CN115612482A - 一种光-气协同变色材料及其合成方法和应用 - Google Patents
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Abstract
本发明公开了一种光‑气协同变色材料及其合成方法和应用。利用酸溶液浸泡层状钙钛矿材料,通过离子置换,部分氢离子取代层状钙钛矿中的碱金属离子,在无氧条件下通过紫外光照射发生光致变色,而有氧光照条件下可以瞬间恢复原始颜色。相对于其它光致变色材料,其优点为:一是传统光致变色材料只响应紫外光产生变色,对材料所处的气氛环境没有要求;二是该光‑气协同变色材料变色效率极高,响应快,并且可逆;三是对于氧气极为敏感,有氧条件下光照瞬间恢复原来的颜色。基于这些特点,该新型光‑气协同变色材料可用于气密性检测,防伪标码、保险柜防盗、可见光光催化剂等用途。
Description
技术领域
本发明涉及一种光-气协同变色材料及其合成方法和应用,属于光致变色和气致变色领域。
背景技术
光致变色材料(PC)是指化合物A在受到某一波长的光照时,可通过特定的化学反应生成结构和光谱性能不同的产物B,而在另一波长的光照或热的作用下,B又可逆地生成化合物 A 的现象。目前,光致变色材料被大量的研究,特别是集中在过度金属氧化物材料,通过对光致变色特性的研究,将其应用于汽车玻璃、激光印刷、显示器以及超高密度光信息存储及防伪辨伪等诸多行业。
气致变色材料(GC)在接触某些挥发性有机化合物后会发生颜色或发射率可逆的变化,由于其在化学传感器、发光二极管和环境监测仪等方面的广泛应用,近年来受到越来越多的关注。例如,当暴露在空气或无氧中时,一些气致变色材料可以分解气体分子并迅速恢复其原有的颜色。随着新型高稳定性蒸汽色体系统的发展,蒸汽色体材料在化学传感器和电子元件中得到更广泛的应用。
目前,光致变色材料和气致变色材料,只能单一的在光照或者气体存在下相应地发生颜色变化。传统光致变色材料只响应紫外光产生变色,对材料所处的气氛环境没有要求。另外,这些变色材料恢复的时间也比较长,普遍存在敏感度低和恢复原色时间较长等问题。
发明内容
为了解决上述现有技术存在的不足,本发明提供一种光-气协同致变色材料及其合成方法和应用,其中,在无氧条件下,该材料可在紫外光照射下迅速发生变色;而在氧气条件下进行光照,可瞬间变为原来颜色。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提出的一种光-气协同变色材料及其合成方法,利用酸溶液浸泡层状钙钛矿材料,通过离子置换,部分氢离子取代层状钙钛矿中的碱金属离子,包括以下步骤:
(1)将层状钙钛矿材料加入酸溶液中;
(2)恒温搅拌数天;
(3)离心洗涤;
(4)样品干燥。
较佳的,步骤(1)中,酸溶液为硝酸溶液或盐酸溶液,其浓度为1M~6M。
较佳的,步骤(1)中,层状钙钛矿材料需耐强酸,层状钙钛矿材料为K-Ca-Nb-O或Na-Ca-Nb-O材料。
较佳的,步骤(2)中,搅拌温度为20℃~80℃,搅拌时间为1天~1周。
较佳的,步骤(3)中,所述样品洗涤需要要用纯水和乙醇洗涤数次至PH=7。
较佳的,步骤(4)中,干燥温度为60℃~80℃,干燥时间不少于12h。
本发明还提供了上述光-气协同变色材料在光致变色和气致变色方面的用途。
较佳的,上述光-气协同变色材料的作为防伪材料的用途。
较佳的,上述光-气协同变色材料在真空密闭环境气密性排查中的用途。
较佳的,上述光-气协同变色材料在保险柜防盗中的用途。
