CN102304737A - Zinc oxide/graphene oxide composite optical switch material and electrochemical preparation method thereof - Google Patents
Zinc oxide/graphene oxide composite optical switch material and electrochemical preparation method thereof Download PDFInfo
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Abstract
The invention discloses a zinc oxide/graphene oxide composite optical switch material and an electrochemical preparation method thereof. The composite material uses conductive glass as the substrate and is prepared by depositing a columnar zinc oxide film with thickness of 300-800 nm on an electrochemically deposited graphene oxide film with thickness of 8-30 nm through an electrochemical deposition method. The preparation method comprises the following steps: depositing a graphene oxide film with thickness of 8-30 nm by using a three-electrode system and taking indium tin oxide (ITO) as the working electrode; and then depositing columnar zinc oxide nano-crystals in a zinc nitrate solution by using the three-electrode system and taking the uniformly deposited graphene oxide film electrode as the working electrode to obtain the zinc oxide/graphene oxide composite optical switch material. The prepared composite material has the advantages of good film-forming property, uniform thickness, controllable optical and electrical properties, short photoelectric response time and the like; and the preparation process is simple, the yield is high and the period is short.
Description
Technical field
The present invention relates to a kind of zinc oxide/graphene oxide complex light switching material and electrochemical preparation method thereof, belong to light, electricity and transductive material technology of preparing.
Background technology
Zinc oxide is a kind of good conductor oxidate material, and energy gap is 3.37eV under the room temperature, and exciton binding energy is up to 60MeV.When its size is small; Specific surface area sharply increases; Thereby produce a series of unusual physical influences; Like quantum confined effect, surface effects, macro quanta tunnel effect etc.; Make it have many unusual characteristics, thereby produced the not available special property of its body phase material at aspects such as optics, electricity, magnetics, chemistry.It is had a wide range of applications aspect numerous at photoelectric device, chemical industry, medicine etc., and its prospect is very wide.
The photoelectric properties of ZnO nanometer stick array are paid attention to (Konenkamp R by people gradually at the beginning of 21 century; Word R C; Godinez M; Ultraviolet electro-luminescence from ZnO/polymer heterojunction light-emit-ring diodes[J] .Nano Lett; 2005; 5:2005); And can regulate the photoelectric property of material effectively through the control of pattern, therefore the control through preparation condition prepares the film that the ZnO nanoparticle of specific morphology constitutes and has evoked people's very big research enthusiasm.The method for preparing the ZnO nano thin-film has metal organic vapor phase epitaxy (MOCVD), sol-gel method, magnetron sputtering, electrochemical deposition (G.W.She, X H usually.Zhang，W．S?Shi，et?a1．Controlled?Synthesis?of?Oriented?Single-crystal?Zn0?Nanotube Arrays?on?Transparent?Conductive?Substrates[J]．
App1.Phys.Lett, 2008 (92): 0531l1.) wherein electrochemical deposition method owing to having the quality of forming film height, can realizing that atom level is mixed, equipment relatively simply, does not need the advantage of ultrahigh vacuum(HHV) to obtain special concern.
Graphene is a kind ofly to form the flat film that hexangle type is the honeycomb lattice by carbon atom with the sp2 hybridized orbital, has only two-dimensional material ((1.K.S. Novoselov, the A.K. Geim of a carbon atom thickness; S.V. Morozov, et al., Science science; 2004,306 volumes, 666; 2.C. Berger, Z.M. Song, X.B. Li, et al., Science science, 2006,312 volumes, 1191; 3.I. Meric, M.Y. Han, A.F. Young, et al., Nature Nanotechnology nature: nanosecond science and technology, 2008,3 volumes, 654.)).Graphene is a kind of semi-conductor of zero band gap, and its carrier mobility is up to 200000 cm
2/ (Vs), tensile modulus can reach 1100 GPa, thermal conductivity 5000 W/ (mK), and specific surface area can reach 2630 m
2/ g.Preparation method of graphene mainly contains mechanically peel method (K.S. Novoselov, A.K. Geim, S.V. Morozov at present; Et al., Science science, 2004; 306 volumes; 666.), chemical Vapor deposition process (K.S. Kim, Y. Zhao; H. Jang; Et al., Nature nature, 2009; 457 volumes; 706.) and chemistry redox method (C. Gomez-Navarro, R.T. Weitz, A.M. Bittner; Et al. Nano Letters nanometer wall bulletin; 2007,7 volumes, 3499.) etc.In these methods, the chemistry redox method is widely adopted because realizing the preparation low-cost in enormous quantities of Graphene.The film forming method of Graphene that oxidation reduction process is made has spin coating, pulling film forming, spraying film forming etc. still because the prepared Graphene of chemistry redox method has membrane thickness unevenness in film forming process; Institute's shortcoming such as blocked up of filming; The someone utilizes the method for electrochemical deposition to prepare uniform nano level graphene oxide film (［ 1 ］ Guo in recent years; C.X.; Et al.
.ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2010.
49(17): p. 3014-3017.).
Summary of the invention
The object of the present invention is to provide a kind of zinc oxide/graphene oxide complex light switching material and electrochemical preparation method thereof, this complex light switching material, it is good to have the even photoresponse performance of film forming, light, electrical property easy-regulating, advantage such as opto-electronic conversion speed is fast.Its preparation method process is simple, is suitable for scale operation.
The present invention realizes through following technical proposals: a kind of zinc oxide/graphene oxide complex light switching material; It is characterized in that; This complex light switching material is substrate with the ITO conductive glass; Reach the graphene oxide settled layer of 8-30nm in the substrate for thickness, reach the deposition of zinc oxide layer of 300-800nm on the graphene oxide layer for thickness.
The preparation method of above-mentioned zinc oxide/graphene oxide complex light switching material is characterized in that comprising following process:
1. tin indium oxide (ITO) conductive glass places acetone and deionized water for ultrasonic half an hour respectively, and nitrogen dries up subsequent use;
2. electrochemical deposition graphene oxide layer
Graphene oxide is scattered in the deionized water; Being made into concentration is the graphene oxide electrochemical deposition liquid of 0.2 mg/mL; In this electrochemical deposition liquid; The ITO conductive glass that cleans with step 1 is working electrode (resistance 15 Ω/square); Platinized platinum is a counter electrode; Mercurous chloride electrode is a reference electrode, at 25 ℃ of temperature and continuous current 0.5mA/cm
2Carry out electrochemical deposition under the condition 150 seconds-300 seconds, settling is dried up under condition of nitrogen gas, obtain the ITO electrode that surface coverage thickness reaches the graphene oxide layer of 8-30nm;
3. with Zn (NO
3)
26H
2O is scattered in the deionized water; Being made into concentration is the zinc nitrate electrochemical deposition liquid of 0.005mol/L-0.02mol/L; In this electrochemical deposition liquid; ITO electrode with the capping oxidation graphene layer of step 2 system is a working electrode; Platinized platinum is a counter electrode; Mercurous chloride electrode is that reference electrode carried out electrochemical deposition 5 minutes-20 minutes under 65 ℃ of temperature and constant voltage-1V condition, and settling is dried up under condition of nitrogen gas, obtains zinc oxide/graphene oxide complex light switching material.
This patent does not need high temperature and high vacuum condition not to need special reaction kit because of using the electrochemical production zinc oxide nano rod, and is simple with other zinc oxide/graphene preparation method comparison working condition, preparation cost is cheap realize nano level compound.And electrochemical deposition zinc oxide is because the pattern thickness of zinc oxide etc. exist positive correlation with conditions such as strength of solution reaction times in the electrochemical reaction; So can regulate and control the pattern of zinc oxide nano rod through simple regulation and control reaction solution concentration and growth time, thereby reach the purpose of regulation and control photoelectric properties.The method of the electrochemical growth graphene oxide of Cai Yonging is because of the characteristics that electrochemical growth had simultaneously, can produce thinner graphene film (8-30nm) than the method that other patents are in the past mentioned, and guarantee its uniform deposition on electrode.
