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CN109626422A - A kind of TiO2/g-C3N4The preparation method and applications of light anode nanocomposite - Google Patents

A kind of TiO2/g-C3N4The preparation method and applications of light anode nanocomposite Download PDF

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CN109626422A
CN109626422A CN201811510058.5A CN201811510058A CN109626422A CN 109626422 A CN109626422 A CN 109626422A CN 201811510058 A CN201811510058 A CN 201811510058A CN 109626422 A CN109626422 A CN 109626422A
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tio
photoanode
nanocomposite
nanocomposite material
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范晓星
王晓娜
蔡鹤
成祥祥
刘京
韩宇
王绩伟
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Liaoning University
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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Abstract

The present invention relates to optical electro-chemistry fields, disclose a kind of TiO2/g‑C3N4Light anode nanocomposite stirs the preparation method comprises the following steps: melamine and butyl titanate are mixed in ethyl alcohol, mixed material is made to be uniformly dispersed, and using hydro-thermal method, after drying, powder the high temperature anneal is cooled to room temperature for centrifugal filtration, and grinding obtains TiO2/g‑C3N4Light anode nanocomposite.The light anode nanocomposite is also disclosed in preparation TiO2/g‑C3N4Application in photoelectricity very thin films.The TiO2/g‑C3N4The advantages that light anode nanocomposite and photoelectricity very thin films all have good photochemical properties, and preparation method has low energy consumption, and condition is simple, easy scale.

