CN106007714B - 用于铝及铝合金熔体中定氢探头固体电解质及制备方法 - Google Patents
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Abstract
本发明公开了一种用于铝及铝合金熔体中定氢探头固体电解质,所述电解质的通式为BaCe1‑x‑y‑zInxSnyYzO3‑a,其中,0.01≤x≤0.25,0<y≤0.25,0<z≤0.25。还公开了其制备方法。本发明提供的用于铝及铝合金熔体中定氢探头固体电解质,电导率高,化学稳定性好。通过本发明固体电解质制备得到的固体电解质管具有优良的力学性能。本发明的固体电解质加入铟之后,提高质子导电性,加入Y2O3后增加了固体电解质材料的稳定性及抗热震性能,从而提高了电解质的灵敏度,降低了误差,扩展了应用范围。本发明的制备方法,步骤简单,易操作实现,反应条件易控制,减少烧结能耗,保障了固体电解质的性能稳定。
Description
技术领域
本发明涉及用于铝及铝合金熔体中定氢探头固体电解质及制备方法,具体属于定氢探头用电解质技术领域。
背景技术
铝及铝合金铸件容易产生气孔、夹杂等缺陷,使其内在质量大幅度下降。铝及其合金的液态质量又直接影响到铸件的质量。因氢含量过高造成的废品率约占全部铝铸件废品的一半。铝及其合金在凝固时由于含氢造成诸如力学性能、内部质量大为下降等许多缺陷,氢在铝中不但造成宏观缺陷,而且影响组织结构,对于强度、疲劳、韧性、耐腐、阳极氧化等一系列性能都有影响。因此测氢尤为重要。
目前在铝及铝合金熔体中定氢探头化学传感器中,常使用CaZr0.9In0.1O3-a材料作为固体电解质,用氢气混合气体为参比电极。实际使用过程中,由于CaZr0.9In0.1O3-a固体电解质材料,稳定性低,从而使灵敏度降低,误差增加,现场应用受到限制。而对于BaCeO3基固体电解质材料,电导率不够高,化学稳定性低。因此,发明一种电导率高、稳定性好的适用于铝及铝合金熔体中定氢探头的固体电解质,显得尤为必要。
发明内容
为解决现有技术的不足,本发明的目的在于提供一种用于铝及铝合金熔体中定氢探头固体电解质及制备方法,所得定氢探头用固体电解质具有较高的电导率,其制备方法步骤简单易操作。
为了实现上述目标,本发明采用如下的技术方案:
用于铝及铝合金熔体中定氢探头固体电解质,所述电解质的通式为BaCe1-x-y- zInxSnyYzO3-a,其中,0.01≤x≤0.25,0<y≤0.25,0<z≤0.25。
前述用于铝及铝合金熔体中定氢探头固体电解质,具体地,所述电解质为BaCe0.80In0.05Sn0.05Y0.10O3-a。
前述用于铝及铝合金熔体中定氢探头固体电解质的制备方法,包括以下步骤:
(1)按通式中摩尔比称取预先脱水干燥后的In2O3和SnO2粉末混合均匀,随后烧结、粉碎得到预粉体;
(2)按通式中摩尔比称取预先脱水干燥后的BaCO3、CeO2和Y2O3,加入预粉体中混合均匀,得到混合粉体,再进行烧结,冷却后即得。
前述用于铝及铝合金熔体中定氢探头固体电解质的制备方法,步骤(1)中,In2O3和SnO2粉末混合采用机械混合均匀,预粉体颗粒中径粒度小于50微米。
前述用于铝及铝合金熔体中定氢探头固体电解质的制备方法,步骤(1)中,以3℃~10℃/min的升温速率加热至600~1000℃下进行烧结3h~5h。
前述用于铝及铝合金熔体中定氢探头固体电解质的制备方法,步骤(2)中,混合采用机械混合,所得混合粉体颗粒中径粒度为10~25微米。粒度适中保障了成分均匀,易于充分反应,同时粒度易控制,不会造成操作成本的增加。
