CN110241433B - Size-controllable AgCuO2 nano material and preparation and application thereof - Google Patents

Size-controllable AgCuO2 nano material and preparation and application thereof Download PDF

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CN110241433B
CN110241433B CN201910549145.XA CN201910549145A CN110241433B CN 110241433 B CN110241433 B CN 110241433B CN 201910549145 A CN201910549145 A CN 201910549145A CN 110241433 B CN110241433 B CN 110241433B
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李斌
范心怡
顾燕芳
徐菁利
芮一川
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Shanghai University of Engineering Science
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Abstract

The invention relates to AgCuO with controllable size2The nanometer material and the preparation and the application thereof, the specific preparation process of the nanometer material is as follows: (1) adding silver nitrate or silver acetate as silver source and cupric source into pure water in sequence for dissolving, and then adding NH under stirring3H2Forming mixed solution by O, adding an alkali source to make the solution be strongly alkaline, finally obtaining a reaction solution obtained by the stable and transparent dark blue solution (2), reacting at a certain temperature by adopting an electrodeposition method and an anodic oxidation method, passing current for a certain time on a working electrode, repeatedly washing with deionized water and ethanol after deposition, and drying to finally obtain AgCuO2And (3) nano materials. Compared with the prior art, the method has the advantages of lower raw material cost, simple operation, short reaction time and low temperature, and the obtained AgCuO2The nano particles are smaller in size, can be directly prepared into a transparent film, and have excellent physical and chemical properties and the like.

Description

Size-controllable AgCuO2Nano material and preparation and application thereof
Technical Field
The invention belongs to the technical field of p-type semiconductor nano materials, and relates to AgCuO with controllable size2Nanosheets and their preparation.
Background
AgCuO2The material is composed of copper, silver and oxygen elements which are abundant in earth reserves and nontoxic, is an environment-friendly Ag-Cu multi-element metal oxide p-type narrow-band-gap semiconductor material with a similar manganite structure, has the forbidden band width of 1.5-2.2eV, has good carrier mobility, optical transparency, good thermal stability and other properties, and is widely applied to the fields of p-type transparent semiconductors, battery anode materials, photocatalysis, diodes, solar batteries and the like. However, there are problems that: (1) to obtain pure phase AgCuO2Material, requires Ag2Cu2O3The intermediate has high energy consumption and poor grain dispersibility; (2) the synthesized crystal grain has overlarge size (micron level), small specific surface area, difficult film formation and incapability of fully highlighting the advantages of the nano material, and limits the application of the materialThe range is used. Therefore, AgCuO with smaller grain size is prepared by a low-temperature method2Nanoparticles are of great significance.
AgCuO2The crystal belongs to monoclinic system, C2/m space group, AgCuO due to different electronic structures2The crystal is in a layered structure and is similar to a manganese copper ore Cu+Mn3+O2Equivalent to the respective substitution of silver ions and copper ions for Cu+And Mn3+But AgCuO2Electron valence structure of (1) and manganese copper ore Cu+Mn3+O2Not exactly the same. In AgCuO2In the oxide, Ag and Cu are not in single +1 and +3 valence states, charge delocalization exists among three atoms of Ag, Cu and O, and both Ag and Cu are partially oxidized into high valence states, so that the oxide can be expressed as Ag(1+x)+Cu(2+y)+O2Wherein the values of x and y vary depending on the preparation method.
Conventional preparation of AgCuO2The crystal is prepared by precursor Ag2Cu2O3Preparing Ag2Cu2O3On the basis of using persulfate, ozone and the like as oxidants to Ag2Cu2O3Chemical oxidation is carried out on the suspension to prepare AgCuO2But due to AgCuO obtained by chemical precipitation2The crystallinity is not high. People also go through Ag2Cu2O3Carries out electrochemical oxidation to prepare AgCuO2And (3) a solid. Curda et al, K in 20012S2O8As an oxidizing agent, Ag is used respectively2Cu2O3Suspension and AgNO3、Cu(NO3)2The alkaline aqueous solution is used as a precursor, and AgCuO is obtained by chemical oxidation2And (3) solid powder. (J.Curda, W.Klein, and M.Jansen, J.solid State chem., 162,220 (2001.))
