CN107879318B - 一种气泡剥离法制备类石墨相氮化碳纳米片的方法 - Google Patents
一种气泡剥离法制备类石墨相氮化碳纳米片的方法 Download PDFInfo
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Abstract
本发明涉及一种气泡剥离法制备类石墨相氮化碳纳米片的方法,是以三聚氰胺为前驱体材料、碳酸氢钠水溶液做电解液,采用脉冲电压电解法进行电解,收集类石墨相氮化碳粉末,经洗涤、离心分离、真空冷冻干燥,制得终产物类石墨相氮化碳纳米片,纳米片厚度为1.67nm,产物纯度达99.8%,可在光照条件下催化降解有机物,可在光伏产品中使用,是先进的制备类石墨相氮化碳纳米片的方法。
Description
技术领域
本发明涉及一种气泡剥离法制备类石墨相氮化碳纳米片的方法、属光催化材料制备及应用的技术领域。
背景技术
新兴的光催化技术由于能够利用太阳光分解水制氢气和降解环境污染物,使其成为解决能源危机和环境污染问题的研究热点;传统的光催化剂存在光响应范围窄、太阳能利用率低、量子效率低的问题,严重限制了它们的应用;近年来,由碳元素和氮元素组成的有机聚合物半导体光催化剂——类石墨相氮化碳,由于禁带宽度较窄,对可见光有响应,而且具有较高的化学稳定性、易改性和高的光催化性能;类石墨相氮化碳制备过程简单,可通过直接加热三聚氰胺、尿素和双氰氨制得,可在光催化领域应用。
但是类石墨相氮化碳也存在一些不足之处,例如比表面积较小、带隙宽度相对较大、对可见光响应的范围较窄、光生电子和空穴分离程度不高、容易复合;这些不足制约了类石墨相氮化碳在光催化领域和能源领域的应用;由于类石墨相氮化碳是一种层状化合物,层状结构之间靠范德华力连接,所以可通过剥离法得到二维纳米片结构,得到的二维纳米片由于比表面积增大使其表面活性位点增多,由于晶体的各向异性,随着纳米片厚度减小使载流子迁移到表面的垂直距离缩短;此外,由于量子限制效应,使纳米片具有独特的物理化学性能,比如增大的带隙可以提高电荷载体的氧化还原能力;类石墨相氮化碳制备成纳米片后光吸收和光响应体相有増强;通过热侵蚀、超声剥离、化学剥离以及利用浓盐酸、浓硝酸方法剥离类石墨相氮化碳,可以成功获得比表面积高、光催化活性好、应用范围广的类石墨相氮化碳纳米片;上述制备过程既费时又低效,而且存在安全隐患;因此,需要开发一种绿色方法来制备类石墨相氮化碳纳米片,此技术还在科学研究中。
发明内容
发明目的
本发明的目的是针对背景技术的不足和弊端,采用电化学计时电流法电解碳酸氢钠电解液产生气体,利用气泡剥离类石墨相氮化碳,制得类石墨相氮化碳纳米片,以获得比表面积高、光催化活性好、应用范围广的类石墨相氮化碳纳米片。
技术方案
本发明使用的化学物质为:三聚氰胺、泡沫镍片、甘汞片、碳酸氢钠、去离子水,其组合准备用量如下:以克、毫升、毫米为计量单位
制备方法如下:
(1)制备类石墨相氮化碳细粉
将三聚氰胺10g±0.01g置于坩埚中,将坩埚放于热处理炉中,加热温度550℃,保温2h,然后停止加热,随炉冷却至25℃,成类石墨相氮化碳;
研磨、过筛,热处理后将类石墨相氮化碳用玛瑙研钵、研棒进行研磨,然后用300目筛网过筛,研磨,过筛反复进行,成类石墨相氮化碳细粉;
(2)制备工作电极
将泡沫镍片平展置于钢质平板上,将类石墨相氮化碳细粉0.5g±0.01g均匀铺在泡沫镍片上部,然后将另一泡沫镍片压在类石墨相氮化碳细粉上部,并压实,成工作电极;
