CN107216147B - 一种高击穿场强钛酸锆铜镉巨介电陶瓷材料及其制备方法 - Google Patents
一种高击穿场强钛酸锆铜镉巨介电陶瓷材料及其制备方法 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 40
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 230000015556 catabolic process Effects 0.000 title claims abstract description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- PLZFHNWCKKPCMI-UHFFFAOYSA-N cadmium copper Chemical compound [Cu].[Cd] PLZFHNWCKKPCMI-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 14
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229960000583 acetic acid Drugs 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 9
- 238000005469 granulation Methods 0.000 claims abstract description 4
- 230000003179 granulation Effects 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910008334 ZrO(NO3)2 Inorganic materials 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims 1
- 229910006219 ZrO(NO3)2·2H2O Inorganic materials 0.000 abstract description 6
- 239000002243 precursor Substances 0.000 abstract description 4
- 229910003068 Ti(C4H9O)4 Inorganic materials 0.000 abstract description 2
- 239000002738 chelating agent Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 238000004146 energy storage Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 229910002966 CaCu3Ti4O12 Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002661 O–Ti–O Inorganic materials 0.000 description 1
- 229910002655 O−Ti−O Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910003083 TiO6 Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种高击穿场强钛酸锆铜镉巨介电陶瓷材料及其制备方法,该陶瓷材料由CdCu3ZrxTi4‑xO12表示的材料组成,其中x的取值为0.05~0.20,其是以Cd(NO3)2·4H2O、Cu(NO3)2·3H2O、ZrO(NO3)2·2H2O、Ti(C4H9O)4为原料,冰醋酸为螯合剂,先采用溶胶‑凝胶法制备前驱粉体,并将前驱粉体在较低温度下煅烧,得到能在分子水平上混合且均匀性较好、活性高的CdCu3ZrxTi4‑xO12陶瓷粉体,然后将陶瓷粉体经造粒、压片、排胶、烧结制备而成。本发明陶瓷材料的制备方法简单、反应温度较低、重复性好、成品率高,且陶瓷材料的介电性能优良,具有较高的击穿场强,实用性强,因此在高压电容等领域具有广泛的应用前景。
Description
技术领域
本发明属于电子陶瓷材料技术领域,具体涉及到一种高击穿场强钛酸锆铜镉巨介电陶瓷材料及其制备方法。
背景技术
介质材料是国家十三五规划中新型储能材料开发的一类关键材料。电介质电容器结合了传统电容器和电池的优点,避免了电化学超级电容器的缺陷,是一种应用前景广阔的固体电源。相较于电池和电化学超级电容器,电介质电容器具有高的功率密度(比电池高5个数量级)、可实现瞬间充电以及充放电过程不涉及电化学反应,安全可靠等优点,但其储能密度比电池低5个数量级、不利于储能元件的小型化。如何提高电介质电容器储能密度是当前固态超级电容器领域中的研究热点和前沿。对于线性电介质而言其储能密度(γ)取决于相对介电常数ε与介电强度Eb,γ=ε0εEb 2/2,从公式可以看出,获得高介电常数和高介电强度(高击穿场强)是获得高储能密度的前提条件。因此,开发高介电常数(>103)、高击穿场强的介电材料是迫切需要的。
