CN109292740A - 一种石墨相氮化碳基光电材料的低温制备方法及其用途 - Google Patents
一种石墨相氮化碳基光电材料的低温制备方法及其用途 Download PDFInfo
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000000463 material Substances 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000010439 graphite Substances 0.000 title claims abstract description 17
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000004202 carbamide Substances 0.000 claims abstract description 76
- 238000001354 calcination Methods 0.000 claims abstract description 38
- 230000005496 eutectics Effects 0.000 claims abstract description 29
- 239000002904 solvent Substances 0.000 claims abstract description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000002585 base Substances 0.000 claims description 48
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 45
- 235000019743 Choline chloride Nutrition 0.000 claims description 45
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical group [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 45
- 229960003178 choline chloride Drugs 0.000 claims description 45
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000011592 zinc chloride Substances 0.000 claims description 19
- 235000005074 zinc chloride Nutrition 0.000 claims description 19
- 239000011521 glass Substances 0.000 claims description 15
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 235000019437 butane-1,3-diol Nutrition 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 229940058015 1,3-butylene glycol Drugs 0.000 claims description 5
- 238000005660 chlorination reaction Methods 0.000 claims description 4
- VXJIMUZIBHBWBV-UHFFFAOYSA-M lithium;chloride;hydrate Chemical compound [Li+].O.[Cl-] VXJIMUZIBHBWBV-UHFFFAOYSA-M 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical class Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229940097267 cobaltous chloride Drugs 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 27
