CN111111735A - 一种Bi@Ti3C2/g-C3N4复合材料及其制备方法 - Google Patents
一种Bi@Ti3C2/g-C3N4复合材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种Bi@Ti3C2/g‑C3N4复合材料及其制备方法,属于光催化制剂领域。本发明的制备方法具体为:(1)将g‑C3N4加入无水乙醇中,超声处理在室温下3小时;得到g‑C3N4的悬浮液;(2)将Bi@Ti3C2分散于去离子水中;并缓慢滴加到步骤(1)得到的g‑C3N4悬浮液中,搅拌,离心、干燥,即得到Bi@Ti3C2/g‑C3N4。本发明通过利用Bi纳米粒子对Ti3C2插层改性得到表面性能和层结构优化的双助催化剂,Ti3C2的层间限域效应得到粒径尺寸均一、分散较好的Bi纳米颗粒,同时又有效的抑制了Ti3C2的堆叠。
Description
技术领域
本发明涉及一种Bi@Ti3C2/g-C3N4复合材料及其制备方法,属于光催化制剂领域。
背景技术
MXenes是一类新型的二维(2D)早期过渡金属碳化物/碳氮化物材料,自2011年Gogotsi 及其同事发现以来,引起了人们极大的研究兴趣。由于其良好的导电性、亲水性和稳定性,氙在电化学超级电容器、电池、光催化等领域得到了广泛的研究。近年来,Ti3C2、Ti2C、Nb2C 等MXenes被研究作为光催化剂(如TiO2、Ag3PO4、CdS、g-C3N4)的高效共催化剂用于水分解。理论研究表明:MXenes的氢吸附的吉布斯自由能(ΔGH)几种接近于零,因此这些MXenes被视为有效电催化剂,并通过实验验证了这类催化剂的电催化析氢活性。其中,Ti3C2Mxene已被广泛研究,与半导体催化剂形成肖特基结,可以作为一种有效的光催化制氢助催化剂,形成Ti3C2和半导体界面,极大地促进光诱导电子和空穴的分离。研究表明Ti3C2可以显著促进光催化氢气的生产性能(λ≥420nm)。H2产生量和表观量子效率(AQE)cd/Ti3C2混合光催化剂可能达到14342μmol/(h·g)和40.1%,分别可以归因于导电性好和肖特基结的形成。
目前,采用HF制备的MXene容易形成层状堆垛结构,通过TEM观察可知每层堆垛又由若干单层MXene组成,相邻的MXene纳米片层间存在较强的范德华力,因此片层间的聚集和堆叠往往是不可避免的,这些都严重降低了MXene片层的电化学利用率。但是这样制得的MXene,由于干燥过程中的毛细效应和静电作用力,导致在堆垛的边缘处形成“塌缩”结构,从而减小了MXene的比表面积。
发明内容
为了解决上述至少一个问题,本发明选择Ti3C2作为助催化剂,并通过Bi纳米粒子插层形成一种双助催化剂(Bi@Ti3C2);通过2种助催化剂的之间的协同作用,提升了助催化能力。
本发明在层间引入Bi纳米粒子有效的抑制了堆叠的发生,Bi和MXene形成了双助催化剂体系,不但在层间得到尺寸均一且分散性较好的Bi纳米粒子,同时也有效的抑制了Mxene 的堆叠,形成的Bi@Ti3C2双助催化剂有利于加强电荷与物质的传输、拓宽光谱范围。本发明结合表面自组装技术,制备得到Bi@Ti3C2/g-C3N4新型肖特基结复合催化剂。将本发明的催化剂应用于光催化制氢反应,在两种助催化剂协同作用下显著提高了光催化产氢的性能。
本发明的第一个目的是提供一种Bi@Ti3C2的制备方法,具体包括以下步骤:
将PVP和BiCl3加入水中,搅拌均匀,然后加入NaBH4,反应完成之后,加入Ti3C2Tx纳米片,继续搅拌反应,反应结束之后将得到的产物进行离心、干燥即得到Bi@Ti3C2。
在一种实施方式中,所述的Ti3C2Tx纳米片的制备方法为:
将0.5g Ti3AlC2粉末倒入一个含有10mL HF的塑料容器中,在35℃下浸泡24小时,以腐蚀铝层,得到混合物;然后将所得的混合物经多次纯水洗涤,使得其pH值为6~7;之后通过超声处理和低速离心去除杂质得到Ti3C2Tx纳米片。
在一种实施方式中,所述的PVP和BiCl3的质量比为1:1。
在一种实施方式中,所述的PVP和水的质量比为1:100。
在一种实施方式中,所述的PVP购自阿拉丁,平均分子量1300000,K88-96。
在一种实施方式中,所述的BiCl3购自阿拉丁,纯度为AR。
在一种实施方式中,所述的PVP和NaBH4的质量比为3:2。
在一种实施方式中,所述的NaBH4购自阿拉丁,浓度为98%。