较佳的,将所述光-气协同变色材料置于无氧环境中,经紫外光照射,发生光致变色;将变色样品暴露于空气中,恢复原色。
更佳的,将所述光-气协同变色材料置于无氧环境中,经紫外光照射,发生光致变色,可见光照射下不变色;将变色样品暴露于空气中,经光照(紫外光或可见光)可以瞬间恢复原色,无光照缓慢恢复原色。
更佳的,无氧环境为真空或者或其它不含氧的气氛。
本发明还提供了上述光-气协同变色材料作为可见光分解水制氢光催化剂的用途。
较佳的,该光-气协同变色材料在有氧环境下表现为白色只能吸收紫外光,经过无氧紫外光活化变成蓝色后,具有可见光吸收特性能够作为分解水制氢光催化剂。
与现有技术相比,本发明的优点是:一是传统光致变色材料只响应紫外光产生变色,对材料所处的气氛环境没有要求;二是该光-气协同变色材料变色效率极高,响应快,并且可逆;三是对于氧气极为敏感,有氧条件下光照瞬间恢复原来的颜色。与现有技术相比,实现了光-气协同变色。
附图说明
图1为本发明所述光-气协同变色材料的光-气协同变色过程。
图2 为本发明所述光-气协同变色材料的光-气协同致变色展示图。
图3 为本发明所述光-气协同变色材料经过无氧紫外照射后在可见光下分解水制氢的性能图。
具体实施方式
下面结合附图和实施例对本发明进行进一步阐述。
本发明的原理是:本申请通过将层状钙钛矿材料(K-Ca-Nb-O或Na-Ca-Nb-O)采用酸浸泡数天,其作用主要是把K-Ca-Nb-O或Na-Ca-Nb-O中的K或Na置换为H,这样层状钙钛矿材料的光电性能会提高很多,层状钙钛矿材料吸收光子后,激发出电子-空穴对,在无氧的环境下光生电子会将Nb还原为低价态,从而发生光致变色;而在有氧的环境下光生电子会优先与O2结合,所以不发生光致变色。结合图1,具体变色过程为:首先,该材料在有氧环境下光照(紫外光或可见光)不发生变色;其次,当该材料处于无氧环境下紫外光照,材料由白色变为蓝色;继而将变为蓝色的材料放入无氧无光照(或无氧可见光照)的环境下,保持蓝色不变;最后,将变为蓝色的材料暴露氧气在环境下,在光照(紫外光或可见光)恢复为白色。另外,该材料(不管变色前还是变色后)在无氧可见光光照下均不发生变色。
下面实施例中仅以KCa2Nb3O10层状钙钛矿材料作为代表,然其并非用以限定本发明的保护范围。
实施例1
一种新型光-气协同变色材料合成方法,过程如下:
(1)配制3M的硝酸溶液;(2)将层状钙钛矿材料KCa2Nb3O10(0.6g)加入硝酸溶液中;(3)40℃恒温搅拌3天;(4)用纯水和乙醇洗涤数次至PH=7;(5)放入烘箱60℃烘干24h;(6)回收样品,颜色为白色。光-气协同致变色性能如图2所示,把样品放入反应器后抽真空,放在太阳光下光照5秒变成蓝色;打开反应器使空气进入其中,瞬间变回白色。
实施例2
一种新型光-气协同变色材料应用方法,过程如下:
(1)配制3M的硝酸溶液;(2)将层状钙钛矿材料KCa2Nb3O10(0.6g)加入硝酸溶液中;(3)40℃恒温搅拌3天;(4)用纯水和乙醇洗涤数次至PH=7;(5)放入烘箱60℃烘干24h;(6)回收样品,颜色为白色。
将上述样品制作成薄膜附着在贴纸上。将贴纸贴在贵重物品保护罩内下层,保护罩内通入保护气排尽罩内空气,用紫外光灯照射贴纸,贴纸表面的产品薄膜变为蓝色;当保护罩气密性不好有空气进入后,贴纸由蓝色变为白色,表示工作人员需要检查展示品保护罩的气密性。
实施例3
一种新型光-气协同变色材料应用方法,过程如下:
(1)配制3M的硝酸溶液;(2)将层状钙钛矿材料KCa2Nb3O10(0.6g)加入硝酸溶液中;(3)40℃恒温搅拌3天;(4)用纯水和乙醇洗涤数次至PH=7;(5)放入烘箱60℃烘干24h;(6)回收样品,颜色为白色。
将上述样品制作成薄膜附着在贴纸上。将贴纸放入密封压缩袋中,放入保险柜内,保险柜内设置一紫外光源,只要保险柜非正常打开,就会触发紫外灯自动打开,贴纸瞬间变成蓝色,定期查看保险箱内贴纸便可以知道柜子是否被打开过。
实施例4
一种新型光-气协同变色材料应用方法,过程如下:
(1)配制3M的硝酸溶液;(2)将层状钙钛矿材料KCa2Nb3O10(0.6g)加入硝酸溶液中;(3)40℃恒温搅拌3天;(4)用纯水和乙醇洗涤数次至至PH=7;(5)放入烘箱60℃烘干24h;(6)回收样品,颜色为白色。
将P25粉体制备成薄膜覆盖在衬底(如:FTO、ITO玻璃)表面,再把上述样品粉体印刷成标码喷涂在P25材料表面,待覆盖平整后表面呈现纯白色;把密钥放入无氧环境后采用紫外光照射,表面的标码立刻显现为蓝色,暴露空气立马消失变成白色。
实施例5
一种新型光-气协同变色材料合成方法,过程如下:
(1)配制3M的硝酸溶液;(2)将层状钙钛矿材料KCa2Nb3O10(0.6g)加入硝酸溶液中;(3)40℃恒温搅拌3天;(4)用纯水和乙醇洗涤数次至PH=7;(5)放入烘箱60℃烘干24h;(6)回收样品,颜色为白色。
取0.2g上述样品和100mL去离子水放入光催化制氢反应器后抽真空,先在300W氙灯下全波段照射5分钟,待颜色变为蓝色后,再在氙灯上加上420nm截止滤光片(中教金源cutoff-420nm)滤掉紫外光,由于上述材料(不管变色前还是变色后)在无氧可见光光照下均不发生变色,所以在可见光照射下溶液颜色一直保持蓝色,可见光分解水制氢的性能如图3所示,可以看出这种光-气协同变色材料在有氧环境下表现为白色只能吸收紫外光,但在经过无氧紫外光活化变成蓝色后便具有了可见光吸收特性且能够满足分解水制氢的化学电位要求,实现可见光分解水制氢。
Claims (10)
1.一种光-气协同变色材料的合成方法,其特征在于,包括以下步骤:
(1)将层状钙钛矿材料加入酸溶液中;
(2)恒温搅拌数天;
(3)离心洗涤;
(4)样品干燥。
2.如权利要求1所述的方法,其特征在于,酸溶液为硝酸溶液或盐酸溶液,其浓度为1M~6M;层状钙钛矿材料为K-Ca-Nb-O或Na-Ca-Nb-O材料;搅拌温度为20℃~80℃,搅拌时间为1天~1周;干燥温度为60℃~80℃,干燥时间不少于12h。
3.如权利要求1或2所述的方法制备的光-气协同变色材料。
4.如权利要求1或2所述的方法制备的光-气协同变色材料在光致变色和气致变色方面的用途。
5.如权利要求4所述的用途,其特征在于,将所述光-气协同变色材料置于无氧环境中,经紫外光照射,发生光致变色;将变色样品暴露于空气中,恢复原色。
6.如权利要求4所述的用途,其特征在于,将所述光-气协同变色材料置于无氧环境中,经紫外光照射,发生光致变色;将变色样品暴露于空气中,经光照(紫外光或可见光)瞬间恢复原色,无光照缓慢恢复原色。
7.如权利要求1或2所述的方法制备的光-气协同变色材料作为防伪材料的用途。
8.如权利要求1或2所述的方法制备的光-气协同变色材料在真空密闭环境气密性排查中的用途。
9.如权利要求1或2所述的方法制备的光-气协同变色材料在保险柜防盗中的用途。
10.如权利要求1或2所述的方法制备的光-气协同变色材料作为可见光分解水制氢光催化剂的用途。
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