Description

A kind of TiO2/g-C3N4The preparation method and applications of light anode nanocomposite
Technical field
The invention belongs to PhotoelectrochemicalTechnique Technique fields, and in particular to a kind of TiO2/g-C3N4Light anode nanocomposite Preparation method and applications.
Background technique
Optical electro-chemistry (PEC) water dissociation technology is current very active research field, utilizes sun photodegradation water system Hydrogen obtains renewable energy, is the current main means for solving environment and energy problem.The exploitation of optical anode material is photoelectrochemical The most important thing of credit solution water large-scale application.With effective carrier transport, suitable band gap, conduction band valence-band level, steady The semiconductor material of the conditions such as qualitative good and at low cost is considered to be ideal light anode semiconductor material.In order to obtain in satisfaction The optoelectronic pole material for stating condition improves the performance of existing semiconductor material, while developing the new light anode with application prospect New material is imperative.
TiO2Forbidden bandwidth is wider (3.0~3.2eV), only absorbs visible light.g-C3N4Photo-generate electron-hole recombination rate is high, Quantum efficiency is low, and conductive capability is poor.Studies have shown that TiO can be improved by the compound of two kinds of semiconductor materials2Photoelectricity Chemical property.Currently, there is research using composite Ti O2/g-C3N4The method of semiconductor material, but operating process is relative complex, no Easily carry out large scale preparation.Therefore, it is necessary to study its production method and performance.
Summary of the invention
It is an object of the present invention to provide a kind of TiO2/g-C3N4The preparation method and applications of light anode nanocomposite, this Invention preparation method is simple and convenient to operate, mild condition, is conducive to large scale preparation.
Another object of the present invention is to provide a kind of TiO2/g-C3N4Light anode nanocomposite is in preparation TiO2/g-C3N4 Application in photoelectricity very thin films.
The technical solution adopted by the present invention are as follows:
A kind of TiO2/g-C3N4Light anode nanocomposite, the preparation method comprises the following steps: melamine and butyl titanate are mixed Together in ethyl alcohol, stirring makes mixed material be uniformly dispersed, using hydro-thermal method, centrifugal filtration, after drying, by powder high annealing Processing, is cooled to room temperature, and grinds, obtains TiO2/g-C3N4Light anode nanocomposite.
A kind of TiO2/g-C3N4Light anode nanocomposite, mole of the melamine and butyl titanate Than for 3:1.
A kind of TiO2/g-C3N4Light anode nanocomposite, the condition of the hydro-thermal method are as follows: hydrothermal temperature is 180 DEG C -200 DEG C, time 18h-24h.
A kind of TiO2/g-C3N4Light anode nanocomposite, the high temperature anneal condition are as follows: temperature 500-550 DEG C, time 3-5h.
A kind of TiO2/g-C3N4Light anode nanocomposite, the product TiO2/g-C3N4Light anode nanometer is multiple Condensation material is N-type semiconductor material.
A kind of TiO2/g-C3N4Light anode nanocomposite, melamine, butyl titanate and ethyl alcohol are consolidated Liquid mixture is as precursor solution.
A kind of TiO2/g-C3N4Light anode nanocomposite is in preparation TiO2/g-C3N4Answering in photoelectricity very thin films With specifically comprising the following steps:
1) containing I2Aqueous acetone solution in disperse TiO as described in any one in claim 1-52/g-C3N4Light anode is received Nano composite material, and make TiO using ultrasonic oscillation2/g-C3N4Light anode nanocomposite is suspended in containing I2Acetone it is water-soluble In liquid, that is, obtain electrophoretic deposition suspension；
2) it is put into the transparent conducting glass FTO of two panels homalographic in electrophoretic deposition suspension, and enables two panels electro-conductive glass Conducting surface is opposite, and is parallel to each other and immerses in electrophoretic deposition suspension, deposits 1-5min under the conditions of DC voltage；
3) electric current is cut off, two panels electro-conductive glass is taken out from electrophoretic deposition suspension, after drying at room temperature, in Muffle In furnace, high-temperature roasting obtains TiO2/g-C3N4Photoelectricity very thin films.
The application contains I described in step 1)2Aqueous acetone solution in, by volume, acetone: water=25:1；Often Contain the I of 0.4mg in 1ml aqueous acetone solution2。
The application, DC voltage is 20V-25V in step 2).
The application, maturing temperature is 400-500 DEG C in Muffle furnace in step 3), roasts 90min.
The invention has the following advantages:
A kind of TiO of the present invention2/g-C3N4Light anode nanocomposite, the TiO2/g-C3N4Nanocomposite is The composite material of nano-titanium dioxide and graphite phase carbon nitride, preparation process are two-step method, and first step Direct Hydrothermal presoma is molten Liquid obtains the titanium dioxide nano-rod of attachment melamine.Second step the high temperature anneal makes be attached to titanium dioxide surface three Poly cyanamid is converted into graphite phase carbon nitride.The TiO being prepared2/g-C3N4Nanocomposite, by nano titania material The high conductivity of material and the big light absorption range of graphite phase carbon nitride, have good photochemical properties, which has low The advantages that energy consumption, condition is simple, easy scale.