Description of drawings:
Fig. 1 is the SEM photo of ITO electrode of the surface deposition graphene oxide layer of the embodiment of the invention 1 system.
Be deposited in the form of sheets on the ITO conductive glass face by the visible graphene oxide of this figure.
Fig. 2 is the zinc oxide/graphene oxide complex light switching material SEM photo of the embodiment of the invention 1 system.
By the zinc oxide film of this figure visible deposition on graphene oxide, wherein, zinc oxide is column, and diameter is 100-500 nm, and length is 300-800nm.
Embodiment
Providing 7 embodiment of the present invention below, is to further specify of the present invention, rather than limits scope of the present invention.
Embodiment 1:
Take by weighing the 10mg graphene oxide, be scattered in the 50ml deionized water, after ultra-sonic dispersion is even, adopt the three-electrode system electrochemical deposition, and working electrode employing ITO conductive glass (resistance 15 Ω/square), depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode adopts mercurous chloride electrode.25 ℃ of following continuous current 0.5mA/cm
2Deposit 150 seconds.Product dries up under condition of nitrogen gas, obtains the ITO electrode of surface coverage graphene oxide film.Take by weighing 297.5mg Zn (NO
3)
26H
2O is scattered in the 50ml deionized water, adopts the three-electrode system electrochemical deposition, and working electrode adopts the ITO electrode of the capping oxidation graphene film for preparing, depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode is selected mercurous chloride electrode for use.65 ℃ of following constant voltages-1V depositing time 20 minutes.Product dries up under condition of nitrogen gas, and products therefrom is optical Response zinc oxide/graphene composite material.
With the gained matrix material as working electrode; Be counter electrode with the platinized platinum simultaneously; Mercurous chloride electrode is constructed three-electrode system as reference electrode, and this zinc oxide/graphene oxide material has tangible photocurrent response under the 365nm UV-irradiation in the KCl of 0.1M solution, and the time of response is less than 0.5s.
Embodiment 2:
Take by weighing the 10mg graphene oxide, be scattered in the 50ml deionized water, after ultra-sonic dispersion is even, adopt the three-electrode system electrochemical deposition, and working electrode employing ITO conductive glass (resistance 15 Ω/square), depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode adopts mercurous chloride electrode.25 ℃ of following continuous current 0.5mA/cm
2Deposit 150 seconds.Product dries up under condition of nitrogen gas, obtains the ITO electrode of surface coverage graphene oxide film.Take by weighing 148.75mg Zn (NO
3)
26H
2O is scattered in the 50ml deionized water, adopts the three-electrode system electrochemical deposition, and working electrode adopts the ITO electrode of the capping oxidation graphene film for preparing, depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode is selected mercurous chloride electrode for use.65 ℃ of following constant voltages-1V depositing time 20 minutes.Product dries up under condition of nitrogen gas, and products therefrom is optical Response zinc oxide/graphene composite material.
With the gained matrix material as working electrode; Be counter electrode with the platinized platinum simultaneously; Mercurous chloride electrode is constructed three-electrode system as reference electrode, and this zinc oxide/graphene oxide material has tangible photocurrent response under the 365nm UV-irradiation in the KCl of 0.1M solution, and the time of response is less than 0.5s.
Embodiment 3:
Take by weighing the 10mg graphene oxide, be scattered in the 50ml deionized water, after ultra-sonic dispersion is even, adopt the three-electrode system electrochemical deposition, and working electrode employing ITO conductive glass (resistance 15 Ω/square), depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode adopts mercurous chloride electrode.25 ℃ of following continuous current 0.5mA/cm
2Deposit 225 seconds.Product dries up under condition of nitrogen gas, obtains the ITO electrode of surface coverage graphene oxide film.Take by weighing 223.12mg Zn (NO
3)
26H
2O is scattered in the 50ml deionized water, adopts the three-electrode system electrochemical deposition, and working electrode adopts the ITO electrode of the capping oxidation graphene film for preparing, depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode is selected mercurous chloride electrode for use.65 ℃ of following constant voltages-1V depositing time 15 minutes.Product dries up under condition of nitrogen gas, and products therefrom is optical Response zinc oxide/graphene composite material.
