CN105244408A - Method for preparing cuprous oxide photoelectric film by copper chloride - Google Patents
Method for preparing cuprous oxide photoelectric film by copper chloride Download PDFInfo
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- CN105244408A CN105244408A CN201410261274.6A CN201410261274A CN105244408A CN 105244408 A CN105244408 A CN 105244408A CN 201410261274 A CN201410261274 A CN 201410261274A CN 105244408 A CN105244408 A CN 105244408A
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- cuprous oxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a method for preparing a cuprous oxide photoelectric film by copper chloride, and belongs to the technical field of photoelectric film preparation. The method comprises the steps of firstly cleaning a substrate, then putting CuCl2.2H2O and sodium citrate into a solvent, carrying out constant potential deposition on a tin dioxide conductive glass substrate by adopting an electro-deposition method, and finally carrying out cleaning and drying to acquire the cuprous oxide photoelectric film. The method provided by the invention does not need a high-temperature high-vacuum condition, has low requirements for instruments and equipment, and is low in production cost, high in production efficiency and easy to operate. The prepared cuprous oxide photoelectric film has good continuity and uniformity. The new technology is easy to control composition and structure of a target product, and a preparation method, which is low in cost and capable of realizing industrialization, is provided for preparing the high-performance cuprous oxide photoelectric film.
Description
Technical field
The invention belongs to optoelectronic film preparing technical field, particularly relate to a kind of method being prepared cuprous oxide optoelectronic film by copper chloride.
Background technology
The direct energy-gap semiconductor of cuprous oxide to be a kind of energy gap be 1.9 ~ 2.2eV, exciton can transport continuously in monocrystalline, it is made to have higher absorptivity, become the important materials making photovoltaic converter, because it has unique light, magnetic performance, in solar energy conversion, electronics, magnetic storage device, bio-sensing and catalysis, there is potential application.And asepsis environment-protecting, theoretical efficiency is about 20%, and cost is cheap, has good photovoltaic application prospect.
Prepare cuprous oxide film and can adopt thermal oxidation method, free-radical oxidation method, magnetron sputtering method, pulsed laser deposition and electrochemical deposition technique.Current employing electrodeposition process prepares Cu
2in the research of O film, mainly contain following three kinds of sedimentary systems available: (l) copper nitrate system; (2) Schweinfurt green and cruel sour sodium system; (3) copper sulphate and acid system.
The present invention adopts copper chloride and natrium citricum system to prepare cuprous oxide optoelectronic film with electrochemical deposition method in acid condition, the method has low temperature, low cost, large-scale production prospect, can at the deposited on substrates film of complex topography and pattern and the composition of being convenient to control objectives deposit film, the equal wide material sources of raw material, weigh and easy and simple to handle, environmentally friendly.
As method noted earlier, other method also has different defects.Related to the present invention also has as Publication about Document:
[1] swallow roc, Cai Shu, military defense soldier, electrochemical production p-type Cu
2the sign of O semiconductive thin film and performance thereof. XI AN JIAOTONG UNIVERSITY Subject Index 45.3 (2011): 121-124.
Article essentially describes and utilizes copper sulphate and lactic acid etc. to do raw material to utilize the method for electro-deposition to prepare cuprous oxide film, have studied the impact on cuprous oxide film stuctures and properties of complexing agent kind, sedimentation potential and solution ph. result shows: large in the film crystallite dimension that to take lactic acid as the crystallite dimension of the cuprous oxide film deposited in the electrolyte of complexing agent than with triethanolamine be deposits in the electrolyte of complexing agent, better crystallinity degree, density is higher.
[2]Wang,Lida,GuichangLiu,andDongfengXue，EffectsofsupportingelectrolyteongalvanicdepositionofCu
2Ocrystals，ElectrochimicaActa56.18(2011):6277-6283.
There is provided copper ion to utilize the method for electro-deposition to prepare cuprous oxide film with copper nitrate herein, mainly have studied the impact of additive on film, result shows that the existence of additive not only also has impact to the Cheng Xiangyou impact of film to the structure of growing thin-film crystal.
[3]Mao-ChiaHuang,TsingHaiWang,Wen-ShengChang.Temperaturedependenceonp-Cu
2Othinfilmelectrochemicallydepositedontocoppersubstrate.AppliedSurfaceScience.02.085(2014):27301.