在一种实施方式中,所述的Bi@Ti3C2的制备方法具体为:将0.3g PVP和0.3g BiCl3加入30mL纯水中,搅拌10min,得到混合液;然后加入0.2g NaBH4到混合液中去氧化Bi3+;反应完成后,加入28mg Ti3C2Tx纳米片,连续搅拌6小时,得到产物;最后将得到的产物进行离心,在真空条件下于35℃下干燥48h,即得到Bi@Ti3C2。
本发明的第二个目的是本发明的制备方法制备得到的Bi@Ti3C2。
本发明的第三个目的是利用本发明的Bi@Ti3C2制备Bi@Ti3C2/g-C3N4复合材料的方法。
在一种实施方式中,具体的制备方法为:
(1)将g-C3N4加入无水乙醇中,超声处理在室温下3小时;得到g-C3N4的悬浮液;
(2)将Bi@Ti3C2分散于去离子水中;并缓慢滴加到步骤(1)得到的g-C3N4悬浮液中,搅拌,离心、干燥,即得到Bi@Ti3C2/g-C3N4。
在一种实施方式中,所述的g-C3N4和无水乙醇的质量体积比为:0.3:50,具体为0.3g: 50mL。
在一种实施方式中,所述的超声处理具体为:室温(25℃)下超声(500W)处理3h。
在一种实施方式中,所述的Bi@Ti3C2和水的质量比为0.08:40,具体为80mg Bi@Ti3C2分散于40mL去离子水中。
在一种实施方式中,所述的搅拌具体为:搅拌速度为500rpm,搅拌时间为1h。
在一种实施方式中,所述的离心具体为:离心时间为5min,速度为6000rpm。
在一种实施方式中,所述的干燥具体为:60℃干燥24h。
本发明的第四个目的是利用本发明的Bi@Ti3C2制备Bi@Ti3C2/g-C3N4复合材料的方法制得的Bi@Ti3C2/g-C3N4复合材料。
本发明的第五个目的是本发明的Bi@Ti3C2/g-C3N4复合材料制备得到的光催化剂。
本发明的第六个目的是本发明的光催化剂在光催化制氢中的应用。
本发明的有益效果:
(1)本发明通过利用Bi纳米粒子对Ti3C2插层改性得到表面性能和层结构优化的双助催化剂,Ti3C2的层间限域效应得到粒径尺寸均一、分散较好的Bi纳米颗粒,同时又有效的抑制了Ti3C2的堆叠。
(2)本发明利用双助催化剂Bi@Ti3C2 Mxene优化了g-C3N4的光催化性能。
附图说明
图1为Bi@Ti3C2/g-C3N4的制备过程示意图。
图2为实施例1的Bi@Ti3C2/g-C3N4的TEM图;(a-d)为TEM图像;(e-j)为元素映射图。
图3为实施例1的Bi@Ti3C2/g-C3N4和g-C3N4的UV-vis DRS光谱图。
图4为实施例1的Bi@Ti3C2/g-C3N4和g-C3N4的XPS图。
图5为实施例1的Bi@Ti3C2/g-C3N4和g-C3N4的PL图谱。
具体实施方式
以下对本发明的优选实施例进行说明,应当理解实施例是为了更好地解释本发明,不用于限制本发明。
XRD测试:Bruker D8 X射线粉末衍射仪,参数设置如下:2θ=10-80°(扫描速度8°/min), 40kV,40mA,Cu靶。
XPS测试:ESCALAB250Xi光电子能谱仪(Mg/Al靶)。
UV-vis DRS测试:Cary 500紫外可见光漫反射光谱(测试范围200-800nm)。
PL光谱:爱丁堡RF-5301光致发光光谱(激发波长360nm,室温)。
TEM测试:Tecnai G2 F30 S-TWIN(FEI,美国)场发射透射电镜,加速电压300kv 实施例1
一种Bi@Ti3C2/g-C3N4复合材料的制备方法,包括以下步骤:具体如图1所示:
1、Ti3C2Tx纳米片的制备
将0.5g Ti3AlC2粉末倒入一个含有10mL HF塑料容器中,在35℃下浸泡24小时,以腐蚀铝层,得到混合物;所得的混合物经多次纯水洗涤,使得其pH值为6~7;然后通过超声处理和低速离心去除杂质得到了Ti3C2Tx纳米片。
2、Bi@Ti3C2的制备
将0.3g PVP和0.3g BiCl3加入30mL纯水中,搅拌10min,得到混合液,然后加入0.2g NaBH4到混合液中去氧化Bi3+;反应完成后,加入步骤1中的Ti3C2Tx纳米片,连续搅拌6 小时,得到产物;最后将得到的产物进行离心,在真空条件下于35℃下干燥48小时,制得 Bi@Ti3C2。
3、Bi@Ti3C2/g-C3N4复合材料的制备
(1)将g-C3N4(0.3g)加入50mL无水乙醇溶液中,在室温下超声处理3小时,得到g-C3N4悬浮液;
(2)将80mg Bi@Ti3C2分散于40mL去离子水中,缓慢滴加到步骤(1)的g-C3N4悬浮液中,搅拌1h,6000rpm离心5min得到固体物质;