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
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- AXPZIVKEZRHGAS-UHFFFAOYSA-N 3-benzyl-5-[(2-nitrophenoxy)methyl]oxolan-2-one Chemical compound [O-][N+](=O)C1=CC=CC=C1OCC1OC(=O)C(CC=2C=CC=CC=2)C1 AXPZIVKEZRHGAS-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
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- 229910021607 Silver chloride Inorganic materials 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
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- 229910052697 platinum Inorganic materials 0.000 description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000008055 phosphate buffer solution Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
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- FZRNJOXQNWVMIH-UHFFFAOYSA-N lithium;hydrate Chemical compound [Li].O FZRNJOXQNWVMIH-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- 240000008067 Cucumis sativus Species 0.000 description 1
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- -1 dicyanodiamine Chemical compound 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 238000001548 drop coating Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
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- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
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- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
- C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
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Abstract
本发明属于光电材料领域,公开了一种石墨相氮化碳基光电材料的低温制备方法及其用途,制备步骤如下:将尿素和氯化物按摩尔比在一定温度下恒温反应,得到尿素/氯化物低共熔溶剂;将尿素/氯化物低共熔溶剂置于马弗炉中进行煅烧,煅烧完成后,得到粗石墨相氮化碳基光电材料;将粗石墨相氮化碳基光电材料超声分散于清洗液中,进行搅拌或超声,离心分离得到石墨相氮化碳基光电材料。本发明采用了一种较新的合成方法,扩宽了CN基材料的合成方法。本发明所使用的合成方法是低共熔溶剂煅烧法,相比于较高温煅烧法,具有安全,节能等优点。
Description
技术领域
