CN116639727A - 一种改性钒酸铋基氧离子导体材料及其制备方法 - Google Patents
一种改性钒酸铋基氧离子导体材料及其制备方法 Download PDFInfo
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- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 53
- 239000001301 oxygen Substances 0.000 title claims abstract description 53
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000010416 ion conductor Substances 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 39
- -1 Modified bismuth vanadate Chemical class 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 150000001768 cations Chemical class 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 15
- 239000010949 copper Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical group [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910052797 bismuth Inorganic materials 0.000 claims description 9
- 239000011651 chromium Substances 0.000 claims description 9
- 229910052720 vanadium Inorganic materials 0.000 claims description 9
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 2
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 12
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- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 5
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
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- 208000001408 Carbon monoxide poisoning Diseases 0.000 description 1
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- 238000010248 power generation Methods 0.000 description 1
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- C01G31/006—Compounds containing, besides vanadium, two or more other elements, with the exception of oxygen or hydrogen
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Abstract
本发明涉及一种中低温区具有高氧离子电导率的氧离子导体材料及其制备方法。所述材料的化学组成表示式为:Bi4(V1‑yMy)xO11+z,其中M为金属阳离子,1.7≤x≤2.2且x≠2,0<y≤0.3,z取决于所述金属阳离子组成电中性平衡。本发明制备的改性钒酸铋基Bi4(V1‑yMy)xO11+z材料,其制备工艺简易、成本低,结构稳定、电导率高,其中Bi4(V0.9Cu0.1)1.9O10.465在300℃时,晶粒电导率在10‑2S/cm量级,陶瓷总离子电导率达1.2×10‑3S/cm,高于当前最高文献报道值约1个数量级,可满足中低温氧化物燃料电池及氧传感器的应用要求。
Description
技术领域
本发明属于新型固态氧离子导体与固态电解质技术领域,涉及在中低温固态氧化物燃料电池电解质、氧传感器用的固态离子导体材料及制备方法,具体涉及一种改性钒酸铋基氧离子导体材料及其制备方法。
背景技术
固态氧化物燃料电池(Solid Oxide Fuel Cell,SOFC)作为一种新型、清洁的能源转换装置,因其全固态结构耐久性强、转换效率高(60-80%)、燃料种类多、电极无需贵金属、无一氧化碳中毒威胁等优点而备受关注,在发电、交通、空间宇航等领域具有广阔的应用前景,被称为21世纪的绿色能源。夹在两个电极之间的致密电解质层是固态氧化物燃料电池的关键材料,负责载流子输运和隔绝两电极的反应气体。氧化钇稳定氧化锆(YSZ)电解质在800-1000℃下离子电导率可达到0.1S/cm,是目前普遍商用的氧离子导体,但其高工作温度引起的电极烧结、密封成本高、电解质与电极材料之间的界面扩散和热不稳定性等问题限制以YSZ为电解质的SOFC电池的应用。降低SOFC的操作温度、保持相/热稳定性并且达到所需电导率水平是SOFC电解质研究开发的主要目标。设计和开发中低温(300-750℃)下的新型固态氧离子导体是实现中低温固态氧化物燃料电池应用的关键。