前述用于铝及铝合金熔体中定氢探头固体电解质的制备方法,步骤(2)中,以5℃~8℃/min的升温速率加热至1300~1500℃下进行烧结2h~4h。减少了烧结能耗,同时保障所得固体电解质符合定氢探头使用要求。
用于铝及铝合金熔体中定氢探头固体电解质在定氢装置中的应用。有效提升了定氢装置的灵敏度,扩大了测氢的检测范围。
在铝及铝合金熔体中进行测氢时,对定氢探头要求较高。而定氢探头中重要的组成部分为固体电解质管。固体电解质管的首要条件是高的致密度。而影响固体电解质管致密度的影响因素包括:固体电解质粉末特性,烧结温度,升温速率,成型压力等。采用本发明中的固体电解质,在粉体粒径分布均匀基础上,经过高温致密化烧结,可消除粉体引起的密度差异,降低孔隙率,提升固体电解质管的致密度。在同等烧结条件下,与传统固体电解质相比,采用本发明的固体电解质,所得固体电解质管的致密度有明显提升,孔隙率可降低20%~25%,机械性能提升约25%~30%。
本发明的固体电解质是一种具有足够的化学稳定性、抗热震性能和较高的电导特性的复合材料。采用的五原料体系,合理改变原料的混合比例,从而得到具有较高的电导率的电解质。本发明的固体电解质加入铟之后,提高质子导电性,与传统固体电解质相比,本发明的电解质电导率提升15%~20%。
此外,本发明的用于铝及铝合金熔体中定氢探头用固体电解质中,由于添加了Y2O3,稳定性及抗热震性能都得以提升,在测试温度范围内可提高使用寿命一倍以上次数。
本发明的有益之处在于:本发明提供的用于铝及铝合金熔体中定氢探头固体电解质,电导率高、化学稳定性好、抗热震性能好。通过本发明固体电解质制备得到的固体电解质管具有优良的力学性能。本发明的固体电解质加入铟之后,提高质子导电性,加入Y2O3后增加了固体电解质材料的稳定性及抗热震性能,从而提高了电解质的灵敏度,降低了误差,扩展了应用范围。本发明的制备方法,步骤简单,易操作实现,反应条件易控制,减少了烧结能耗,保障了固体电解质的性能稳定。
具体实施方式
以下结合具体实施例对本发明作进一步的介绍。
实施例1
用于铝及铝合金熔体中定氢探头固体电解质,所述电解质的通式为BaCe1-x-y- zInxSnyYzO3-a,其中,x=0.05,y=0.05,z=0.1。
用于铝及铝合金熔体中定氢探头固体电解质的制备方法,包括以下步骤:
(1)按通式中摩尔比称取预先脱水干燥后的In2O3和SnO2粉末采用混合均匀,随后以10℃/min的升温速率加热至600℃下进行烧结3h,粉碎得到预粉体;预粉体颗粒中径粒度小于50微米;
(2)按通式中摩尔比称取预先脱水干燥后的BaCO3、CeO2和Y2O3,加入预粉体中混合均匀,得到混合粉体,混合粉体颗粒中径粒度为10微米;再以8℃/min的升温速率加热至1500℃下进行烧结2h,冷却后即得。
实施例2
用于铝及铝合金熔体中定氢探头固体电解质,所述电解质的通式为BaCe1-x-y- zInxSnyYzO3-a,其中,x=0.25,y=0.25,z=0.25。
用于铝及铝合金熔体中定氢探头固体电解质的制备方法,包括以下步骤:
(1)按通式中摩尔比称取预先脱水干燥后的In2O3和SnO2粉末采用机械混合混合均匀,随后以3℃/min的升温速率加热至1000℃下进行烧结5h,粉碎得到预粉体;预粉体颗粒中径粒度小于50微米;
(2)按通式中摩尔比称取预先脱水干燥后的BaCO3、CeO2和Y2O3,加入预粉体中采用机械混合均匀,得到混合粉体,混合粉体颗粒中径粒度为25微米;再以5℃/min的升温速率加热至1300℃下进行烧结4h,冷却后即得。