ACu3Ti4O12(A为碱金属或稀土金属或空缺)这一族氧化物是在1967年被发现的,人们对ACu3Ti4O12族氧化物的结构进行了精确的测定,并测量了其介电性能。2002年,Subramanian等人首次报道CdCu3Ti4O12(CdCTO)陶瓷材料,其作为ACu3Ti4O12氧化物陶瓷材料的一种,具有与CaCu3Ti4O12(CCTO)陶瓷相似的结构,但却具有较低的介电常数,10kHz下,相对介电常数为409,介电损耗为0.093。近些年来,虽然一些研究者采用传统固相法获得了较高的介电常数,但其介电损耗依然较高,同时该类材料偏压性能差、击穿电压低,限制了其在储能电容器方面的实际应用,很难广泛应用于电容器、存储器等电子市场中需要的高介电常数的电子器件。
发明内容
本发明所要解决的技术问题在于提供一种具有高击穿场强的钛酸锆铜镉巨介电陶瓷材料,并为其提供一种制备方法。
解决上述技术问题所采用的陶瓷材料由该陶瓷材料由CdCu3ZrxTi4-xO12表示的材料组成,其中x的取值为0.02~0.20,优选x的取值为0.05~0.10。
本发明高击穿场强钛酸锆铜镉巨介电陶瓷材料的制备方法由下述步骤组成:
1、按照CdCu3ZrxTi4-xO12的化学计量比,将Cd(NO3)2·4H2O、Cu(NO3)2·3H2O、ZrO(NO3)2·2H2O加入到无水乙醇与去离子水的混合溶剂中配制成溶液A,将Ti(C4H9O)4加入到无水乙醇中配制成溶液B;将溶液A和溶液B混合,并加入冰醋酸,所得混合液中钛酸丁酯的浓度为0.3~0.7mol/L、冰醋酸的体积分数为2.5%~10%、去离子水的体积分数为5%~15%,在30~75℃下加热并搅拌均匀,得到溶胶,继续搅拌直至溶胶变为凝胶,将凝胶陈化后干燥,得到干凝胶;将干凝胶研磨后,在600~700℃下煅烧8~10小时,得到CdCu3ZrxTi4- xO12陶瓷粉体。
2、将CdCu3ZrxTi4-xO12陶瓷粉体经造粒、压片、排胶后,在980~1000℃烧结10~15小时,得到高击穿场强钛酸锆铜镉巨介电陶瓷材料。
上述步骤1中,优选所得混合液中钛酸丁酯的浓度为0.5mol/L、冰醋酸的体积分数为5%、去离子水的体积分数为10%。
上述步骤1中,进一步优选在40~50℃下加热并搅拌均匀,得到溶胶。
上述步骤1中,更优选将干凝胶研磨后,在650℃下煅烧10小时。
上述步骤2中,优选在990℃下烧结15小时。
本发明以Cd(NO3)2·4H2O、Cu(NO3)2·3H2O、ZrO(NO3)2·2H2O、Ti(C4H9O)4为原料,冰醋酸为螯合剂,先采用溶胶-凝胶法制备前驱粉体,并将前驱粉体在较低温度下煅烧,得到能在分子水平上混合且均匀性较好、活性高的CdCu3ZrxTi4-xO12陶瓷粉体,然后将陶瓷粉体经造粒、压片、排胶、烧结,即可得到高击穿场强钛酸锆铜镉巨介电陶瓷材料。
本发明陶瓷材料的制备方法简单、反应温度较低、重复性好、成品率高,且陶瓷材料的介电性能优良,具有较高的击穿场强,当x=0.05时,即CdCu3Zr0.05Ti3.95O12陶瓷获得较优的介电性能,1kHz下,其相对介电常数为15082,介电损耗为0.07,同时击穿场强高达1530V/cm,有望应用于高储能密度动态随机存储器和高压电容器领域。
附图说明
图1是对比例1和实施例1~3制备的陶瓷材料的XRD图。
图2是对比例1和实施例1~3制备的陶瓷材料的介电常数随测试频率的变化关系图。
图3是对比例1和实施例1~3制备的陶瓷材料的拉曼强度随测试波长的变化关系图。
图4是对比例1和实施例1制备的陶瓷材料工作场强随电流密度的变化关系图。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明,但本发明的保护范围不仅限于这些实施例。
实施例1
1、按照CdCu3Zr0.05Ti3.95O12的化学计量比,将3.1159g Cd(NO3)2·4H2O、7.3212g Cu(NO3)2·3H2O、0.1168g ZrO(NO3)2·2H2O加入到10mL无水乙醇与去离子水的混合溶剂中配制成溶液A,将13.6mLTi(C4H9O)4加入到52.4mL无水乙醇中配制成溶液B;将溶液A和溶液B混合,并加入4mL冰醋酸,所得混合液中钛酸丁酯的浓度为0.5mol/L、冰醋酸的体积分数为5.0%、去离子水的体积分数为10%,在45℃下加热并搅拌均匀,得到溶胶,继续搅拌直至溶胶变为凝胶,将凝胶陈化12小时后,在100℃下干燥48小时,得到干凝胶;将干凝胶研磨后,在650℃下煅烧10小时,得到CdCu3Zr0.05Ti3.95O12陶瓷粉体。
2、向CdCu3Ti4O12陶瓷粉体中加入质量分数为5%的聚乙烯醇水溶液,研磨造粒,过120目筛后,用粉末压片机在6MPa压力下压制成11.5mm圆柱形坯件,将圆柱状坯件置于氧化锆平板上,用380分钟升温至500℃,保温2小时,然后以2℃/分钟的升温速率升温至990℃,恒温烧结15小时,随炉冷却至室温,得到高击穿场强钛酸锆铜镉巨介电陶瓷材料。