(3)制备对电极
将另一泡沫镍片平展置于另一钢质平板上,将类石墨相氮化碳细粉0.5g±0.01g均匀铺在泡沫镍片上部,然后将另一泡沫镍片压在类石墨相氮化碳细粉上部,并压实,成对电极;
(4)制备碳酸氢钠电解液
称取碳酸氢钠7g±0.01g,量取去离子水100mL±0.01mL,加入烧杯中,用搅拌器搅拌5min,成0.833mol/L的碳酸氢钠电解液;
(5)制备类石墨相氮化碳纳米片
类石墨相氮化碳纳米片的制备是在电解槽内进行的,是在电化学工作站脉冲电压电解作用下,在工作电极、对电极、参比电极作用下完成的;
①将配置的碳酸氢钠电解液加入电解槽内;
②将工作电极、对电极、参比电极垂直置于电解槽内,电解液要淹没工作电极、对电极、参比电极;
③开启电化学工作站,采用计时电流法来提供脉冲电压,高电位0.8V(相对于甘汞片电位)、低电位-0.8V(相对于甘汞片电位),脉冲步数320,脉冲持续时间6s,总时间1920s;脉冲电压对工作电极、对电极内的类石墨相氮化碳细粉进行电解;
④电解后,将工作电极、对电极内的类石墨相氮化碳细粉进行收集,并置于烧杯中;
⑤洗涤,将烧杯中的类石墨相氮化碳细粉加入去离子水100mL,搅拌清洗10min,成洗涤液;
⑥离心分离,将洗涤液加入离心机的离心管内,进行离心分离,分离转速8000r/min,分离时间10min;
分离后,留存沉淀物,并去洗涤液;
⑦真空冷冻干燥,将沉淀物置于石英容器中,然后置于真空冷冻干燥箱中冷冻干燥,冷冻干燥温度-80℃,真空度2Pa,冷冻干燥时间10h,冷冻干燥后得类石墨相氮化碳纳米片;
(6)检测、分析、表征
对制备的类石墨相氮化碳纳米片的形貌、成份、化学物理性能进行检测、分析、表征;
用扫描电子显微镜对类石墨相氮化碳纳米片进行形貌和结构分析;
用原子力显微镜对类石墨相氮化碳纳米片厚度进行测量;
用X射线衍射仪对类石墨相氮化碳纳米片进行衍射强度分析;
用紫外-可见分光光度计对类石墨相氮化碳纳米片进行紫外可见光吸收分析;
结论:类石墨相氮化碳纳米片为淡黄色粉体片层状结构,层与层之间呈堆垛状,剥离后的类石墨相氮化碳纳米片厚度为1.67nm,产物纯度达99.8%;
(7)产物储存
对制备的类石墨相氮化碳纳米片储存于棕色透明的玻璃瓶中,密闭避光保存,要防潮、防晒、防酸碱盐侵蚀,储存温度20℃,相对湿度10%。
有益效果
本发明与背景技术相比具有明显的先进性,是以三聚氰胺作为前驱体材料、碳酸氢钠水溶液做电解液,采用脉冲电压进行电解,收集类石墨相氮化碳纳米片粉末,经洗涤、离心分离、真空冷冻干燥,制得类石墨相氮化碳纳米片,此制备方法工艺先进,数据精确翔实,制备的类石墨相氮化碳纳米片呈片状结构,纳米片厚度为1.67nm,产物纯度达99.8%,可在光催化应用中使用,是先进的制备类石墨相氮化碳纳米片的方法。
附图说明
图1、类石墨相氮化碳电解状态图
图2、类石墨相氮化碳与类石墨相氮化碳纳米片形貌对比图
图3、类石墨相氮化碳与类石墨相氮化碳纳米片原子力对比图谱
图4、类石墨相氮化碳与类石墨相氮化碳纳米片X射线衍射强度对比图谱
图5、类石墨相氮化碳与类石墨相氮化碳纳米片紫外可见光吸收对比图谱
图中所示,附图标记清单如下:
1、电化学工作站,2、脉冲电解槽,3、顶盖,4、显示屏,5、指示灯,6、电源开关,7、脉冲电源控制器,8、第一吊丝,9、第二吊丝,10、第三吊丝,11、碳酸氢钠电解液,12、工作电极,13、参比电极,14、对电极。