化合物Bi4V2O11是由(Bi2O2)2+层和类钙钛矿(VO3.5□0.5)2-层交替形成,□表示本征氧空位,晶体结构中存在的氧空位使得该类材料在中低温下具有良好的离子电导率,其中Cu掺杂形成的四方相Bi4V1.8Cu0.2O10.7是目前报道中低温下离子电导率最高的化合物,在300℃时晶粒电导率达到了1×10-3S/cm,但因陶瓷晶界电阻较大,材料总体电导率约为10-4S/cm量级,在实际应用中仍待进一步提高,以实现更好的电学性能。另外,氧离子导体材料在氧传感器中也具有广泛的应用,中低温高电导率的氧离子导体材料对于提高传感器的性能也具有重要价值。
发明内容
为了避免现有技术的不足之处,本发明提出一种改性钒酸铋基氧离子导体材料及其制备方法,本发明的改性钒酸铋基氧离子导体材料在300℃及以上温度具有高氧离子电导率。
按照本发明的一个方面,提供一种改性钒酸铋基氧离子导体材料,其特征在于所述改性钒酸铋基氧离子导体材料的化学组成表示式为:Bi4(V1-yMy)xO11+z,其中M为金属阳离子,选自铜、铬、银、镁、钛、镍、锌等中的一种或几种,其中1.7≤x≤2.2且x≠2,0<y≤0.3,z取决于所述M阳离子组成电中性平衡。
其中,优选地,所述M为铜,并且x=1.9,y=0.1。
按照本发明的另一个方面,提供上述改性钒酸铋基氧离子导体材料的制备方法,包括如下步骤:
(1)以含铋化合物、含钒化合物和含金属M化合物作为原料,按上述化学组成表示式中铋、钒和金属M元素占比进行配料,然后混合均匀得到混合物;
(2)将混合物烘干后煅烧;
(3)将煅烧后的粉末以聚乙烯醇(PVA)溶液为粘结剂压制成型后烧结,得到所述改性钒酸铋基氧离子导体材料。
其中,所述方法还可以包括在混合前将含铋化合物、含钒化合物和含金属M化合物原料在100~500℃下干燥2-12小时。
其中,所述混合是在行星球磨机中进行的,球料比为2:1,球磨介质为无水乙醇,转速为300r/min,球磨时间2~12小时。
其中,所述煅烧的煅烧温度为500~800℃,煅烧时间为12~96小时。
其中,所述烧结的烧结温度为750~900℃,烧结时间为0.5~6小时。
优选地,步骤(1)中含铋化合物为氧化铋,含钒化合物为五氧化二钒,含金属M化合物为金属M的氧化物或者碳酸盐。
本发明制备的改性钒酸铋基氧离子导体材料Bi4(V1-yMy)xO11+z结构稳定,电导率高,其中Bi4(V0.9Cu0.1)1.9O10.465在300℃时,晶粒电导率在10-2S/cm量级,陶瓷总离子电导率达1.2×10-3S/cm,高于当前最高文献报道值约1个数量级,其原料成本低、制备工艺简单,可满足中低温氧化物燃料电池及氧传感器的应用要求。
附图说明
图1为按照本发明实施例1的改性钒酸铋基氧离子导体材料的X射线衍射图谱;
图2为按照本发明实施例1的改性钒酸铋基氧离子导体材料的扫描电镜图;
图3示出了按照本发明实施例1的改性钒酸铋基氧离子导体材料的温度-电导率数据。
具体实施方式
为了更清楚地理解本发明的目的、技术方案及优点,以下结合附图及实施例,对本发明进行进一步详细说明。
本发明提供的改性钒酸铋基氧离子导体材料的化学式为Bi4(V1-yMy)xO11+z,其中M为金属阳离子,选自铜、铬、银、镁、钛、镍、锌等中一种或几种金属元素,其中x的数值在1.7到2.2之间且x≠2,y的数值大于0并且小于等于0.3,z由M阳离子组成决定。
所述的改性钒酸铋基氧离子导体材料的制备方法,包括如下步骤:
(1)将含铋化合物、含钒化合物和含金属M化合物原料在100~500℃下干燥2~12小时。
(2)将步骤(1)中的原料干粉按化学式Bi4(V1-yMy)xO11+z称量配料。
(3)将步骤(2)中称量的粉料在球磨机中混合,球料比为2:1,无水乙醇为球磨介质,转速为300r/min,球磨2~12小时。
(4)将步骤(3)获得的浆料在烘箱中烘干。
(5)将步骤(4)中得到的混合料在500~800℃煅烧12~96小时。
(6)将步骤(5)煅烧的粉末添加聚乙烯醇(PVA)溶液作为粘结剂压制成型,在750~900℃烧结0.5~6小时,即得到本发明的高氧离子电导率的改性钒酸铋基氧离子导体材料。
实施例1:
制备Bi4(V0.9Cu0.1)1.9O10.465氧离子导体材料
步骤如下:
(1)以Bi2O3、V2O5和CuO为原料,在500℃干燥12小时,按Bi4(V0.9Cu0.1)1.9O10.465中各金属元素的比例进行称量配料;将称量好的粉料用球磨机混合均匀,球磨介质为无水乙醇,转速为300r/min,球磨时间为12小时;将混合均匀的浆料在烘箱中烘干。
(2)烘干的混合原料在650℃煅烧48小时;将处理好的粉料进行研磨,接着在650℃继续煅烧48小时。
(3)煅烧之后的粉料以聚乙烯醇(PVA)溶液为粘结剂在压片机中压制成型,在大气气氛下进行烧结,烧结温度为830℃,烧结时间为2小时;即得到所述高氧离子电导率的四方相结构氧离子导体陶瓷。