本发明属于光电材料领域,具体涉及一种石墨相氮化碳基光电材料的低温制备方法及其用途。
背景技术
光电效应是指在高于某特定频率的光照射下,某些物质内部的电子会被光子激发出来而形成电流,即光生电。近年来,具有光学和电学性质的光催化剂,在光催化降解污染物,太阳能电池及光电检测方面有较为广泛的应用。而光催化剂的作用原理是光催化剂被光激发产生光生电子-空穴对,即被光激发产生的电子的数量决定了光催化剂的性能,因此研究光催化剂的光电性能有一定的实际意义。
石墨相氮化碳(CN)是禁带宽度为2.7eV半导体材料,它不仅在可见光区具有光催化能力,同时具有廉价、低毒、易于合成等特点,成为研究人员关注的热点。研究人员常用的CN合成方法是高温煅烧法,将尿素、二氰二胺、三聚氰胺等高温聚合即可生成CN。研究表明,常用的煅烧法制备CN的煅烧温度在500℃以上。较高的温度一方面使得煅烧过程的危险性上升,另一方面较高的温度也意味着维持煅烧反应所需的能耗较大。故此开发一种能够低温下合成CN的方法不仅能够降低CN合成的能耗,也能提高煅烧过程的安全性。
近年来研究发现尿素能够与氯化胆碱或氯化锌等形成一种液态溶剂,由于其熔点显著低于各个组分纯物质的熔点而被称为低共熔溶剂(Smith.EL,Abbott.AP,Ryder.KS,Chem.Rev.2014,114,11060-11082)。低共熔溶剂是由一定化学计量比的氢键受体(如季铵盐、金属盐等)和氢键给体(如尿素、有机酸等)组合而成的两组分或三组分低共熔混合物。低共熔溶剂熔点低于尿素的熔点,那么理论上也可以降低尿素到达能够聚合生成CN这一状态所需的温度,即实现CN的低温煅烧合成。
发明内容
本发明提供一种采用低共熔溶剂低温煅烧法合成CN光电材料的制备方法,并研究其光电性能。该方法降低了尿素到达能够聚合生成CN这一状态所需的温度,实现了CN的低温煅烧合成。
本发明采用的技术方案为:
本发明提供一种采用低共熔溶剂低温煅烧法合成CN光电材料的制备方法,按照下述步骤进行:
CN基光电材料的制备是通过低共熔溶剂煅烧法制得:首先,将尿素和氯化物按摩尔比在一定温度下恒温反应,得到尿素/氯化物低共熔溶剂;将尿素/氯化物低共熔溶剂置于马弗炉中进行煅烧,升温速率2.9K/min,煅烧完成后,得到粗CN基光电材料;
CN基光电材料的纯化是通过溶液进行清洗实现的:将粗CN基光电材料超声分散于清洗液中,进行搅拌或超声,离心分离得到CN基光电材料。
所述的氯化物和尿素的用量比为0.1mol:0.1~0.5mol。
所述恒温反应的条件为:油浴中80~140℃反应5min~3h;所述的称取的低共熔溶剂的量为1.5~2.5g,所述的马弗炉中煅烧温度为250~450℃,煅烧时间为2~14h。
所述的氯化物为氯化胆碱、无水氯化锌、无水氯化铁、无水氯化钴、无水氯化镍、无水氯化铜、无水氯化铝、一水合氯化锂、五水氯化铁、六水合氯化镍、六水氯化钴、二水氯化铜中的一种。
所述的清洗液为去离子水、甲醇、乙醇、1,3-丁二醇、硝酸、盐酸中的一种。
所述的搅拌时间为4~72h,超声时间为3~60min。
所制备的CN基光电材料用于制备修饰电极,即光电电极,研究其光电性能。
所述的CN基光电材料光电性能的研究,所述的修饰电极的制备方法为:
将CN基光电材料分散到去离子水中,超声分散,得到稳定的悬浊液;然后,取悬浊液滴涂于预处理的ITO导电玻璃上,室温自然干燥后待用;所制得的修饰电极记作CN-ITO。所制备的悬浊液浓度为1.0mg/mL;所述滴涂于预处理的ITO导电玻璃上的悬浊液为50μL。
利用电化学工作站来探讨上述制备方法制备得到的CN-ITO材料的光电性能。
探讨光电化学性能的具体方法为:将磷酸缓冲液移入样品池中,将修饰电极作为工作电极,铂丝电极作为对电极,饱和Ag/AgCl电极作为参比电极装入样品池中;通过高亮度氙灯平行光源系统仪器对工作电极进行光照,在工作电极上产生电流信号;电流信号通过电化学工作站传送到计算机转化为数字信号,表现为光电流响应。其中,所述的磷酸缓冲溶液是通过配置0.1mol/L的磷酸二氢钠和磷酸氢二钠互调,使pH值为7.0制得。其浓度为0.1mol/L。
本发明具有以下优势:
(1)本发明得到的低共熔溶剂通过较低温度下煅烧得到了一种具有光电响应的材料,并通过红外表征证明合成的材料为CN基光电材料。
(2)本发明采用了一种较新的合成方法,扩宽了CN基材料的合成方法。
