CN108380223A - 一种基于TiO2/SiO2骨架的四元光子晶体材料及其制备方法 - Google Patents
一种基于TiO2/SiO2骨架的四元光子晶体材料及其制备方法 Download PDFInfo
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- 239000000377 silicon dioxide Substances 0.000 claims abstract description 72
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 61
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 61
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- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 1
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- 150000002343 gold Chemical class 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 229910021505 gold(III) hydroxide Inorganic materials 0.000 description 1
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- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
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- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
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Abstract
本发明公开了一种基于TiO2/SiO2骨架的四元光子晶体材料,包括反蛋白石结构TiO2/SiO2骨架、金纳米颗粒和反蛋白石结构CdS。所述反蛋白石结构TiO2/SiO2骨架具有成分和尺寸连续可调的特性;所述金纳米颗粒分布于整个四元光子晶体材料中,具有电子传输协同作用和表面等离子体共振效应;所述反蛋白石结构CdS具有拓展和增强可见光吸收特性。该四元光子晶体材料可表现出优异的光催化性能;且涉及的制备方法简单,产物尺寸和组成可调,适合推广应用。
Description
技术领域
本发明涉及纳米光催化材料技术领域,具体涉及一种基于TiO2/SiO2骨架的四元光子晶体材料及其制备方法。
背景技术
光子晶体作为一种三维有序多孔材料,能大大增加材料的比表面积,使光与材料充分接触,并且由于光在材料内部的多重散射,材料对光的吸收效率得以提高。与此同时,在接近光子带隙的边缘位置,光子群速度由于慢光效应会显著降低,从而进一步增加了材料与光接触的时间,提高了材料对光的整体利用率。因此制备出具有光子晶体结构的光催化剂对于提升光催化性能具有重要意义。
目前,现有的提升光子晶体光催化性能的方法为采用复合手段,如:将光子晶体与染料分子复合,利用染料的光敏性提升对光的吸收与利用(G.Z.Liao,S.Chen,X.Quan,H.Chen and Y.B.Zhang,Environ.Sci.Technol.,2010,44,3481.);将光子晶体与贵金属复合,利用表面等离子体共振效应与慢光子晶体效应耦合,增强光子与材料的相互作用等。
然而光子晶体与染料复合之后,在光催化反应的过程中,染料不稳定,易被降解;贵金属价格昂贵,提高了催化剂的成本,但是负载少量的贵金属又不利于性能的提升,并且不能扩展光吸收范围;金属氧化物构成的光子晶体本身透光性、亲水性差,影响了性能的提升。
发明内容