In recent years, researches show that AgCuO can be greatly reduced by adopting a chemical deposition process2Reaction temperature and particle size of the nanomaterial. In 2014, Padmavathy N and the like use persulfate (K) under alkaline conditions by using silver acetate and copper acetate as raw materials2S2O8) For oxidation ofAgCuO with the size close to 100nm is prepared at room temperature2Nanoparticles, but cannot be made into films due to poor dispersibility. (RSC Advances,2014,4(107):62746-2And (3) a solid. Lu et al successfully prepared nanosheets with a size of approximately 500nm on an ITO working electrode by an electrochemical deposition method in 2017, but the film formed by the oversize has a low transmittance and is not suitable for solar cells. (Journal of The Electrochemical Society, 2017,164(4): D130-D134.)
It can be found that AgCuO with small particle size and high dispersion can be prepared at low temperature2The nano particles are still a technical problem, and AgCuO is regulated and controlled by controlling the concentration of a precursor and the reaction time2The size of the nanoparticles is more difficult. If the size of the superfine AgCuO can be controlled2The macro production of the nano particles can obtain high economic benefit and can simultaneously treat AgCuO2The promotion of the fields of catalyst-based materials, solar cells, and the like is of great benefit.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide AgCuO with controllable size2Nano material, preparation and application thereof, innovatively adopting low-Cost (CH)3COOAg or AgNO3) Silver acetate or silver nitrate as silver source, and any cupric copper such as Cu (NO)3)2Or Cu (CH)3COO)2Is a Cu source, and can obtain superfine AgCuO with controllable size through electrodeposition reaction in water bath at low temperature2Nanoparticles, with a particle size of at least approximately 80 nm.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention is to provide AgCuO with controllable size2The preparation method of the nano material is characterized by comprising the following steps:
(1) uniformly mixing a silver source and a cupric source solution, adding ammonia water, stirring, and adding an alkali source to make the solution be strongly alkaline (the pH value is more than or equal to 13) to obtain a stable and transparent mixed solution for later use;
(2) will step withTaking the mixed solution obtained in the step (1) as an electrolyte solution, adopting an electrodeposition method, electrifying the working electrode by an anodic oxidation method, and depositing to obtain AgCuO2And (4) nanosheet, namely completing.
Further, the silver source is silver nitrate or silver acetate, and the cupric source is cupric nitrate or cupric acetate.
Further, the molar ratio of the silver source to the divalent copper source is 1.1-1.5: 1.
Further, the alkali source is sodium hydroxide and/or potassium hydroxide, and the addition amount of the alkali source is 1-10mol/L of hydroxide ion concentration in the mixed solution.
Further, the addition amount of ammonia water satisfies: the concentration of the compound in the mixed solution is 1-10 mol/L.
Furthermore, the electrifying current of the working electrode is 0.01-0.4A, and the electrifying time is 30-300 s.
Further, the temperature of the electrochemical deposition is 40-70 ℃.
The second technical scheme of the invention is to provide AgCuO with controllable size2The nano material is prepared by the preparation method, and the prepared AgCuO2The nano material is a two-dimensional nano sheet, the minimum transverse dimension of the nano material is 80nm, and the thickness of the nano material is 15-30 nm.
The third technical proposal of the invention is to provide AgCuO with controllable size2The application of the nano material as a p-type hole transport material in the preparation of solar cells.
AgCuO prepared in the invention2The nano-sheet has controllable size, the minimum size reaches 80 nanometers, and the nano-sheet is an excellent p-type hole transport material and can be used for perovskite solar cells and organic solar cells. The invention adopts silver acetate as a silver source in an electrochemical deposition method for the first time, and prepares the superfine AgCuO at low temperature2Nanosheets. The solution before electrodeposition needs to be added with excessive ammonia water and strong base to adjust the acidity or basicity, so as to form a stable complex. If the amounts of the ammonia water and the alkali source are not within the limits of the conditions, the stable complex transparent solution cannot be formed by electrodepositing the precursor solution. Is unfavorable for the synthesis of substances and the synthesis of uniform sizeThe product of (1). If the current magnitude is not in a limited range during the electrodeposition process, the phase of the synthesized product is impure due to low electrifying current, and the particle size of the product is overlarge and uneven due to high electrifying current. If the temperature is not within the limited range during the electrodeposition process, the excessively low temperature will result in the solution being unable to form crystal nuclei, and the crystal nuclei will have uneven sizes, thereby affecting the product size and making the product size uneven. Too high a temperature causes a large number of nuclei to be rapidly formed inside the solution, and the size of the formed nuclei is too large, so that the product size is affected and the product size is not uniform.
