CN114643078A - 一种纸基有机-无机双z型异质结的制备方法 - Google Patents
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Abstract
本发明提供了一种纸基有机‑无机双Z型异质结的制备方法,制备步骤如下:以金纸芯片为基底,采用水热生长技术在纸芯片表面生长硫化铋,随后使用温和高效的方法原位合成COF‑318‑TiO2,将合成的COF‑318‑TiO2滴加到纸基硫化铋后,通过一步退火法形成Bi2S3‑共轭聚合物‑TiO2异质结。所制备的异质结具有高稳定性、高吸光率,大大提高了光电性能,为有机‑无机复合材料在柔性基底上的应用建立良好的基础。
Description
技术领域
本发明涉及Bi2S3-共轭聚合物-TiO2异质结的制备方法,属于无机与有机结合的纳米材料制备领域。
背景技术
晶体共价有机框架(COF)已被证明是各种光催化反应的优秀光催化剂,其优点如下:i)丰富的有机建筑单元为具有可调带隙的COF提供了巨大机会;ii)COFs中广泛的π-共轭骨架可以确保光生载流子的迁移率。但合成COF涉及到超低温冷冻以及动态真空等比较苛刻的条件,限制了其在纸基传感方向的应用。本工作开发了一种新的方法制备有机纳米材料,拓宽COF材料在柔性基底上的应用。
在各种光活性材料中,二氧化钛(TiO2)和硫化铋(Bi2S3)在光化学应用催化剂方面显示出良好的潜力。但是由于TiO2有限的可见光吸收以及Bi2S3的空穴和电子的快速复合限制了其大规模应用。无机和有机半导体在异质结中的结合被认为是克服每种材料类别局限性的一种有前途的方法。因此通过二者与COF组成双Z型异质结可以改善电荷分离、增加载流子的寿命,从而提高光催化剂的光电转换效率。
纸张成本低、简单、重量轻、灵活、多路复用能力强、减少分析时间,并且不需要标记,其三维基质可为样品生长提供巨大的表面积,其中,基于微流控纸的光电化学分析装置实现了光激发源和光电流检测信号的完全分离,可有效降低检测背景,提高光电化学分析方法的检出限。因此,以纸芯片作为基底设计的生物传感器具有非常大的应用潜力。本项研究采用水热生长技术在纸纤维表面生长Bi2S3,结合原位反应法合成COF-TiO2,将合成的COF-TiO2滴加到纸基Bi2S3后,通过一步退火法形成Bi2S3-共轭聚合物-TiO2异质结。所形成的双Z型异质结具有高稳定性、高光吸光率,为纸基材料的新应用奠定了基础。
发明内容
本发明要解决的技术问题是实现一种Bi2S3-共轭聚合物-TiO2异质结的简单、高效、温和的制备方法。
为了解决上述技术问题,本发明是通过以下措施来实现的:一种高效、温和的Bi2S3-共轭聚合物-TiO2异质结制备方法,其特征是包括以下步骤:
(1)将色谱纸裁剪为1 cm×5 cm纸片,滴加金种子液自然干燥,重复三次,继而滴加生长液,在滴加生长液后30 min用去离子水冲洗浮金,室温晾干得到金纸芯片;
(2)制备纸基硫化铋:
水热法制备纸基硫化铋:称取0.25 g硫脲和0.5 g硝酸铋溶解到50 mL去离子水,搅拌1 h,将步骤(1)制备的金纸芯片与15 mL混合溶液放入50 mL聚四氟乙烯高压釜中,145°C条件下反应12 h,冷却至室温,用去离子水冲洗三次,于60 °C的烘箱中干燥过夜,得到纸基硫化铋;
(3)制备COF-318-TiO2:
原位反应法合成COF-318-TiO2:将25 mg 2,3,6,7,10,11-六羟基苯并菲、20 mg2,3,5,6-四氟-4-吡啶碳三腈和16 mg TiO2、0.4 mL 1,4-二氧六环、0.4 mL 1,3,5-三甲苯混合后,超声处理20 min,随后滴加0.072 mL三甲胺,超声处理10 min;于120 °C的氮气气氛下加热混合物,保持48 h;过滤后用二甲基甲酰胺和四氢呋喃分别洗涤三次,最后,在130°C真空下干燥过夜得到COF-318-TiO2;
(4)制备纸基Bi2S3-共轭聚合物-TiO2异质结:
将步骤(3)制得的样品取0.1 g加入10 mL乙醇溶液,滴入0.05 mL的萘酚,然后进行5 min的超声波处理,将混合液滴加到步骤(2)所制备的纸基硫化铋上,随后在130 °C下退火45 min,即可得到纸基Bi2S3-共轭聚合物-TiO2异质结。
本发明的有益效果:
(1)COF与半导体共价连接,为光催化剂提供了高稳定性。此异质结可以通过界面控制来增强内部电场,提高了光生载流子的迁移效率,实现了高效的光吸收。
(2)有机骨架和半导体之间的有效共价耦合使光生电子在有机官能团和半导体对应物之间有效转移,提高了电荷分离,同时提高了电荷载流子的氧化还原能力,实现了较高的光电转换效率。
具体实施方式
为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。
实施例1
(1)将色谱纸裁剪为1 cm×5 cm纸片,滴加金种子液自然干燥,重复三次,继而滴加生长液,在滴加生长液后30 min用去离子水冲洗浮金,室温晾干得到金纸芯片;
(2)制备纸基硫化铋:
水热法制备纸基硫化铋:称取0.25 g硫脲和0.5 g硝酸铋溶解到50 mL去离子水,搅拌1 h,将步骤(1)制备的金纸芯片与15 mL混合溶液放入50 mL聚四氟乙烯高压釜中,145°C条件下反应12 h,冷却至室温,用去离子水冲洗三次,于60 °C的烘箱中干燥过夜,得到纸基硫化铋;
(3)制备COF-318-TiO2:
原位反应法合成COF-318-TiO2:将25 mg 2,3,6,7,10,11-六羟基苯并菲、20 mg2,3,5,6-四氟-4-吡啶碳三腈和16 mg TiO2、0.4 mL 1,4-二氧六环、0.4 mL 1,3,5-三甲苯混合后,超声处理20 min,随后滴加0.072 mL三甲胺,超声处理10 min;于120 °C的氮气气氛下加热混合物,保持48 h;过滤后用二甲基甲酰胺和四氢呋喃分别洗涤三次,最后,在130°C真空下干燥过夜得到COF-318-TiO2;
(4)制备纸基Bi2S3-共轭聚合物-TiO2异质结:
将步骤(3)制得的样品取0.1 g加入10 mL乙醇溶液,滴入0.05 mL的萘酚,然后进行5 min的超声波处理,将混合液滴加到步骤(2)所制备的纸基硫化铋上,随后在130 °C下退火45 min,即可得到纸基Bi2S3-共轭聚合物-TiO2异质结。
Claims (1)
1.一种高效、温和的Bi2S3-共轭聚合物-TiO2异质结制备方法,其特征在于该方法的制备步骤如下:
(1)将色谱纸裁剪为1 cm×5 cm纸片,滴加金种子液自然干燥,重复三次,继而滴加生长液,在滴加生长液后30 min用去离子水冲洗浮金,室温晾干得到金纸芯片;
(2)制备纸基硫化铋:
水热法制备纸基硫化铋:称取0.25 g硫脲和0.5 g硝酸铋溶解到50 mL去离子水,搅拌1h,将步骤(1)制备的金纸芯片与15 mL混合溶液放入50 mL聚四氟乙烯高压釜中,145 °C条件下反应12 h,冷却至室温,用去离子水冲洗三次,于60 °C的烘箱中干燥过夜,得到纸基硫化铋;
(3)制备COF-318-TiO2:
原位反应法合成COF-318-TiO2:将25 mg 2,3,6,7,10,11-六羟基苯并菲、20 mg 2,3,5,6-四氟-4-吡啶碳三腈和16 mg TiO2、0.4 mL 1,4-二氧六环、0.4 mL 1,3,5-三甲苯混合后,超声处理20 min,随后滴加0.072 mL三甲胺,超声处理10 min;于120 °C的氮气气氛下加热混合物,保持48 h;过滤后用二甲基甲酰胺和四氢呋喃分别洗涤三次,最后,在130 °C真空下干燥过夜得到COF-318-TiO2;
(4)制备纸基Bi2S3-共轭聚合物-TiO2异质结:
将步骤(3)制得的样品取0.1 g加入10 mL乙醇溶液,滴入0.05 mL的萘酚,然后进行5min的超声波处理,将混合液滴加到步骤(2)所制备的纸基硫化铋上,随后在130 °C下退火45 min,即可得到纸基Bi2S3-共轭聚合物-TiO2异质结。
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