本发明的目的是针对现有技术存在的不足,提供一种基于TiO2/SiO2骨架的四元光子晶体材料及其制备方法;该四元光子晶体材料以具有反蛋白石结构的TiO2/SiO2为骨架,并依次负载金纳米颗粒和CdS而成,可表现出优异的光催化性能;且涉及的制备方法简单,产物尺寸和组成可调,适合推广应用。
为实现上述目的,本发明采用的技术方案为:
一种基于TiO2/SiO2骨架的四元光子晶体材料,它自内而外依次包括具有反蛋白石结构的TiO2/SiO2骨架、金纳米颗粒和具有反蛋白石结构的CdS。
上述方案中,所述基于TiO2/SiO2骨架的四元光子晶体材料具有规则的多孔结构,包括大孔、介孔,其中大孔呈面心立方密堆形式,大孔尺寸为250~380nm;大孔之间孔孔相连,形成介孔,介孔尺寸为11~17nm。
上述方案中,所述金纳米颗粒尺寸为25~35nm。
上述方案中,所述四元光子晶体材料中(SiO2+TiO2)、Au、CdS之间的质量比为(70~80):1:(19~29)。
优选的,所述TiO2/SiO2骨架由TiO2包覆在反蛋白石结构的SiO2骨架表面而成,其中TiO2含量为1~2.5wt%。
更优选的,所述TiO2/SiO2骨架中二氧化钛含量为2~2.5wt%。
上述一种基于TiO2/SiO2骨架的四元光子晶体材料的制备方法,它包括如下步骤:
1)将聚苯乙烯小球置于水中进行超声分散,然后在40~60℃进行烘干,得到具有蛋白石结构的聚苯乙烯硬模板;
2)配制二氧化硅溶胶,将步骤1)所得聚苯乙烯硬模板置于铺设滤纸的漏斗中,将二氧化硅溶胶倒入聚苯乙烯硬模板中,收集在重力作用下透过滤纸的溶胶,并重新倒入聚苯乙烯硬模板中,重复上述收集和倒入步骤,直至配制的二氧化硅溶胶完全附着在聚苯乙烯硬模板中,然后进行老化处理,得二氧化硅干凝胶;然后进行煅烧,得具有反蛋白石结构的SiO2骨架;
3)将所得SiO2骨架置于铺设滤纸的漏斗中,配制二氧化钛溶胶,然后采用步骤2)所述步骤,将二氧化钛溶胶倒入SiO2骨架中,直至二氧化钛溶胶完全附着在SiO2骨架中,然后依次进行老化、煅烧,得具有反蛋白石结构的TiO2/SiO2复合骨架;
4)将TiO2/SiO2复合骨架置于氯金酸溶液中,采用晶种法,在TiO2/SiO2复合骨架表面生长纳米金粒子,得具有反蛋白石结构的Au/TiO2/SiO2复合材料;
5)将所得Au/TiO2/SiO2复合材料加入镉源溶液中搅拌10-30min,然后加入硫源溶液继续搅拌1-2.5h,得基于TiO2/SiO2骨架的四元光子晶体材料(CdS/Au/TiO2/SiO2)。
上述方案中,所述聚苯乙烯小球采用无皂乳液聚合法制备而成,其尺寸大小为330~450nm。
上述方案中,所述二氧化硅溶胶中SiO2的质量浓度为15~20%;通过将硅源与混合溶剂均匀混合而成;其中混合溶剂由乙醇、水和盐酸按5:1:1的体积比混合而成。
上述方案中,所述硅源可选用分析纯正硅酸四乙酯;所述盐酸选用质量浓度为36.0~38.0%的盐酸。
上述方案中,所述二氧化硅溶胶与聚苯乙烯硬模板的质量比为1:(2~8)。
上述方案中,所述二氧化钛溶胶中TiO2的质量浓度为0.7~1.9%;通过将钛源与混合溶剂均匀混合而成;其中混合溶剂由乙醇、水和盐酸按5:1:1的体积比混合而成。
上述方案中,所述二氧化钛溶胶与SiO2骨架的质量比为1~1.3:1。
上述方案中,所述钛源可选用钛酸异丙酯,所述盐酸选用质量浓度为36.0~38.0%的分析纯盐酸。
上述方案中,所述煅烧步骤采用程序升温制度,依次为:加热至280~320℃保温50~60min、加热至380~420℃保温50~60min、加热至500-550℃保温50~60min,然后降至室温;升温速率为2~4℃/min。
上述方案中,所述晶种法为:对氯金酸溶液进行加热,然后加入一定量柠檬酸钠溶液保温10-15min,得纳米晶晶种,再加入一定量柠檬酸钠溶液,继续保温范围1~1.5h。
上述方案中,所述加热温度为150~160℃。
上述方案中,所述氯金酸溶液的浓度为0.05~0.2mg/ml;TiO2/SiO2复合骨架与氯金酸溶液的质量比为1:(150~200)。
上述方案中,所述晶种法得到的反应体系中,氯金酸与柠檬酸钠总的摩尔比为1:7,第一次柠檬酸钠添加的量占总柠檬酸钠的1/2。
上述方案中,所述镉源溶液的浓度为0.03~0.05M与Au/TiO2/SiO2复合材料的质量比为(30~42):1;硫源溶液的浓度为0.03~0.05M,与Au/TiO2/SiO2复合材料的质量比为30~42:1。