Electrodeposition of AgCuO2The main principle of (1) is that Ag (I) and Cu (II) in the solution before electrodeposition are mainly [ Ag (NH)3)2]+And [ Cu (NH)3)4]2+Form exists, and as electrodeposition proceeds, the pH of the electrode surface decreases, Ag+And Cu2+Is gradually released and reacts with OH in the solution-After the reaction, the co-oxide AgCuO is generated2. In addition, the invention has cheap raw materials and simple and convenient reaction operation, and is more suitable for commercial popularization.
Compared with the prior art, the invention has the following advantages:
(1) the size can be controlled: according to the invention, the grain size of the nanosheet can be flexibly regulated and controlled by adjusting the concentration, temperature, electrifying time and current of the precursor of the reaction system, so that the nanosheet with controllable size is obtained;
(2) the preparation method can be used for preparing the film: the silver source and the copper source adopted by the invention have low price, can be directly prepared on the working electrode to form a film, have high transmittance, and solve the defects of large particle size, poor dispersibility and difficult film formation.
(3) The preparation process is simple: the invention adopts a simple and high-efficiency electrodeposition synthesis method to synthesize AgCuO2The nano-sheet has simple and convenient process route, low energy consumption, short time consumption and high yield, and can realize AgCuO with controllable size and high crystallinity2Preparing a nano sheet;
(4) the product performance is excellent: AgCuO synthesized by the invention2The nano-sheet has good crystallinity and excellent photoelectric property, and is used for perovskite sunThe photoelectric conversion efficiency can exceed 4% after the cell is used.
Drawings
FIG. 1 is AgCuO prepared in example 12A field emission scanning electron microscope image of the nanosheets;
FIG. 2 is AgCuO prepared in example 22A field emission scanning electron microscope image of the nanosheets;
FIG. 3 is AgCuO prepared in example 32A field emission scanning electron microscope image of the nanosheets;
FIG. 4 is AgCuO prepared in example 42A field emission scanning electron microscope image of the nanosheets;
FIG. 5 is an X-ray diffraction pattern of a reaction product prepared in example 1 with a molar ratio of Ag to Cu of 1.25: 1;
FIG. 6 is AgCuO prepared in comparative example 12A field emission scanning electron microscope image of the nano material;
FIG. 7 is AgCuO prepared in comparative example 22A field emission scanning electron microscope image of the nano material;
FIG. 8 shows AgCuO prepared in example 32The nano-sheet is used for a photocurrent voltage curve of the perovskite solar cell.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, the starting materials and the treatment steps used are conventional commercial products and conventional techniques, unless otherwise specified.
Example 1
CH was weighed at room temperature according to a Ag: Cu molar ratio of 1.25:13COOAg and Cu (NO)3)2·3H2Taking 50 ml of pure water, sequentially adding 0.001875mol of silver acetate and 0.0015mol of copper nitrate trihydrate under the condition of magnetic stirring, and then adding 0.05mol of ammonia water and 0.5mol of sodium hydroxide to form a stable and transparent dark blue solution; the obtained reaction solution is subjected to an electrodeposition method, and the reaction solution is subjected to a reaction of passing through 0 on a working electrode04A, controlling the reaction temperature at 40 ℃ and the electrifying time at 100 s; and taking out the precipitate after the reaction is finished, and repeatedly washing and drying the precipitate by using pure water and ethanol. FIG. 1 is AgCuO prepared in example 12The field emission scanning electron microscope image of the nano sheet shows AgCuO2The nanoplatelets have an average diameter of about 80-100 nanometers.
Example 2
CH was weighed at room temperature according to a Ag: Cu molar ratio of 1.25:13COOAg and Cu (NO)3)2·3H2Taking 50 ml of pure water, sequentially adding 0.001875mol of silver acetate and 0.0015mol of copper nitrate trihydrate under the condition of magnetic stirring, and then adding 0.05mol of ammonia water and 0.1mol of sodium hydroxide to form a stable and transparent dark blue solution; the obtained reaction solution is subjected to an electrodeposition method, 0.04A current is passed through a working electrode, the reaction temperature is controlled at 40 ℃, and the electrifying time is 150 s; and taking out the precipitate after the reaction is finished, and repeatedly washing and drying the precipitate by using pure water and ethanol. FIG. 2 is AgCuO prepared in example 22The field emission scanning electron microscope image of the nano sheet shows AgCuO2The average diameter of the nanosheets is about 200-300 nm.