(3)本发明所使用的合成方法是低共熔溶剂煅烧法,相比于较高温煅烧法,具有安全,节能等优点。
附图说明
图1为CN基材料的傅里叶红外(FT-IR)图;
图2为修饰电极CN基材料的光电流图;
图3为CN基材料的交流阻抗(EIS)图;
图4为修饰电极CN基材料纯化前后的光电流图;
图5为CN基材料的制备示意图。
具体实施方式
下面结合具体实施实例对本发明做进一步说明,以使本领域技术人员更好地理解本发明,但本发明的保护范围并不局限于以下实施例。
实施例1:
(1)CN基光电材料的制备是通过低共熔溶剂煅烧法制得:首先,按摩尔比称取一定量的尿素及氯化胆碱于100mL圆底烧瓶中,80℃油浴3h得到无色澄清透明溶液,该溶液即为尿素/氯化胆碱低共熔溶剂。再称取2g的尿素/氯化胆碱低共熔溶剂于10mL坩埚中,置于马弗炉中,300℃保持6h,升温速率2.9K/min,产物即为CN基光电材料;
(2)CN基光电材料的纯化是通过1,3-丁二醇进行清洗实现的:将CN基光电材料超声分散于1,3-丁二醇中,超声5min,12000r离心分离取上层液,于烘箱中140℃烘干,得到纯化的CN基光电材料;
(3)修饰电极的制备:首先是ITO导电玻璃预处理过程,将ITO导电玻璃分别在去离子水、乙醇中依次超声清洗半小时后,用去离子水多次冲洗。然后将导电玻璃放入0.1mol/LNaOH水溶液中,将其煮沸,并保持30分钟,用去离子水清洗并吹干待用。配置1mg/mL CN基材料的水溶液,将其进行超声分散,得到稳定的悬浊液。然后,取50μL悬浊液滴涂于预处理的ITO导电玻璃上,室温自然吹干后待用。所制得的修饰电极记作CN-ITO。为了与上述制备方法制备得到的CN-ITO比较,按类似方法制得尿素煅烧产物urea-ITO修饰电极,氯化胆碱煅烧产物ChCl-ITO,纯化的CN基光电材料CN-ITO。
(4)光电化学检测方法和条件:
光源取自高亮度氙灯平行光源系统仪器,购买于北京泊菲莱科技有限公司,型号为:PLS-SXE300,参数为:光源强度150W。用400nm滤光片滤掉氙灯的紫外光。电化学实验使用电化学工作站,买于上海辰华仪器有限公司,型号为:CHI660E,测试参数为:电压0V。利用传统的三电极体系:修饰电极为工作电极,铂丝电极为对电极,饱和Ag/AgCl电极为参比电极(所有电位均相对于SCE)。电化学实验均在室温、磷酸缓冲溶液(0.1mol/L,pH=7.0)中进行,电位为0V(vs SCE)。EIS实验在含有5mmol/L Fe(CN)6 3-/4-的0.1mol/L KCl溶液中进行,频率范围为0.01Hz~10kHz,初始电位为0.24V,交流振幅为5mV。
实施例2:
(1)CN基光电材料的制备是通过低共熔溶剂煅烧法制得:首先,按摩尔比称取一定量的尿素及氯化锌于100mL圆底烧瓶中,140℃油浴5min得到无色澄清透明溶液,该溶液即为尿素/氯化锌低共熔溶剂。再称取2g的尿素/氯化锌低共熔溶剂于10mL坩埚中,置于马弗炉中,300℃保持4h,升温速率2.9K/min,产物即为CN基光电材料;
(2)CN基光电材料的纯化是通过盐酸进行清洗实现的:取20mL浓盐酸与60mL去离子水混合配得盐酸,将CN基光电材料超声分散于配备的盐酸中,搅拌24h,12000r离心分离取下层固体,于烘箱中60℃烘干,得到纯化的CN基光电材料;
(3)修饰电极的制备:首先是ITO导电玻璃预处理过程,将ITO导电玻璃分别在去离子水、乙醇中依次超声清洗半小时后,用去离子水多次冲洗。然后将导电玻璃放入0.1mol/LNaOH水溶液中,将其煮沸,并保持30分钟,用去离子水清洗并吹干待用。配置1mg/mL CN基材料的水溶液,将其进行超声分散,得到稳定的悬浊液。然后,取50μL悬浊液滴涂于预处理的ITO导电玻璃上,室温自然吹干后待用。所制得的修饰电极记作CN-ITO。为了与上述制备方法制备得到的CN-ITO比较,按类似方法制得尿素煅烧产物urea-ITO修饰电极,氯化锌煅烧产物ZnCl2-ITO,纯化的CN基光电材料CN-ITO。
(4)光电化学检测方法和条件:
光源取自高亮度氙灯平行光源系统仪器,并以500W氙灯(CHF-XM35-500W,北京畅拓科技有限公司)作为可见光源。用400nm滤光片滤掉氙灯的紫外光。电化学实验使用CHI660 B电化学工作站(上海辰华仪器有限公司),利用传统的三电极体系:修饰电极为工作电极,铂丝电极为对电极,饱和Ag/AgCl电极为参比电极(所有电位均相对于SCE)。电化学实验均在室温、磷酸缓冲溶液(0.1mol/L,pH=7.0)中进行,电位为0V(vs SCE)。EIS实验在含有5mmol/L Fe(CN)6 3-/4-的0.1mol/L KCl溶液中进行,频率范围为0.01Hz~10kHz,初始电位为0.24V,交流振幅为5mV。
实施例3:
(1)CN基光电材料的制备是通过低共熔溶剂煅烧法制得:首先,按摩尔比称取一定量的尿素及一水合氯化锂于100mL圆底烧瓶中,140℃油浴10min得到无色澄清透明溶液,该溶液即为尿素/一水合氯化锂低共熔溶剂。再称取2g的尿素/一水合氯化锂低共熔溶剂于10mL坩埚中,置于马弗炉中,350℃保持6h,升温速率2.9K/min,产物即为CN基光电材料;
(2)CN基光电材料的纯化是通过盐酸进行清洗实现的:取20mL浓盐酸与60mL去离子水混合配得盐酸,将CN基光电材料超声分散于配备的盐酸中,搅拌24h,12000r离心分离取下层固体,于烘箱中60℃烘干,得到纯化的CN基光电材料;
(3)修饰电极的制备:首先是ITO导电玻璃预处理过程,将ITO导电玻璃分别在去离子水、乙醇中依次超声清洗半小时后,用去离子水多次冲洗。然后将导电玻璃放入0.1mol/LNaOH水溶液中,将其煮沸,并保持30分钟,用去离子水清洗并吹干待用。配置1mg/mL CN基材料的水溶液,将其进行超声分散,得到稳定的悬浊液。然后,取50μL悬浊液滴涂于预处理的ITO导电玻璃上,室温自然吹干后待用。所制得的修饰电极记作CN-ITO。为了与上述制备方法制备得到的CN-ITO比较,按类似方法制得尿素煅烧产物urea-ITO修饰电极,一水合氯化锂煅烧产物LiCl*H2O-ITO,纯化的CN基光电材料CN-ITO。
(4)光电化学检测方法和条件:
光源取自高亮度氙灯平行光源系统仪器,并以500W氙灯(CHF-XM35-500W,北京畅拓科技有限公司)作为可见光源。用400nm滤光片滤掉氙灯的紫外光。电化学实验使用CHI660 B电化学工作站(上海辰华仪器有限公司),利用传统的三电极体系:修饰电极为工作电极,铂丝电极为对电极,饱和Ag/AgCl电极为参比电极(所有电位均相对于SCE)。电化学实验均在室温、磷酸缓冲溶液(0.1mol/L,pH=7.0)中进行,电位为0V(vs SCE)。EIS实验在含有5mmol/L Fe(CN)6 3-/4-的0.1mol/L KCl溶液中进行,频率范围为0.01Hz~10kHz,初始电位为0.24V,交流振幅为5mV。
实施例1~3中的1,3-丁二醇或盐酸均可以用去离子水、甲醇、乙醇、硝酸中的任意一种代替,实施例1~3中的氯化胆碱、无水氯化锌、一水合氯化锂均可用无水氯化铁、无水氯化钴、无水氯化镍、无水氯化铜、无水氯化铝、五水氯化铁、六水合氯化镍、六水氯化钴、二水氯化铜中的任意一种代替。
图1为CN基光电材料的傅里叶红外(FT-IR)图,图A中a为尿素煅烧产物,b为氯化胆碱煅烧产物,图B为尿素/氯化胆碱煅烧产物的傅里叶红外(FT-IR)图。从图中可以发现,对比于尿素煅烧产物及氯化胆碱煅烧产物,尿素/氯化胆碱煅烧产物有着不同于两种单体的红外峰,证明尿素与氯化胆碱油浴后煅烧并非仅仅是尿素与氯化胆碱的一种简单复合,而是两者之间存在一种较强的相互作用—氢键,这一点从尿素与氯化胆碱形成低共熔溶剂可以看出,尿素与氯化胆碱之间氢键的存在使得尿素/氯化胆碱的熔点低于尿素与氯化胆碱,同时氢键的存在也使得尿素/氯化胆碱的煅烧产物不同于尿素与氯化胆碱的煅烧产物,这从尿素/氯化胆碱煅烧产物有着不同于尿素与氯化胆碱的红外峰可以看出。为了研究尿素/氯化胆碱煅烧产物的组成,对尿素/氯化胆碱煅烧产物的红外图进行研究,从图B中发现,尿素/氯化胆碱煅烧产物在1200~1700cm-1区间存在一系列吸收峰,对应于CN杂环的红外吸收峰,800cm-1附近的吸收对应于三嗪环的振动峰,证明尿素/氯化胆碱的煅烧产物为CN基材料。
图2为修饰电极CN基光电材料的光电流图(a为尿素煅烧产物,b为氯化胆碱煅烧产物,c为尿素/氯化胆碱煅烧产物)。从图2中可以看出,尿素与氯化胆碱煅烧产物有着较低的光电流响应值,表明纯的尿素与氯化胆碱在低温煅烧时并不能生成具有较好光电响应的材料,而尿素/氯化胆碱煅烧产物有着200nA以上的光电响应,是纯的尿素及氯化胆碱煅烧产物光电响应的4倍,表明采用低共熔溶剂煅烧法可以合成具有较好光电响应的CN光电材料。