上述方案中,所述镉源可选用硝酸镉等;硫源可选用硫化钠等。
本发明的原理为:
本发明首先采用硬模板法制备具有反蛋白石结构的TiO2/SiO2复合骨架,在增强可见光吸收和亲水性能的同时,将TiO2同时作为光催化剂(产生光生电子)和电子传输骨架,有利于提升所得复合材料的光催化性能和导电性能;然后在TiO2/SiO2复合骨架上负载纳米金颗粒,金纳米颗粒分布于整个光子晶体材料中,具有电子传输协同作用和表面等离子体共振效应,通过表面等离子体效应与慢光子效应耦合,增强对光的吸收;最后包覆一层CdS,CdS呈反蛋白石结构,CdS具有拓展和增强可见光吸收特性,并与TiO2形成Z-scheme的能带结构,有利于光生电子和空穴的分离,进一步增强对光的吸收。
与现有技术相比,本发明的有益效果为:
1)本发明首先采用硬模板法制备具有反蛋白石结构的TiO2/SiO2复合骨架,并依次进行纳米金粒子负载和CdS层的包覆,得具有反蛋白石结构的四元光子晶体材料,具有优异的光催化性能和使用性能。
2)本发明涉及的制备方法简单,反应条件温和,孔道结构和组成连续可控,适应性广。
附图说明
图1为实施例1所得产物的扫描电镜图片;
图2为实施例2所得产物的扫描电镜图片;
图3为实施例1、3获得的基于不同钛含量TiO2/SiO2骨架的四元光子晶体材料的X射线衍射图谱
图4为实施例1、3获得的基于不同钛含量TiO2/SiO2骨架的四元光子晶体材料的紫外可见吸收光谱;
图5、6为实施例1、3获得的基于不同钛含量TiO2/SiO2骨架的四元光子晶体材料的吸脱附曲线和孔径分布图;
图7为实施例3获得的基于不同钛含量TiO2/SiO2骨架的四元光子晶体材料的接触角图。
图8为实施例1、3和对比例1所得产物单位时间、单位质量TiO2条件下在可见光下的产氢对比图。
具体实施方式
为了更清楚地说明本发明,下面结合优选实施例和附图对本发明做进一步的说明。本领域技术人员应当理解,下面所具体描述的内容是说明性的而非限制性的,不应以此限制本发明的保护范围。
实施例1
一种基于TiO2/SiO2骨架的四元光子晶体材料,其制备方法包括以下步骤:
1)将390ml去离子水加入500ml两口或三口烧瓶中密封,在油浴锅上加热至70℃,保温30min;然后加入事先去除了阻聚剂的30ml苯乙烯,保持30min;称取0.325g过二硫酸钾溶于10ml去离子水,待完全溶解后倒入烧瓶中,同时插上装有高纯氮气的气球,排除烧瓶内的空气;反应10h后取出,进行旋转蒸发,得单分散的聚苯乙烯小球乳液(聚苯乙烯小球尺寸大小为340+10nm);将200~400ml聚苯乙烯小球乳液加入200~400ml去离子水中,超声分散3min,然后置于烘箱中,在40℃温度条件下进行干燥,得尺寸为340+10nm的具有蛋白石结构的聚苯乙烯硬模板;
2)在10ml烧杯中先后加入5ml无水乙醇,1ml浓度为36%的盐酸,5ml硅酸四乙酯,1ml水,搅拌10min,得到二氧化硅溶胶(SiO2的质量浓度为18.59%);取5g 340nm聚苯乙烯硬模板放置在布氏漏斗中的定性滤纸上,布氏漏斗下端连接离心管;然后将配制好的二氧化硅溶胶,倒入聚苯乙烯硬模板中,待漏斗中溶胶流干,再将离心管中收集的溶胶倒入漏斗中,如此反复循环多次,直至溶胶全部附着在硬模板中;然后老化1天,得到二氧化硅干凝胶;将老化后的二氧化硅干凝胶放入马弗炉中依次由室温加热至300℃保温60min、加热至400℃保温60min、加热至550℃保温60min,升温速率为2℃/min,将后将至室温,以去除聚苯乙烯硬模板,得到具有反蛋白石结构的SiO2骨架;
3)在10ml烧杯中先后加入5ml无水乙醇,1ml浓度为36%的盐酸,51μl钛酸异丙酯和1ml水,搅拌10min;得到二氧化钛溶胶(TiO2的质量浓度为0.75%);然后采用步骤2)所述步骤,将6.17g二氧化钛溶胶倒入5g SiO2骨架中,直至二氧化钛溶胶完全附着在SiO2骨架中;然后老化1天,得到二氧化钛干凝胶;将老化后的凝胶放入马弗炉中依次由室温加热至300℃保温60min、加热至400℃保温60min、加热至550℃保温60min,升温速率为2℃/min,将后将至室温,得到具有反蛋白石结构的TiO2/SiO2复合骨架;
