征在于,包括如下步骤:打磨、清洗权利要求5所述材料,在前述材料的正反两面均匀涂覆银电极浆料,800-850 ℃热处理15-20 min。
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