(3)将步骤(2)得到的固体在60℃下干燥24h,即得到Bi@Ti3C2/g-C3N4。
将实施例1得到的Bi@Ti3C2/g-C3N4复合材料和g-C3N4进行性能测试,测试结果如下:
图2为实施例1的Bi@Ti3C2/g-C3N4的TEM图;(a-d)为TEM图像;(e-j)为元素映射图。从图中可以看出:Bi纳米粒子、Ti3C2和g-C3N4很好的复合到了一起,且分散性良好。
图3为实施例1的Bi@Ti3C2/g-C3N4和g-C3N4的UV-vis DRS光谱图,从图中可以看出:双助催化剂Bi@Ti3C2的加入有效的改善了光响应性能,有利于吸收更多的可见光从而产生更多的光生载流子。
图4为实施例1的Bi@Ti3C2/g-C3N4和g-C3N4的XPS图。图4进一步证实了各种元素的存在,和TEM中Maping(图2e-2j)的检测结果相符合。
图5为实施例1的Bi@Ti3C2/g-C3N4和g-C3N4的PL图谱,从图中可以看出:复合之后的光催化剂显示了更低的发射强度,说明更快的迁移速度和光生载流子的再复合可以被很好的抑制。
虽然本发明已以较佳实施例公开如上,但其并非用以限定本发明,任何熟悉此技术的人,在不脱离本发明的精神和范围内,都可做各种的改动与修饰,因此本发明的保护范围应该以权利要求书所界定的为准。
Claims (10)
1.一种Bi@Ti3C2的制备方法,其特征在于,包括以下步骤:
将PVP和BiCl3加入水中,搅拌均匀,然后加入NaBH4,反应完成之后,加入Ti3C2Tx纳米片,继续搅拌反应,反应结束之后将得到的产物进行离心、干燥即得到Bi@Ti3C2。
2.根据权利要求1所述的制备方法,其特征在于,所述的PVP和BiCl3的质量比为1:1;所述的PVP和水的质量比为1:100;所述的PVP和NaBH4的质量比为3:2。
3.根据权利要求1或2所述的制备方法得到的Bi@Ti3C2。
4.采用权利要求3的Bi@Ti3C2制备Bi@Ti3C2/g-C3N4复合材料的方法,其特征在于,包括以下步骤:
(1)将g-C3N4加入无水乙醇中,超声处理在室温下3小时,得到g-C3N4的悬浮液;
(2)将Bi@Ti3C2分散于去离子水中;并缓慢滴加到步骤(1)得到的g-C3N4悬浮液中,搅拌,离心、干燥,即得到Bi@Ti3C2/g-C3N4。
5.根据权利要求4的制备方法,其特征在于,步骤(1)所述的g-C3N4和无水乙醇的质量体积比为0.3:50。
6.根据权利要求4的制备方法,其特征在于,步骤(2)所述的Bi@Ti3C2和水的质量比为0.08:40。
7.根据权利要求4的制备方法,其特征在于,具体的制备方法为:
(1)将0.3g的g-C3N4加入50mL无水乙醇溶液中,在室温下超声处理3小时,得到g-C3N4悬浮液;
(2)将80mg Bi@Ti3C2分散于40mL去离子水中,缓慢滴加到步骤(1)的g-C3N4悬浮液中,搅拌1h,6000rpm离心5min,得到固体物质;
(3)将步骤(2)得到的固体在60℃下干燥24h,即得到Bi@Ti3C2/g-C3N4。
8.权利要求4-7任一所述的制备方法得到的Bi@Ti3C2/g-C3N4复合材料。
9.权利要求8所述的Bi@Ti3C2/g-C3N4复合材料制备得到的光催化剂。
10.权利要求9所述的光催化剂在光催化制氢中的应用。
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CN114335458A (zh) * | 2021-12-15 | 2022-04-12 | 北京航空航天大学 | 一种Ti3C2Tx@g-C3N4复合材料及其制备方法和应用 |
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CN113617375B (zh) * | 2021-08-09 | 2023-06-30 | 东莞理工学院 | 一种石墨相氮化碳光催化材料及其制备方法 |
CN114335458A (zh) * | 2021-12-15 | 2022-04-12 | 北京航空航天大学 | 一种Ti3C2Tx@g-C3N4复合材料及其制备方法和应用 |
CN114335458B (zh) * | 2021-12-15 | 2024-04-09 | 北京航空航天大学 | 一种Ti3C2Tx@g-C3N4复合材料及其制备方法和应用 |
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