4)取0.5g TiO2/SiO2复合骨架加入圆底烧瓶,加入1ml 10mg/ml的氯金酸溶液,在160℃搅拌并加热30min,然后滴入1.5ml 10g/l柠檬酸三钠溶液,15min后再滴入1.5ml10g/l柠檬酸三钠溶液,继续加热1h,冷却、抽滤、干燥后,得到金纳米颗粒负载的反蛋白石结构(具有反蛋白石结构的Au/TiO2/SiO2复合材料);
5)取0.5g负载了金颗粒的反蛋白石骨架,放入20ml 0.05M硝酸镉溶液中搅拌30min,然后将20ml 0.05M硫化钠溶液倒入硝酸镉溶液中,搅拌2.5h,抽滤干燥后,制备得到基于TiO2/SiO2骨架四元光子晶体材料(记为CATS-IO-1%-250,1%表示Ti在钛硅骨架中的钛含量为1%,250表示PS小球烧结之后的大孔孔径尺寸为250nm)。
图1为本实施例所得产物的扫描电镜图,图中可以看出所得产物呈规则的孔道结构,孔的排列呈现ABCABC……的方式,为面心立方密堆积,并且沿着(111)面排列,孔道结构完好;
图3为本实施例所得产物的XRD衍射图,峰位与标准卡片匹配表明,材料兼具有锐钛矿TiO2和立方相CdS的衍射峰;图4为所得产物的紫外可见吸收光谱,其中,200-350nm波段的鼓包对应TiO2的吸收,350-600nm波段的鼓包对应CdS的吸收,虽然锐钛矿本身的吸收边应该在400nm左右,但是由于锐钛矿含量太少,所以会显得锐钛矿的吸收显得蓝移,而Au纳米颗粒的吸收在550nm左右,被CdS的吸收拖尾边掩盖;结合XRD和紫外可见吸收光谱测试结果,说明本发明所得产物为CdS/Au/TiO2/SiO2的四元复合材料。
图5为本实施所得产物的N2吸脱附曲线,其中在0.8-1.0之间有回滞环,为Ⅱ类吸附等温线;图6为孔径分布图,表明其孔径分布主要集中在介孔,介孔尺寸为11、17nm,回滞环与介孔相对应;比表面积表见表1。开放大孔方便催化剂与外部的水的接触,有利于物质的流通扩散性,并且大孔的结构有利于光的多次反射,增加光与催化剂作用的时间;介孔有利于催化反应进行,同时有利于水在催化剂内部的扩散与传输。
本实施例所得产物在可见光下产氢性能测试结果见图8(单位时间、单位质量TiO2),结果表明,骨架中二氧化钛掺杂量为1%的四元光子晶体的产氢量为2.01mmol·h-1·gTiO2 -1。
实施例2
一种基于TiO2/SiO2骨架的四元光子晶体材料,其制备方法与实施例1大致相同,不同之处在于:将“30ml苯乙烯”改为“16ml苯乙烯”,“0.325g过二硫酸钾”改为“0.255g过二硫酸钾”可得到直径为450nm左右的PS小球,“51μl钛酸异丙酯”改为“5ml钛酸异丙酯”经过煅烧可得孔径为375nm左右TiO2/SiO2骨架四元光子晶体材料(CdS/Au/TiO2/SiO2记为CATS-IO-1%-375)。
图2为本实施例获得产物的扫描电镜图,图中可以看出所得产物呈规则的多孔结构,孔的排列呈现ABCABC……,为面心立方密堆积,并且沿着(111)面排列,孔道结构完好。
实施例3
一种基于TiO2/SiO2骨架的四元光子晶体材料,其制备方法与实施例1大致相同,不同之处在于:将“5ml钛酸异丙酯”改为“129μl钛酸异丙酯”,可得到钛含量为2.5%的基于TiO2/SiO2骨架的四元光子晶体材料(记为CATS-IO-2.5%-250)。
本实施例所得产物的比表面积测试数据见表2。
图3为本实施例所得产物的XRD衍射图,峰位与标准卡片匹配表明,材料兼具有锐钛矿TiO2和立方相CdS的衍射峰;图4为紫外可见吸收光谱,200-350nm波段的鼓包对应TiO2的吸收,350-600nm波段的鼓包对应CdS的吸收,虽然锐钛矿本身的吸收边应该在400nm左右,但是由于锐钛矿含量太少,所以会显得锐钛矿的吸收显得蓝移,而Au纳米颗粒的吸收在550nm左右,被CdS的吸收拖尾边掩盖;图5为N2吸脱附曲线在0.8-1.0之间有一段回滞环,为Ⅱ类吸附等温线;图6为孔径分布图表明其孔径分布主要集中介孔,可能和大孔相互之间接触的介孔被部分TiO2堵塞有关系;图8为接触角图,结合表2的左右接触角表面,表明其平均接触角为79.9°,为亲水表面,说明我们通过调节TiO2的量实现了改善亲水性的目的。