本实施制备的Bi4(V0.9Cu0.1)1.9O10.465氧离子导体陶瓷XRD谱图如图1所示,物相鉴定与晶体结构精修表明,制备的陶瓷为单一的四方相结构。图2是实施例Bi4(V0.9Cu0.1)1.9O10.465的扫面电镜图,表明制备陶瓷样品具有高的致密度。用交流阻抗分析仪进行对陶瓷导电性的评价,如图3所示,在300℃时,晶粒电导率达到1.1×10-2S/cm,总电导率达1.2×10-3S/cm。
实施例2:
制备Bi4(V0.9Cr0.1)1.75O10.2氧离子导体材料
(1)以Bi2O3、V2O5和Cr2O3为原料,在500℃干燥4小时,按Bi4(V0.9Cr0.1)1.75O10.2中各金属元素的比例进行称量配料;将称量好的粉料用球磨机混合均匀,球磨介质为无水乙醇,转速为300r/min,球磨时间为10小时;将混合均匀的浆料在烘箱中烘干。
(2)烘干的混合原料在660℃煅烧48小时;将处理好的粉料进行研磨,接着在660℃继续煅烧48小时。
(3)煅烧之后的粉料以聚乙烯醇(PVA)溶液为粘结剂在压片机中压制成型,在大气气氛下进行烧结,烧结温度为870℃,烧结时间为4小时;即得到所述高氧离子电导率的氧离子导体陶瓷。在300℃时,晶粒电导率为0.8×10-2S/cm,总电导率达1.1×10-3S/cm。
实施例3:
制备Bi4(V0.9Zn0.1)1.8O10.23氧离子导体材料
(1)以Bi2O3、V2O5和ZnCO3为原料,在400℃干燥6小时,按Bi4(V0.9Zn0.1)1.8O10.23中各金属元素的比例进行称量配料;将称量好的粉料用球磨机混合均匀,球磨介质为无水乙醇,转速为300r/min,球磨时间为5小时;将混合均匀的浆料在烘箱中烘干。
(2)烘干的混合原料在630℃煅烧20小时;将处理好的粉料进行研磨,接着在630℃继续煅烧20小时。
(3)煅烧之后的粉料以聚乙烯醇(PVA)溶液为粘结剂在压片机中压制成型,在大气气氛下进行烧结,烧结温度为850℃,烧结时间为3小时;即得到所述高氧离子电导率的氧离子导体材料陶瓷。在300℃时,晶粒电导率为0.9×10-2S/cm,总电导率达1.1×10-3S/cm。
实施例4:
制备Bi4(V0.7Cu0.3)2.2O10.51氧离子导体材料
(1)以Bi2O3、V2O5和CuCO3为原料,在100℃干燥12小时,按Bi4(V0.9Cr0.1)1.75O10.2中各金属元素的比例进行称量配料;将称量好的粉料用球磨机混合均匀,球磨介质为无水乙醇,转速为300r/min,球磨时间为2小时;将混合均匀的浆料在烘箱中烘干。
(2)烘干的混合原料在800℃煅烧6小时;将处理好的粉料进行研磨,接着在800℃继续煅烧6小时。
(3)煅烧之后的粉料以聚乙烯醇(PVA)溶液为粘结剂在压片机中压制成型,在大气气氛下进行烧结,烧结温度为900℃,烧结时间为0.5小时;即得到所述高氧离子电导率的氧离子导体陶瓷。在300℃时,晶粒电导率为0.4×10-2S/cm,总电导率达0.9×10-3S/cm。
实施例5:
制备Bi4(V0.95Mg0.025Cu0.025)2.1O10.23氧离子导体材料
(1)以Bi2O3、V2O5和Cr2O3为原料,在400℃干燥12小时,按Bi4(V0.9Cr0.1)1.75O10.2中各金属元素的比例进行称量配料;将称量好的粉料用球磨机混合均匀,球磨介质为无水乙醇,转速为300r/min,球磨时间为10小时;将混合均匀的浆料在烘箱中烘干。
(2)烘干的混合原料在550℃煅烧48小时;将处理好的粉料进行研磨,接着在550℃继续煅烧48小时。
(3)煅烧之后的粉料以聚乙烯醇(PVA)溶液为粘结剂在压片机中压制成型,在大气气氛下进行烧结,烧结温度为800℃,烧结时间为6小时;即得到所述高氧离子电导率的氧离子导体陶瓷。在300℃时,晶粒电导率为0.2×10-2S/cm,总电导率达0.8×10-3S/cm。
除上述实施例外,其他组分的改性钒酸铋基氧离子导体材料的制备也均能实现。
Claims (8)
1.一种改性钒酸铋基氧离子导体材料,其中所述改性钒酸铋基氧离子导体材料的化学组成表示式为:Bi4(V1-yMy)xO11+z,其中M为金属阳离子,选自铜、铬、银、镁、钛、镍、锌等中的一种或几种,其中1.7≤x≤2.2且x≠2,0<y≤0.3,z取决于所述金属阳离子组成电中性平衡。
2.按照权利要求1所述的改性钒酸铋基氧离子导体材料,其中所述M为铜,并且x=1.9,y=0.1。
3.一种按照权利要求1所述的改性钒酸铋基氧离子导体材料的制备方法,包括如下步骤:
(1)以含铋化合物、含钒化合物和含金属M化合物作为原料,按所述化学组成表示式中铋、钒和金属M元素占比进行配料,然后混合均匀得到混合物;
(2)将混合物烘干后煅烧;
(3)将煅烧后的粉末以聚乙烯醇溶液为粘结剂压制成型后烧结,得到所述改性钒酸铋基氧离子导体材料。
4.按照权利要求3所述的方法,其中所述方法还包括在混合前将含铋化合物、含钒化合物和含金属M化合物原料在100~500℃下干燥2~12小时。
5.按照权利要求3所述的方法,其中所述混合是在行星球磨机中进行的,球料比为2:1,球磨介质为无水乙醇,转速为300r/min,球磨时间2~12小时。
6.按照权利要求3所述的方法,其中所述煅烧的煅烧温度为500~800℃,煅烧时间为12~96小时。
7.按照权利要求3所述的方法,其中所述烧结的烧结温度为750~900℃,烧结时间为0.5~6小时。
8.按照权利要求3所述的方法,其中所述含铋化合物为氧化铋,含钒化合物为五氧化二钒,含金属M化合物为金属M的氧化物或者碳酸盐。
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