实施例3
用于铝及铝合金熔体中定氢探头固体电解质,所述电解质的通式为BaCe1-x-y- zInxSnyYzO3-a,其中,x=0.01,y=0.1,z=0.1。
用于铝及铝合金熔体中定氢探头固体电解质,包括以下步骤:
(1)按通式中摩尔比称取预先脱水干燥后的In2O3和SnO2粉末采用机械混合混合均匀,随后以9℃/min的升温速率加热至700℃下进行烧结4.5h,粉碎得到预粉体;预粉体颗粒中径粒度小于50微米;
(2)按通式中摩尔比称取预先脱水干燥后的BaCO3、CeO2和Y2O3,加入预粉体中采用机械混合均匀,得到混合粉体,混合粉体颗粒中径粒度为22微米;再以6℃/min的升温速率加热至1450℃下进行烧结3.5h,冷却后即得。
实施例4
用于铝及铝合金熔体中定氢探头固体电解质,所述电解质的通式为BaCe1-x-y- zInxSnyYzO3-a,其中,x=0.08,y=0.12,z=0.23。
用于铝及铝合金熔体中定氢探头固体电解质的制备方法,包括以下步骤:
(1)按通式中摩尔比称取预先脱水干燥后的In2O3和SnO2粉末采用机械混合混合均匀,随后以6℃/min的升温速率加热至800℃下进行烧结4h,粉碎得到预粉体;预粉体颗粒中径粒度小于50微米;
(2)按通式中摩尔比称取预先脱水干燥后的BaCO3、CeO2和Y2O3,加入预粉体中采用机械混合均匀,得到混合粉体,混合粉体颗粒中径粒度为15微米;再以7℃/min的升温速率加热至1400℃下进行烧结3h,冷却后即得。
实施例5
用于铝及铝合金熔体中定氢探头固体电解质,所述电解质的通式为BaCe1-x-y- zInxSnyYzO3-a,其中,x=0.20,y=0.21,z=0.17。
用于铝及铝合金熔体中定氢探头固体电解质的制备方法,包括以下步骤:
(1)按通式中摩尔比称取预先脱水干燥后的In2O3和SnO2粉末采用机械混合混合均匀,随后以5℃/min的升温速率加热至900℃下进行烧结3.5h,粉碎得到预粉体;预粉体颗粒中径粒度小于50微米;
(2)按通式中摩尔比称取预先脱水干燥后的BaCO3、CeO2和Y2O3,加入预粉体中采用机械混合均匀,得到混合粉体,混合粉体颗粒中径粒度为20微米;再以8℃/min的升温速率加热至1350℃下进行烧结2.2h,冷却后即得。
实施例1~5中的定氢探头用固体电解质可应用于定氢装置中。
Claims (2)
1.用于铝及铝合金熔体中定氢探头固体电解质,其特征在于:所述电解质为BaCe0.80In0.05Sn0.05Y0.10O3-a;
所述的用于铝及铝合金熔体中定氢探头固体电解质的制备方法,包括以下步骤:
(1)按通式中摩尔比称取预先脱水干燥后的In2O3和SnO2粉末采用机械混合均匀,随后以3℃~5℃/min的升温速率加热至600~1000℃下进行烧结3h~5h,然后粉碎得到预粉体;
(2)按通式中摩尔比称取预先脱水干燥后的BaCO3、CeO2和Y2O3,加入预粉体中混合均匀,得到混合粉体,再以5℃~8℃/min的升温速率加热至1300~1500℃下进行烧结2h~4h,冷却后即得,
所述步骤(1)中,预粉体颗粒中径粒度小于50微米,
所述步骤(2)中,混合采用机械混合,所得混合粉体颗粒中径粒度为10~25微米。
2.如权利要求1所述的用于铝及铝合金熔体中定氢探头固体电解质在定氢装置中的应用。
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