本实施例所得产物在可见光下产氢性能测试结果见图8(单位时间、单位质量TiO2),结果表明,骨架中二氧化钛掺杂量为2.5%的四元光子晶体的产氢量为4.04mmol·h-1·gTiO2 -1。
对比例
一种三元光子晶体材料,其制备方法与实施例1大致相同,不同之处在于:删除步骤2),将步骤3)中的SiO2骨架替换为PS(聚苯乙烯)硬模板;制备得到CdS/Au/TiO2三元光子晶体材料,记为CAT-IO-250。
将本对比例所得产物与实施例1和实施例3所得四元光子晶体材料进行可见光下产氢性能对比,结果见图8。结果表明,本发明所得四元光子晶体材料具有优异的光催化性能。
表1
表2
显然,本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定,对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动,这里无法对所有的实施方式予以穷举,凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之列。
Claims (10)
1.一种基于TiO2/SiO2骨架的四元光子晶体材料,它自内而外依次包括具有反蛋白石结构的TiO2/SiO2骨架、金纳米颗粒和具有反蛋白石结构的CdS。
2.根据权利要求1所述的四元光子晶体材料,其特征在于,它具有规则的多孔结构,包括大孔和介孔,其中大孔呈面心立方密堆方式,大孔尺寸为250~380nm;大孔之间孔孔相连,并形成介孔,介孔尺寸为11~17nm。
3.根据权利要求1所述的四元光子晶体材料,其特征在于,所述金纳米颗粒尺寸为25~35nm。
4.根据权利要求1所述的四元光子晶体材料,其特征在于,所述TiO2/SiO2骨架由TiO2包覆在反蛋白石结构的SiO2骨架表面而成,其中二氧化钛占TiO2/SiO2骨架的质量百分比为1~2.5%。
5.权利要求1所述基于TiO2/SiO2骨架的四元光子晶体材料的制备方法,其特征在于,它包括如下步骤:
1)将聚苯乙烯小球置于水中进行超声分散,然后在40~60℃进行烘干,得具有蛋白石结构的聚苯乙烯硬模板;
2)配制二氧化硅溶胶,将步骤1)所得聚苯乙烯硬模板置于铺设滤纸的漏斗中,将二氧化硅溶胶倒入聚苯乙烯硬模板中,收集在重力作用下透过滤纸的溶胶,并重新倒入聚苯乙烯硬模板中,重复上述收集和倒入步骤,直至配制的二氧化硅溶胶完全附着在聚苯乙烯硬模板中,然后进行老化处理,得二氧化硅干凝胶;然后进行煅烧,得具有反蛋白石结构的SiO2骨架;
3)将所得SiO2骨架置于铺设滤纸的漏斗中,配制二氧化钛溶胶,然后采用步骤2)所述步骤,将二氧化钛溶胶倒入SiO2骨架中,直至二氧化钛溶胶完全附着在SiO2骨架中,然后依次进行老化、煅烧,得具有反蛋白石结构得TiO2/SiO2复合骨架;
4)将TiO2/SiO2复合骨架置于氯金酸溶液中,再加入柠檬酸钠,采用晶种法,在TiO2/SiO2复合骨架表面生长纳米金粒子,得具有反蛋白石结构的Au/TiO2/SiO2复合材料;
5)将所得Au/TiO2/SiO2复合材料加入镉源溶液中搅拌,然后加入硫源溶液继续搅拌,得基于TiO2/SiO2骨架的四元光子晶体材料。
6.根据权利要求5所述的制备方法,其特征在于,所述聚苯乙烯小球的尺寸大小为330~450nm。
7.根据权利要求5所述的制备方法,其特征在于,所述二氧化硅溶胶中SiO2的质量浓度为15~20%;二氧化硅溶胶与聚苯乙烯硬模板的质量比为15~20:2。
8.根据权利要求5所述的制备方法,其特征在于,所述二氧化钛溶胶中TiO2的质量浓度为0.7~1.9%;二氧化钛溶胶与SiO2骨架的质量比为1~1.3:1。
9.根据权利要求5所述的制备方法,其特征在于,所述氯金酸溶液的浓度为0.05~0.2mg/ml;TiO2/SiO2复合骨架与氯金酸溶液的质量比为1:(150~200)。
10.根据权利要求5所述的制备方法,其特征在于,所述镉源溶液的浓度为0.03~0.05M与Au/TiO2/SiO2复合材料的质量比为(30~42):1;硫源溶液的浓度为0.03~0.05M,与Au/TiO2/SiO2复合材料的质量比为30~42:1。
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