图3为CN基材料的交流阻抗(EIS)图,其中a为尿素煅烧产物,b为氯化胆碱煅烧产物,c为尿素/氯化胆碱煅烧产物。交流阻抗被用来研究材料转移电子的能力,从图3中可以看出,尿素/氯化胆碱煅烧产物有着最小的电化学交流阻抗值,表明尿素/氯化胆碱煅烧产物有着最快的电子转移的能力,这是由于尿素/氯化胆碱之间的氢键作用使得尿素/氯化胆碱煅烧生成了CN基材料,而纯的尿素及氯化胆碱在煅烧过程中聚合不完全,并不能生成较稳定,电子转移较快的材料,即尿素与氯化胆碱之间存在的氢键大大降低了CN材料的煅烧生成温度,使得CN材料能够在300℃的条件下生成。
图4为修饰电极CN基材料纯化前后的光电流图(a为尿素/氯化胆碱煅烧产物纯化前,b为尿素/氯化胆碱煅烧产物纯化后)。从图中可以发现纯化前的CN基光电材料的光电流响应只有200nA左右,而经过纯化的CN基光电材料的光电流响应为400nA以上,说明使用1,3-丁二醇对尿素/氯化胆碱煅烧产物进行纯化能够得到光电响应性能更佳的光电材料。而使用1,3-丁二醇能够对尿素/氯化胆碱煅烧产物进行纯化的原理是利用尿素/氯化胆碱煅烧产物密度的不均一性。将尿素/氯化胆碱煅烧产物分散于1,3-丁二醇溶液中,超声5min,再进行离心分离,结果是尿素/氯化胆碱煅烧产物中密度大的被离心力带至下层沉淀,密度小的依然保留在1,3-丁二醇溶液中,再将1,3-丁二醇溶液置于140℃烘箱中将1,3-丁二醇溶液烘干,得到纯化的CN材料。而对于光电材料来说,密度小一般代表着大的比表面积,大的比表面积对应着多的活性位点,进而对应于更佳的光电性能。
图5为CN基光电材料的制备示意图(A为尿素/氯化锌低共熔溶剂,B为尿素/氯化锌煅烧产物,C为尿素/氯化锌煅烧产物盐酸酸洗纯化后)。从图5(A)中可以发现尿素/氯化锌低共熔溶剂在室温下是一种无色透明澄清液体,这是由于尿素与氯化锌之间存在的较强的氢键的相互作用导致的,使得尿素/氯化锌的熔点低于尿素与氯化锌的熔点。图5(B)为尿素/氯化锌煅烧产物,尿素/氯化锌煅烧产物为黄色固体,这是由于在煅烧过程中,氯化锌生成了微黄色的氧化锌,而氧化锌也是纯化过程希望去除的物质。图5(C)为尿素/氯化锌煅烧产物盐酸酸洗纯化后,可以发现,经过24h的盐酸酸洗后,产物为白色固体粉末,微黄色的氧化锌被盐酸溶解,使得CN基光电材料得到纯化。
Claims (9)
1.一种石墨相氮化碳基光电材料的低温制备方法,其特征在于,步骤如下:
将尿素和氯化物按摩尔比在一定温度下恒温反应,得到尿素/氯化物低共熔溶剂;
将尿素/氯化物低共熔溶剂置于马弗炉中进行煅烧,煅烧完成后,得到粗石墨相氮化碳基光电材料;
将粗石墨相氮化碳基光电材料超声分散于清洗液中,进行搅拌或超声,离心分离得到石墨相氮化碳基光电材料。
2.根据权利要求1所述的一种石墨相氮化碳基光电材料的低温制备方法,其特征在于,所述的氯化物和尿素的用量比为0.1mol:0.1~0.5mol。
3.根据权利要求1所述的一种石墨相氮化碳基光电材料的低温制备方法,其特征在于,所述的氯化物为氯化胆碱、无水氯化锌、无水氯化铁、无水氯化钴、无水氯化镍、无水氯化铜、无水氯化铝、一水合氯化锂、五水氯化铁、六水合氯化镍、六水氯化钴、二水氯化铜中的一种。
4.根据权利要求1所述的一种石墨相氮化碳基光电材料的低温制备方法,其特征在于,所述恒温反应的条件为:油浴中80~140℃反应5min~3h;所述的马弗炉中煅烧温度为250~450℃,煅烧时间为2~14h。
5.根据权利要求1所述的一种石墨相氮化碳基光电材料的低温制备方法,其特征在于,所述的清洗液为去离子水、甲醇、乙醇、1,3-丁二醇、硝酸、盐酸中的一种。
6.根据权利要求1所述的一种石墨相氮化碳基光电材料的低温制备方法,其特征在于,所述的搅拌时间为4~72h,超声时间为3~60min。
7.根据权利要求1~6任意一项所述的制备方法制备的石墨相氮化碳基光电材料。
8.将权利要求7所述的石墨相氮化碳基光电材料用于制备光电电极的用途。
9.根据权利要求8所述的石墨相氮化碳基光电材料用于制备光电电极的用途,其特征在于,步骤如下:将石墨相氮化碳基光电材料分散到去离子水中,超声分散,得到稳定的悬浊液;取悬浊液滴涂于氧化铟锡导电玻璃上,室温自然干燥后,得到所述的光电电极。
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