With the gained matrix material as working electrode; Be counter electrode with the platinized platinum simultaneously; Mercurous chloride electrode is constructed three-electrode system as reference electrode, and this zinc oxide/graphene oxide material has tangible photocurrent response under the 365nm UV-irradiation in the KCl of 0.1M solution, and the time of response is less than 0.5s.
Embodiment 4:
Take by weighing the 10mg graphene oxide, be scattered in the 50ml deionized water, after ultra-sonic dispersion is even, adopt the three-electrode system electrochemical deposition, and working electrode employing ITO conductive glass (resistance 15 Ω/square), depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode adopts mercurous chloride electrode.25 ℃ of following continuous current 0.5mA/cm
2Deposit 300 seconds.Product dries up under condition of nitrogen gas, obtains the ITO electrode of surface coverage graphene oxide film.Take by weighing 74.375mg Zn (NO
3)
26H
2O is scattered in the 50ml deionized water, adopts the three-electrode system electrochemical deposition, and working electrode adopts the ITO electrode of the capping oxidation graphene film for preparing, depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode is selected mercurous chloride electrode for use.65 ℃ of following constant voltages-1V depositing time 5 minutes.Product dries up under condition of nitrogen gas, and products therefrom is optical Response zinc oxide/graphene composite material.
With the gained matrix material as working electrode; Be counter electrode with the platinized platinum simultaneously; Mercurous chloride electrode is constructed three-electrode system as reference electrode, and this zinc oxide/graphene oxide material has tangible photocurrent response under the 365nm UV-irradiation in the KCl of 0.1M solution, and the time of response is less than 0.5s.
Embodiment 5:
Take by weighing the 10mg graphene oxide, be scattered in the 50ml deionized water, after ultra-sonic dispersion is even, adopt the three-electrode system electrochemical deposition, and working electrode employing ITO conductive glass (resistance 15 Ω/square), depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode adopts mercurous chloride electrode.25 ℃ of following continuous current 0.5mA/cm
2Deposit 150 seconds.Product dries up under condition of nitrogen gas, obtains the ITO electrode of surface coverage graphene oxide film.Take by weighing 297.5mg Zn (NO
3)
26H
2O is scattered in the 50ml deionized water, adopts the three-electrode system electrochemical deposition, and working electrode adopts the ITO electrode of the capping oxidation graphene film for preparing, depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode is selected mercurous chloride electrode for use.65 ℃ of following constant voltages-1V depositing time 5 minutes.Product dries up under condition of nitrogen gas, and products therefrom is optical Response zinc oxide/graphene composite material.
With the gained matrix material as working electrode; Be counter electrode with the platinized platinum simultaneously; Mercurous chloride electrode is constructed three-electrode system as reference electrode, and this zinc oxide/graphene oxide material has tangible photocurrent response under the 365nm UV-irradiation in the KCl of 0.1M solution, and the time of response is less than 0.5s.
Embodiment 6:
Take by weighing the 10mg graphene oxide, be scattered in the 50ml deionized water, after ultra-sonic dispersion is even, adopt the three-electrode system electrochemical deposition, and working electrode employing ITO conductive glass (resistance 15 Ω/square), depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode adopts mercurous chloride electrode.25 ℃ of following continuous current 0.5mA/cm
2Deposit 300 seconds.Product dries up under condition of nitrogen gas, obtains the ITO electrode of surface coverage graphene oxide film.Take by weighing 297.5mg Zn (NO
3)
26H
2O is scattered in the 50ml deionized water, adopts the three-electrode system electrochemical deposition, and working electrode adopts the ITO electrode of the capping oxidation graphene film for preparing, depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode is selected mercurous chloride electrode for use.65 ℃ of following constant voltages-1V depositing time 20 minutes.Product dries up under condition of nitrogen gas, and products therefrom is optical Response zinc oxide/graphene composite material.