实施例2
本实施例中,按照CdCu3Zr0.10Ti3.90O12的化学计量比,将3.1159g Cd(NO3)2·4H2O、7.3212g Cu(NO3)2·3H2O、0.2336g ZrO(NO3)2·2H2O加入到10mL无水乙醇与去离子水的混合溶剂中配制成溶液A,将13.4mLTi(C4H9O)4加入到52.6mL无水乙醇中配制成溶液B;其他步骤与实施例1相同,得到高击穿场强钛酸锆铜镉巨介电陶瓷材料。
实施例3
本实施例中,按照CdCu3Zr0.20Ti3.80O12的化学计量比,将3.1159g Cd(NO3)2·4H2O、7.3212g Cu(NO3)2·3H2O、0.4671g ZrO(NO3)2·2H2O加入到10mL无水乙醇与去离子水的混合溶剂中配制成溶液A,将13.1mL Ti(C4H9O)4加入到52.9mL无水乙醇中配制成溶液B;其他步骤与实施例1相同,得到高击穿场强钛酸锆铜镉巨介电陶瓷材料。
对比例1
按照CdCu3Ti4O12的化学计量比,将3.1159g Cd(NO3)2·4H2O、7.3212g Cu(NO3)2·3H2O加入到10mL无水乙醇与去离子水的混合溶剂中配制成溶液A,将13.8mL Ti(C4H9O)4加入到52.2mL无水乙醇中配制成溶液B;其他步骤与实施例1相同,得到钛酸铜镉巨介电陶瓷材料。
分别将上述对比例1和实施例1~3制备的陶瓷材料表面打磨、抛光、超声、搽拭干净,在其上下表面分别涂覆银浆,置于马弗炉中840℃保温30分钟,自然冷却至室温。采用日本理学公司生产的D/max-2200X型射线衍射仪、安捷伦科技有限公司生产的4294A型精密阻抗分析仪、及英国雷尼绍公司生产的显微共焦激光拉曼光谱仪以及美国Radiant生产的铁电测试仪对其结构和性能进行表征测试,结果见图1~4。
由图1可见,对比例1和实施例1~3制备的陶瓷材料均为纯的类钙钛矿结构,无第二相生成。
由图2可见,对比例1和实施例1~3制备的陶瓷材料均呈现良好的巨介电性,在40Hz到100kHz范围内都保持很高的介电常数,其中实施例1即CdCu3Zr0.05Ti3.95O12陶瓷获得较优的介电性能,1kHz下,其相对介电常数为15082,介电损耗为0.07。
由图3可见,对比例1和实施例1~3制备的陶瓷材料在波长274cm-1、442cm-1、510cm-1、575cm-1均出现四个典型的拉曼光谱峰,分别对应于Fg(1)、Ag(1)、Ag(2)的TiO6旋转模式和Fg(3)O-Ti-O的反伸缩振动模式,其结果与XRD一致。
由图4可见,对比例1制备的陶瓷材料即CdCu3Ti4O12陶瓷材料的击穿场强约为1000V/cm,实施例1制备的陶瓷材料即CdCu3Zr0.05Ti3.95O12陶瓷材料击穿场强约为1530V/cm,相对于对比例1明显提高,有望应用于高储能密度动态随机存储器和高压电容器等电子市场应用。
Claims (6)
1.一种高击穿场强钛酸锆铜镉巨介电陶瓷材料,其特征在于:该陶瓷材料由CdCu3ZrxTi4-xO12表示的材料组成,其中x的取值为0.02~0.20;该陶瓷材料由下述方法制备得到:
(1)按照CdCu3ZrxTi4-xO12的化学计量比,将Cd(NO3)2•4H2O、Cu(NO3)2•3H2O、ZrO(NO3)2•2H2O加入到无水乙醇与去离子水的混合溶剂中配制成溶液A,将Ti(C4H9O)4加入到无水乙醇中配制成溶液B;将溶液A和溶液B混合,并加入冰醋酸,所得混合液中钛酸丁酯的浓度为0.3~0.7mol/L、冰醋酸的体积分数为2.5%~10%、去离子水的体积分数为5%~15%,在30~75℃下加热并搅拌均匀,得到溶胶,继续搅拌直至溶胶变为凝胶,将凝胶陈化后干燥,得到干凝胶;将干凝胶研磨后,在600~700℃下煅烧8~10小时,得到CdCu3ZrxTi4-xO12陶瓷粉体;
(2)将CdCu3ZrxTi4-xO12陶瓷粉体经造粒、压片、排胶后,在980~1000℃烧结10~15小时,得到高击穿场强钛酸锆铜镉巨介电陶瓷材料。
2.根据权利要求1所述的高击穿场强钛酸锆铜镉巨介电陶瓷材料,其特征在于:所述x的取值为0.05~0.10。
3.根据权利要求1所述的高击穿场强钛酸锆铜镉巨介电陶瓷材料,其特征在于:步骤(1)中,所得混合液中钛酸丁酯的浓度为0.5mol/L、冰醋酸的体积分数为5%、去离子水的体积分数为10%。
4.根据权利要求1所述的高击穿场强钛酸锆铜镉巨介电陶瓷材料,其特征在于:步骤(1)中,在40~50℃下加热并搅拌均匀,得到溶胶。
5.根据权利要求1所述的高击穿场强钛酸锆铜镉巨介电陶瓷材料,其特征在于:步骤(1)中,将干凝胶研磨后,在650℃下煅烧10小时。
6.根据权利要求1所述的高击穿场强钛酸锆铜镉巨介电陶瓷材料,其特征在于:步骤(2)中,在990℃下烧结15小时。
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