TiO2/g-C3N4Nanocomposite be a kind of non-metal N type semiconductor, there is good optical characteristics, can be with Absorb the visible light for being less than wavelength 450nm, the efficiency of transmission and conductive substrates for improving carrier to the collection efficiency of electronics, Obtain the TiO of high PEC performance2/g-C3N4Light anode.And preparation method provided by the present invention, raw material is cheap, operation letter Single, high degree reduces costs, and no pollution to the environment, realizes Green Chemistry.
Detailed description of the invention
Fig. 1 is the TiO that hydrothermal calcine obtains in embodiment 12/g-C3N4The XRD diagram of powder.
Fig. 2 is the TiO that electrophoretic deposition obtains in embodiment 32/g-C3N4The SEM of film schemes.
Fig. 3 is the TiO obtained under different sedimentation times in embodiment 2-42/g-C3N4The SEM sectional view of film.
Fig. 4 is the TiO obtained under different sedimentation times in embodiment 2-42/g-C3N4The comparison diagram of the photoelectric current of film.
Fig. 5 is the TiO obtained under different sedimentation times in embodiment 2-42/g-C3N4The comparison diagram of the impedance spectrum of film.
Fig. 6 is TiO in embodiment 32/g-C3N4The quantum efficiency figure of film.
Specific embodiment
Embodiment 1:TiO2/g-C3N4Light anode nanocomposite
Preparation method:
0.45g melamine and 2ml butyl titanate are mixed in 40ml ethyl alcohol, stirred, keeps mixed material dispersion equal It is even, it is put into 100ml water heating kettle, hydrothermal temperature is 180 DEG C, and the time is for 24 hours that after the completion of hydro-thermal, powder is put by centrifugal filtration 550 DEG C of annealing 4h, are cooled to room temperature in Muffle furnace, and grinding obtains TiO2/g-C3N4Light anode nanocomposite.
The TiO that will be obtained2/g-C3N4Powder carries out XRD test, as a result as shown in Figure 1, as seen from Figure 1, TiO2/g-C3N4 With good crystallinity.
Embodiment 2:TiO2/g-C3N4Photoelectricity very thin films (TiO2/g-C3N4-1min)
Preparation method:
1) 10mg I is taken2It is placed in 25ml aqueous acetone solution (volume ratio of water and acetone is 1:25), seals ultrasound 30min It is uniformly dispersed to solution, I must be contained2Aqueous acetone solution.
2) TiO for taking 0.6g embodiment 1 to prepare2/g-C3N4Powder is scattered in containing I2Aqueous acetone solution in, sealing is super Sound 120min obtains electrophoretic deposition suspension.
3) two panels electro-conductive glass conducting surface is staggered relatively and be parallel to each other and immerse in electrophoretic deposition suspension, and in two electricity Interpolar applies the DC voltage of 25V, deposits 1min.
4) electric current is cut off, electro-conductive glass (FTO) is taken out from suspension, is dried at room temperature, and in Muffle furnace In, in 450 DEG C of roasting 90min, obtain TiO2/g-C3N4Photoelectricity very thin films are labeled as TiO2/g-C3N4-1min。
Embodiment 3:TiO2/g-C3N4Photoelectricity very thin films (TiO2/g-C3N4-3min)
For preparation method with embodiment 2, the sedimentation time only changed the step 3) is 3min, obtains TiO2/g-C3N4Photoelectricity is very thin Film is labeled as TiO2/g-C3N4-3min。
By TiO2/g-C3N4- 3min sample carries out SEM test, as a result as shown in Fig. 2, it can be observed that TiO in figure2With g-C3N4Pattern.
Embodiment 4:TiO2/g-C3N4Photoelectricity very thin films (TiO2/g-C3N4-5min)
For preparation method with embodiment 2, the sedimentation time only changed the step 3) is 5min, obtains TiO2/g-C3N4Photoelectricity is very thin Film is labeled as TiO2/g-C3N4-5min。
By TiO obtained above2/g-C3N4-1min、TiO2/g-C3N4- 3min and TiO2/g-C3N4Three samples of -5min The test of SEM sectional view is carried out, as a result as shown in figure 3, as seen from Figure 3, with the increase of sedimentation time, film thickness increases.
TiO2/g-C3N4The application of photoelectricity very thin films
The TiO respectively prepared by embodiment 2-42/g-C3N4-1min、TiO2/g-C3N4- 3min and TiO2/g-C3N4-5min Photoelectricity very thin films carry out the photoelectrochemical behaviour test of photoelectric current, impedance and quantum efficiency etc..
All electrochemistry experiment test process are all in the electrochemical workstation of three-electrode system (Princeton Applied Research 2273) in carry out.Sample thin film is to electrode as working electrode, platinized platinum, and Ag/AgCl is reference electrode, electrolysis Liquid is 0.5M sodium sulphate, and sample photoirradiated surface product is 1cm2。
Photoelectricity current test: light source is 300W xenon lamp, and bias is 1.18V vs.VRHE, result is measured as shown in figure 4, result is aobvious Show, sedimentation time is the sample of 3min, and photoelectric current is relatively large；
Electrochemical impedance spectroscopy (EIS) test: fixed voltage is 0V vs.Voc, frequency range is 0.1~105Hz.It measures As a result as shown in figure 5, sedimentation time is the sample of 3min, impedance is relatively small；
Quantum efficiency (IPCE) test: choose multiple wavelength (365nm, 380nm, 390nm, 410nm, 420nm, 430nm, 450nm, 460nm, 490nm, 520nm) monochromatic light exposure embodiment 3 prepare sample TiO2/g-C3N4- 3min, measure its Bias is 1.18V vs.VRHEWhen photoelectric current.Utilize formula:
Wherein, I is density of photocurrent (unit: mA), and λ is incident monochromatic wavelength (nm), P be incident intensity (unit: mW).By the way that the value of quantum efficiency is calculated, as a result as shown in fig. 6, the quantum in the case where wavelength is 365nm monochromatic light exposure is imitated Rate highest.