Utilize the method for electro-deposition to prepare cuprous oxide film with copper sulphate and lactic acid as raw material herein, mainly have studied the pattern of temperature on film and the impact of structure.
[4] Bi Wentuan, the progress of process for preparing Cu 2 O. Chemical Industry in Guangzhou, 37.8 (2009): 56-58.
Mainly describe herein and variously prepare the method for cuprous oxide film and present progress.
[5]Nian,Jun-Nan,Che-ChiaHu,andHsishengTeng,Electrodepositedp-typeCu
2OforH
2evolutionfromphotoelectrolysisofwaterundervisiblelightillumination.Internationaljournalofhydrogenenergy33.12(2008):2897-2903.
Copper sulphate is utilized to provide copper ion herein, the method of electro-deposition is used to prepare cuprous oxide film, mainly have studied the impact of depositing temperature on membrane structure, result surface obtains different membrane structures at different temperature, and high preferred orientation also there occurs change.
Summary of the invention
The present invention in order to solve the deficiencies in the prior art, and invents preparation method that is a kind of and the diverse cuprous oxide optoelectronic film of the preparation method of prior art.
The present invention adopts electro-deposition method, stannous chloride and natrium citricum system is utilized to prepare cuprous oxide optoelectronic thin film material, tin dioxide conductive glass is adopted to be substrate, with copper chloride and natrium citricum for raw material, take distilled water as solvent, be that assist medium is to adjust the pH value of solution with watery hydrochloric acid, by certain stoichiometric proportion obtain solution, adopt three electrode assemblies, platinum electrode is as auxiliary electrode, saturated calomel electrode is as reference electrode, tin dioxide conductive substrate of glass is work electrode, transistor potentiostat is used to deposit under the condition of constant potential, target product is obtained through specific sedimentation time.
Concrete preparation method of the present invention comprises the step of following order:
A. the cleaning of electro-conductive glass substrate is carried out.Be that volume ratio chloroform put into by 20mm × 10mm × 4mm tin dioxide conductive glass: the solution of ethanol=5:1, Ultrasonic Cleaning 30min by size; Again sheet glass is put into volume ratio acetone: the solution of distilled water=5:1, Ultrasonic Cleaning 30min; Again in distilled water by electro-conductive glass substrate sonic oscillation 30min; Being emitted in glass dish by tin dioxide conductive glass substrate obtained above sends in baking oven, dries, for masking at 100 DEG C;
B. by CuCl
22H
2o and natrium citricum are dissolved in solvent, make the material Homogeneous phase mixing in solution, and adjust ph.Specifically, can 1 part of natrium citricum be fully dissolved in the distilled water solvent of 259 parts, by 1.32 parts of CuCl
22H
2o is dissolved in above-mentioned solution, makes the material Homogeneous phase mixing in solution, can add the pH value that 10 ~ 20 parts, watery hydrochloric acid adjusts solution;
C. pour in three electrode assemblies by the solution that step b configures, take platinum electrode as auxiliary electrode, saturated calomel electrode is reference electrode, and tin dioxide conductive glass is Electrode, is linked to transistor potentiostat, deposits under the condition of constant potential;
D., after specific sedimentation time, sample is taken out, cleans print with distilled water, being put in baking oven is heated between 50 ~ 70 DEG C, temperature retention time 10 ~ 20min, and then cool to room temperature takes out, after making its natural drying, namely obtain the cuprous oxide optoelectronic film of compact crystallization.
The present invention does not need high temperature high vacuum condition, and raw material sources are extensive, weigh easy, and require low to instrument and equipment, production cost is low, and production efficiency is high, is easy to operation.Gained cuprous oxide optoelectronic film has good continuity, compactness and uniformity, and this new method is that the high performance cuprous oxide optoelectronic film of preparation provides a kind of method that cost is low, can realize large-scale industrial production.
Accompanying drawing explanation
Accompanying drawing 1 is sedimentation potential is-1.0V, sedimentation time is 30min, the XRD collection of illustrative plates of gained cuprous oxide film, result shows gained cuprous oxide film edge (110), (111), (200), the growth of (211) crystal face.
Embodiment
Embodiment 1
A. the cleaning of glass substrate: carry out cleaning tin dioxide conductive glass substrate (size is 20mm × 10mm × 4mm) as previously mentioned.
B. 1 part of natrium citricum is fully dissolved in the distilled water solvent of 259 parts, by 1.32 parts of CuCl
22H
2o is dissolved in above-mentioned solution, makes the material Homogeneous phase mixing in solution, can add the pH value that 10 ~ 20 parts, watery hydrochloric acid adjusts solution, make the pH=2 of solution.