具体实施方式
以下结合附图对本发明做进一步说明:
图1所示,为类石墨相氮化碳电解状态图,各部位置、连接关系要正确,按量配比,按序操作。
制备使用的化学物质的量值是按预先设置的范围确定的,以克、毫升、毫米为计量单位。
制备类石墨相氮化碳纳米片是在脉冲电解槽内进行的,是在脉冲电源电解、在碳酸氢钠电解液内、在工作电极、参比电极、对电极作用下完成的;
电化学工作站1为立式,在电化学工作站1上部为脉冲电解槽2,脉冲电解槽2上部为顶盖3;顶盖3下部设有第一吊丝8、第二吊丝9、第三吊丝10,并深入脉冲电解槽2内;第一吊丝8下部连接工作电极12,第二吊丝9下部连接参比电极13,第三吊丝10下部连接对电极14;脉冲电解槽2内盛放碳酸氢钠电解液11,碳酸氢钠电解液11要淹没工作电极12、参比电极13、对电极14;在电化学工作站1上设有显示屏4、指示灯5、电源开关6、脉冲电源控制器7。
图2所示,为类石墨相氮化碳与类石墨相氮化碳纳米片对比形貌图,图a、图c为类石墨相氮化碳形貌图,图中可见,类石墨相氮化碳由纳米片相互堆叠而成,是典型的叠层层状结构,图b、图d为类石墨相氮化碳纳米片形貌图,图中可见,类石墨相氮化碳纳米片为片层结构,呈现蓬松的层状结构,类石墨相氮化碳纳米片出现卷曲。
图3所示,为类石墨相氮化碳与类石墨相氮化碳纳米片原子力对比图谱,图a、图b为类石墨相氮化碳原子力图谱,图中可见,类石墨相氮化碳厚度为14.59nm,图c、图d为类石墨相氮化碳纳米片原子力图谱,图中可见,类石墨相氮化碳纳米片厚度为1.67nm。
图4所示,为类石墨相氮化碳与类石墨相氮化碳纳米片X射线衍射强度对比图谱,纵坐标为衍射强度,横坐标为衍射角,(a)为类石墨相氮化碳X射线衍射图谱,(b)为类石墨相氮化碳纳米片X射线衍射图谱,图中可见,类石墨相氮化碳纳米片(100)和(002)晶面接近消失或强度减弱,是由于颗粒的变小和片层结构变薄所致。
图5所示,为类石墨相氮化碳与类石墨相氮化碳纳米片紫外可见光吸收对比图谱,(a)为类石墨相氮化碳紫外可见光吸收图谱,(b)为类石墨相氮化碳纳米片紫外可见光吸收图谱,图中可见,类石墨相氮化碳纳米片出现了蓝移,是由于量子限制效应的作用,进一步说明类石墨相氮化碳颗粒的变小和片层结构变薄。
Claims (2)
1.一种气泡剥离法制备类石墨相氮化碳纳米片的方法,其特征在于:
使用的化学物质为:三聚氰胺、泡沫镍片、甘汞片、碳酸氢钠、去离子水,其组合准备用量如下:以克、毫升、毫米为计量单位
三聚氰胺:C3H6N6 10 g ± 0.01 g
泡沫镍片:Ni 4片 30 mm × 10 mm × 1 mm
甘汞片 1片 30 mm × 10 mm × 1 mm
碳酸氢钠:NaHCO3 7 g ± 0.01g
去离子水:H2O 1000 mL ± 10 mL
制备方法如下:
(1)制备类石墨相氮化碳细粉
将三聚氰胺10 g ± 0.01 g置于坩埚中,将坩埚放于热处理炉中,加热温度550℃,保温2 h,然后停止加热,随炉冷却至25℃,成类石墨相氮化碳;
研磨、过筛,热处理后将类石墨相氮化碳用玛瑙研钵、研棒进行研磨,然后用300目筛网过筛,研磨,过筛反复进行,成类石墨相氮化碳细粉;
(2)制备工作电极
将泡沫镍片平展置于钢质平板上,将类石墨相氮化碳细粉0.5 g ± 0.01 g均匀铺在泡沫镍片上部,然后将另一泡沫镍片压在类石墨相氮化碳细粉上部,并压实,成工作电极;