Claims (9)

1.一种TiO2/g-C3N4光阳极纳米复合材料，其特征在于，制备方法为：将三聚氰胺和钛酸四丁酯混合于乙醇中，搅拌，使混合物料分散均匀，采用水热法，离心过滤，烘干后，将粉体高温退火处理，冷却至室温，研磨，得TiO2/g-C3N4光阳极纳米复合材料。1. TiO 2 /gC 3 N 4 photoanode nanocomposite material, it is characterized in that, preparation method is: mix melamine and tetrabutyl titanate in ethanol, stir, make mixed material disperse uniformly, adopt hydrothermal method , centrifugal filtration, after drying, the powder is annealed at high temperature, cooled to room temperature, and ground to obtain a TiO 2 /gC 3 N 4 photoanode nanocomposite material. 2.如权利要求1所述的一种TiO2/g-C3N4光阳极纳米复合材料，其特征在于，所述三聚氰胺和钛酸四丁酯的摩尔比为3:1。2 . The TiO 2 /gC 3 N 4 photoanode nanocomposite material according to claim 1 , wherein the molar ratio of the melamine and tetrabutyl titanate is 3:1. 3 . 3.如权利要求1所述的一种TiO2/g-C3N4光阳极纳米复合材料，其特征在于，所述水热法的条件为：水热温度为180℃-200℃，时间为18h-24h。3 . The TiO 2 /gC 3 N 4 photoanode nanocomposite material according to claim 1 , wherein the conditions of the hydrothermal method are: the hydrothermal temperature is 180°C-200°C, and the time is 18h. 4 . -24h. 4.如权利要求1所述的一种TiO2/g-C3N4光阳极纳米复合材料，其特征在于，所述高温退火处理条件为：温度500-550℃，时间3-5h。4 . The TiO 2 /gC 3 N 4 photoanode nanocomposite material according to claim 1 , wherein the high temperature annealing treatment conditions are: temperature 500-550° C., time 3-5 h. 5 . 5.如权利要求1所述的一种TiO2/g-C3N4光阳极纳米复合材料，其特征在于，所述产物TiO2/g-C3N4光阳极纳米复合材料是N型半导体材料。5 . The TiO 2 /gC 3 N 4 photoanode nanocomposite material according to claim 1 , wherein the product TiO 2 /gC 3 N 4 photoanode nanocomposite material is an N-type semiconductor material. 6 . 6.如权利要求1-5任一项所述一种TiO2/g-C3N4光阳极纳米复合材料在制备TiO2/g-C3N4光电极薄膜上的应用，其特征在于，具体包括如下步骤：6. The application of a TiO 2 /gC 3 N 4 photoanode nanocomposite material in the preparation of a TiO 2 /gC 3 N 4 photoelectrode film as described in any one of claims 1-5, characterized in that it specifically includes the following step: 1)在含I2的丙酮水溶液中分散如权利要求1-5任一项所述的TiO2/g-C3N4光阳极纳米复合材料，并利用超声波震荡使TiO2/g-C3N4光阳极纳米复合材料悬浮于含I2的丙酮水溶液中，即获得电泳沉积悬浮液；1) Disperse the TiO 2 /gC 3 N 4 photoanode nanocomposite material as described in any one of claims 1-5 in an acetone aqueous solution containing I , and utilize ultrasonic vibration to make the TiO 2 / gC 3 N 4 photoanode The nanocomposite material is suspended in the acetone aqueous solution containing I to obtain the electrophoretic deposition suspension; 2)在电泳沉积悬浮液中放入两片等面积的透明导电玻璃FTO，并令两片导电玻璃导电面相对，且相互平行浸入电泳沉积悬浮液中，在直流电压条件下沉积1-5min；2) Put two pieces of transparent conductive glass FTO of equal area in the electrophoretic deposition suspension, and make the conductive surfaces of the two conductive glass faces face each other, and immerse them in the electrophoretic deposition suspension parallel to each other, and deposit under the condition of DC voltage for 1-5min; 3)切断电流，将两片导电玻璃从电泳沉积悬浮液中取出，在室温下晾干后，于马弗炉中，高温焙烧，得到TiO2/g-C3N4光电极薄膜。3) Cut off the current, take out two pieces of conductive glass from the electrophoretic deposition suspension, dry at room temperature, and bake in a muffle furnace at high temperature to obtain a TiO 2 /gC 3 N 4 photoelectrode film. 7.如权要求6所述的应用，其特征在于，步骤1)中所述的含I2的丙酮水溶液中，按体积比，丙酮:水＝25:1；每1ml丙酮水溶液中含有0.4mg的I2。7. application as claimed in claim 6, is characterized in that, in the acetone aqueous solution containing I described in step 1 ), by volume, acetone: water=25:1; In every 1ml aqueous acetone solution, contain 0.4mg I 2 . 8.如权要求6所述的应用，其特征在于，步骤2)中直流电压为20V-25V。8. The application according to claim 6, wherein the DC voltage in step 2) is 20V-25V. 9.如权要求6所述的应用，其特征在于，步骤3)中于马弗炉中焙烧温度为400-500℃，焙烧90min。9. application as claimed in claim 6, is characterized in that, in step 3) in muffle furnace roasting temperature is 400-500 ℃, roasting 90min.
CN201811510058.5A 2018-12-11 2018-12-11 A kind of TiO2/g-C3N4The preparation method and applications of light anode nanocomposite Pending CN109626422A (en)

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CN110706933A (en) * 2019-11-11 2020-01-17 厦门大学 Preparation method of titanium dioxide nanorod composite photoanode
CN111167500A (en) * 2020-02-02 2020-05-19 辽宁大学 A kind of Ag/g-C3N4 composite film and its preparation method and application
CN113189158A (en) * 2021-04-25 2021-07-30 武汉科技大学 Hydrogen sulfide photoelectrochemical sensor and preparation method thereof
CN113856757A (en) * 2021-11-04 2021-12-31 广东工业大学 A kind of polydopamine modified carbon nitride/titania supported foam nickel composite photocatalyst and its preparation method and application
CN114057406A (en) * 2022-01-17 2022-02-18 青岛理工大学 Composite photoanode film, preparation method and application thereof

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