C. pour in three electrode assemblies by the solution that step b configures, take platinum electrode as auxiliary electrode, saturated calomel electrode is reference electrode, tin dioxide conductive glass is Electrode, is linked to transistor potentiostat, in-1.0V sedimentation potential, normal temperature, deposits under not having the condition stirred.
D. after depositing 30min, taken out by sample, clean print, be put in baking oven and be heated between 50 ~ 70 DEG C, temperature retention time 10 ~ 20min with distilled water, then cool to room temperature takes out, and after making its natural drying, namely obtains the cuprous oxide optoelectronic film of compact crystallization.
Claims (1)
1. prepared a method for cuprous oxide optoelectronic film by copper chloride, comprise the step of following order:
A. carrying out the cleaning of electro-conductive glass substrate, is that volume ratio chloroform put into by 20mm × 10mm × 4mm tin dioxide conductive glass: the solution of ethanol=5:1, Ultrasonic Cleaning 30min by size; Again sheet glass is put into volume ratio acetone: the solution of distilled water=5:1, Ultrasonic Cleaning 30min; Again in distilled water by electro-conductive glass substrate sonic oscillation 30min; Tin dioxide conductive glass substrate obtained above is put into baking oven, dries at 100 DEG C, for masking;
B. by CuCl
22H
2o and natrium citricum are dissolved in solvent, make the material Homogeneous phase mixing in solution, and adjust ph, specifically, can 1 part of natrium citricum be fully dissolved in the distilled water solvent of 259 parts, by 1.32 parts of CuCl
22H
2o is dissolved in above-mentioned solution, makes the material Homogeneous phase mixing in solution, can add the pH value that 10 ~ 20 parts, watery hydrochloric acid adjusts solution;
C. pour in three electrode assemblies by the solution that step b configures, take platinum electrode as auxiliary electrode, saturated calomel electrode is reference electrode, and tin dioxide conductive glass is Electrode, is connected to transistor potentiostat, deposits under the condition of constant potential;
D., after specific sedimentation time, taken out by sample, clean print, be put in baking oven and be heated between 50 ~ 70 DEG C, temperature retention time 10 ~ 20min with distilled water, then cool to room temperature takes out, and after making its natural drying, namely obtains cuprous oxide optoelectronic film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105696047A (en) * | 2016-01-26 | 2016-06-22 | 太原理工大学 | Rapid preparation method for cuprous oxide nano-film |
| CN107020103A (en) * | 2017-03-20 | 2017-08-08 | 浙江工商大学 | A kind of iron oxide molybdenum sulfide cuprous oxide photocatalysis film and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732928A (en) * | 2012-07-18 | 2012-10-17 | 西北工业大学 | Preparation method of cuprous oxide semiconductor film material |
| CN103066345A (en) * | 2011-10-21 | 2013-04-24 | 中国科学院上海硅酸盐研究所 | Photoelectric chemical battery electrode and preparation method and application thereof |
| CN103364464A (en) * | 2013-07-31 | 2013-10-23 | 盐城工学院 | Construction method of photoelectric chemical sensor for detection of reduced glutathione |
-
2014
- 2014-06-13 CN CN201410261274.6A patent/CN105244408B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103066345A (en) * | 2011-10-21 | 2013-04-24 | 中国科学院上海硅酸盐研究所 | Photoelectric chemical battery electrode and preparation method and application thereof |
| CN102732928A (en) * | 2012-07-18 | 2012-10-17 | 西北工业大学 | Preparation method of cuprous oxide semiconductor film material |
| CN103364464A (en) * | 2013-07-31 | 2013-10-23 | 盐城工学院 | Construction method of photoelectric chemical sensor for detection of reduced glutathione |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105696047A (en) * | 2016-01-26 | 2016-06-22 | 太原理工大学 | Rapid preparation method for cuprous oxide nano-film |
| CN107020103A (en) * | 2017-03-20 | 2017-08-08 | 浙江工商大学 | A kind of iron oxide molybdenum sulfide cuprous oxide photocatalysis film and its preparation method and application |
| CN107020103B (en) * | 2017-03-20 | 2019-05-31 | 浙江工商大学 | A kind of iron oxide-molybdenum sulfide-cuprous oxide photocatalysis film and its preparation method and application |
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