(3)制备对电极
将另一泡沫镍片平展置于另一钢质平板上,将类石墨相氮化碳细粉0.5 g ± 0.01 g均匀铺在泡沫镍片上部,然后将另一泡沫镍片压在类石墨相氮化碳细粉上部,并压实,成对电极;
(4)制备碳酸氢钠电解液
称取碳酸氢钠7 g ± 0.01 g,量取去离子水100 mL ± 0.01 mL,加入烧杯中,用搅拌器搅拌5 min,成0.833 mol/L的碳酸氢钠电解液;
(5)制备类石墨相氮化碳纳米片
类石墨相氮化碳纳米片的制备是在电解槽内进行的,是在电化学工作站脉冲电压电解作用下,在工作电极、对电极、参比电极作用下完成的;
① 将配置的碳酸氢钠电解液加入电解槽内;
② 将工作电极、对电极、参比电极垂直置于电解槽内,电解液要淹没工作电极、对电极、参比电极;
③ 开启电化学工作站,采用计时电流法来提供脉冲电压,高电位0.8 V相对于甘汞片电位、低电位-0.8 V相对于甘汞片电位,脉冲步数320,脉冲持续时间6 s,总时间1920 s;脉冲电压对工作电极、对电极内的类石墨相氮化碳细粉进行电解;
④ 电解后,将工作电极、对电极内的类石墨相氮化碳细粉进行收集,并置于烧杯中;
⑤ 洗涤,将烧杯中的类石墨相氮化碳细粉加入去离子水100 mL,搅拌清洗10 min,成洗涤液;
⑥ 离心分离,将洗涤液加入离心机的离心管内,进行离心分离,分离转速8000 r/min,分离时间10 min;
分离后,留存沉淀物,并去洗涤液;
⑦ 真空冷冻干燥,将沉淀物置于石英容器中,然后置于真空冷冻干燥箱中冷冻干燥,冷冻干燥温度-80℃,真空度2 Pa,冷冻干燥时间10 h,冷冻干燥后得类石墨相氮化碳纳米片;
(6)检测、分析、表征
对制备的类石墨相氮化碳纳米片的形貌、成份、化学物理性能进行检测、分析、表征;
用扫描电子显微镜对类石墨相氮化碳纳米片进行形貌和结构分析;
用原子力显微镜对类石墨相氮化碳纳米片厚度进行测量;
用X射线衍射仪对类石墨相氮化碳纳米片进行衍射强度分析;
用紫外-可见分光光度计对类石墨相氮化碳纳米片进行紫外可见光吸收分析;
结论:类石墨相氮化碳纳米片为淡黄色粉体片层状结构,层与层之间呈堆垛状,剥离后的类石墨相氮化碳纳米片厚度为1.67 nm,产物纯度达99.8%;
(7)产物储存
对制备的类石墨相氮化碳纳米片储存于棕色透明的玻璃瓶中,密闭避光保存,要防潮、防晒、防酸碱盐侵蚀,储存温度20℃,相对湿度10%。
2.根据权利要求1所述的一种气泡剥离法制备类石墨相氮化碳纳米片的方法,其特征在于:
制备类石墨相氮化碳纳米片是在电解槽内进行的,是在脉冲电源电解、在碳酸氢钠电解液内、在工作电极、参比电极、对电极作用下完成的;
电化学工作站(1)为立式,在电化学工作站(1)上部为脉冲电解槽(2),脉冲电解槽(2)上部为顶盖(3);顶盖(3)下部设有第一吊丝(8)、第二吊丝(9)、第三吊丝(10),并深入脉冲电解槽(2)内;第一吊丝(8)下部连接工作电极(12),第二吊丝(9)下部连接参比电极(13),第三吊丝(10)下部连接对电极(14);脉冲电解槽(2)内盛放碳酸氢钠电解液(11),碳酸氢钠电解液(11)要淹没工作电极(12)、参比电极(13)、对电极(14);在电化学工作站(1)上设有显示屏(4)、指示灯(5)、电源开关(6)、脉冲电源控制器(7)。
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