With the gained matrix material as working electrode; Be counter electrode with the platinized platinum simultaneously; Mercurous chloride electrode is constructed three-electrode system as reference electrode, and this zinc oxide/graphene oxide material has tangible photocurrent response under the 365nm UV-irradiation in the KCl of 0.1M solution, and the time of response is less than 0.5s.
Embodiment 7:
Take by weighing the 10mg graphene oxide, be scattered in the 50ml deionized water, after ultra-sonic dispersion is even, adopt the three-electrode system electrochemical deposition, and working electrode employing ITO conductive glass (resistance 15 Ω/square), depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode adopts mercurous chloride electrode.25 ℃ of following continuous current 0.5mA/cm
2Deposit 225 seconds.Product dries up under condition of nitrogen gas, obtains the ITO electrode of surface coverage graphene oxide film.Take by weighing 74.375mg Zn (NO
3)
26H
2O is scattered in the 50ml deionized water, adopts the three-electrode system electrochemical deposition, and working electrode adopts the ITO electrode of the capping oxidation graphene film for preparing, depositional area 1cm
2, counter electrode adopts platinized platinum, and reference electrode is selected mercurous chloride electrode for use.65 ℃ of following constant voltages-1V depositing time 10 minutes.Product dries up under condition of nitrogen gas, and products therefrom is optical Response zinc oxide/graphene composite material.
With the gained matrix material as working electrode; Be counter electrode with the platinized platinum simultaneously; Mercurous chloride electrode is constructed three-electrode system as reference electrode, and this zinc oxide/graphene oxide material has tangible photocurrent response under the 365nm UV-irradiation in the KCl of 0.1M solution, and the time of response is less than 0.5s.
Claims (2)
1. zinc oxide/graphene oxide complex light switching material; It is characterized in that; This complex light switching material is substrate with the ITO conductive glass, reaches the graphene oxide settled layer of 8-30nm in the substrate for thickness, reaches the deposition of zinc oxide layer of 300-800nm on the graphene oxide layer for thickness.
2. electrochemical method for preparing the described zinc oxide of claim 1/graphene oxide complex light switching material is characterized in that comprising following process:
(1) indium tin oxide-coated glass places acetone and deionized water for ultrasonic half an hour respectively, and nitrogen dries up subsequent use;
(2) electrochemical deposition graphene oxide layer
Graphene oxide is scattered in the deionized water; Being made into concentration is the graphene oxide electrochemical deposition liquid of 0.2 mg/mL; In this electrochemical deposition liquid; The indium tin oxide-coated glass that cleans with step 1 is a working electrode; Platinized platinum is a counter electrode; Mercurous chloride electrode is a reference electrode, at 25 ℃ of temperature and continuous current 0.5mA/cm
2Carry out electrochemical deposition under the condition 150 seconds-300 seconds, settling is dried up under condition of nitrogen gas, obtain the indium-tin oxide electrode that surface coverage thickness reaches the graphene oxide layer of 8-30nm
;
(3) with Zn (NO
3)
26H
2O is scattered in the deionized water; Being made into concentration is the zinc oxide electrochemical deposition liquid of 0.005mol/L-0.02mol/L; In this electrochemical deposition liquid; Indium-tin oxide electrode with the capping oxidation graphene layer of step 2 system is a working electrode; Platinized platinum is a counter electrode; Mercurous chloride electrode is that reference electrode carried out electrochemical deposition 5 minutes-20 minutes under 65 ℃ of temperature and constant voltage-1V condition, and settling is dried up under condition of nitrogen gas, obtains zinc oxide/graphene oxide complex light switching material.
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| CN104541358B (en) * | 2012-06-05 | 2018-01-16 | 斯特拉塔西斯公司 | The base material of graphene coated and the composite of gained |
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| CN114512681A (en) * | 2022-01-29 | 2022-05-17 | 辽宁大学 | Electrode material for biofuel cell and preparation method and application thereof |
| CN114512681B (en) * | 2022-01-29 | 2024-02-20 | 辽宁大学 | Electrode material for biofuel cell and preparation method and application thereof |
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