Example 3
CH was weighed at room temperature according to a Ag: Cu molar ratio of 1.25:13COOAg and Cu (NO)3)2·3H2Taking 50 ml of pure water, sequentially adding 0.001875mol of silver acetate and 0.0015mol of copper nitrate trihydrate under the condition of magnetic stirring, and then adding 0.05mol of ammonia water and 0.1mol of sodium hydroxide to form a stable and transparent dark blue solution; the obtained reaction solution is subjected to an electrodeposition method, a current of 0.04A is passed through a working electrode, the reaction temperature is controlled at 40 ℃, and the electrifying time is 200 s; and taking out the precipitate after the reaction is finished, and repeatedly washing and drying the precipitate by using pure water and ethanol. FIG. 3 is AgCuO prepared in example 32The field emission scanning electron microscope image of the nano sheet shows AgCuO2The average diameter of the nano-sheets is about 200-500 nm.
AgCuO prepared in examples 1 to 32Compared with nano particles, the method can find that the electrifying time is reduced, and the AgCuO can be effectively reduced2The size of the nanoparticles.
FIG. 5 is an X-ray diffraction pattern of the product prepared in example 3, and it can be found that the product is pure AgCuO2Phase, no other impurities.
Further, AgCuO2Preparation of AgCuO on surface of conductive glass (FTO or ITO) by nano-sheet through electrodeposition technology2The thin film material is used as a hole transport material of the perovskite solar cell. Fig. 8 is a photocurrent-voltage curve of the prepared perovskite solar cell, and it can be found that the efficiency of the cell can reach 13%.
Example 4
CH was weighed at room temperature according to a Ag: Cu molar ratio of 1.5:13COOAg and Cu (NO)3)2·3H2Taking 50 ml of pure water, sequentially adding 0.015mol of silver acetate and 0.0136mol of copper nitrate trihydrate under the condition of magnetic stirring, and then adding 0.5mol of ammonia water and 0.1mol of sodium hydroxide to form a stable and transparent dark blue solution; the obtained reaction solution is subjected to an electrodeposition method, 0.4A current is passed through a working electrode, the reaction temperature is controlled at 70 ℃, and the electrifying time is 30 s; taking out the precipitate after the reaction is finished, repeatedly washing and drying the precipitate by pure water and ethanol to obtain the superfine AgCuO2And (3) nano materials. FIG. 4 is AgCuO prepared in example 42The field emission scanning electron microscope image of the nano sheet shows AgCuO2The average diameter of the nanosheets is about 500-2000 nm.
Comparative example 1
CH was weighed at room temperature according to a Ag: Cu molar ratio of 1.25:13COOAg and Cu (NO)3)2·3H2Taking 50 ml of pure water, sequentially adding 0.001875mol of silver acetate and 0.0015mol of copper nitrate trihydrate under the condition of magnetic stirring, and then adding 0.05mol of ammonia water and 0.1mol of sodium hydroxide to form a stable and transparent dark blue solution; the obtained reaction solution is subjected to an electrodeposition method, a current of 0.04A is passed through a working electrode, the reaction temperature is controlled at 30 ℃, and the electrifying time is 100 s; and taking out the precipitate after the reaction is finished, and repeatedly washing and drying the precipitate by using pure water and ethanol. FIG. 6 is AgCuO prepared in comparative example 12The field emission scanning electron microscope image of the nano material can be seen, from which AgCuO2Shape of materialThe irregular shapes are not uniform in size, and the average diameter is about 100-300 nm.
Comparative example 2
CH was weighed at room temperature according to a Ag: Cu molar ratio of 1.25:13COOAg and Cu (NO)3)2·3H2Taking 50 ml of pure water, sequentially adding 0.001875mol of silver acetate and 0.0015mol of copper nitrate trihydrate under the condition of magnetic stirring, and then adding 0.05mol of ammonia water and 0.1mol of sodium hydroxide to form a stable and transparent dark blue solution; the obtained reaction solution is subjected to an electrodeposition method, a current of 0.04A is passed through a working electrode, the reaction temperature is controlled at 80 ℃, and the electrifying time is 100 s; and taking out the precipitate after the reaction is finished, and repeatedly washing and drying the precipitate by using pure water and ethanol. FIG. 7 is AgCuO prepared in comparative example 22The field emission scanning electron microscope image of the nano sheet shows AgCuO2The nano-material has irregular shapes and uneven sizes, and the average diameter is about 100-300 nm.
Example 5
AgNO was weighed at room temperature according to a Ag to Cu molar ratio of 1.25:13And Cu (NO)3)2·3H2Taking 50 ml of pure water, sequentially adding 0.001875mol of silver nitrate and 0.0015mol of copper nitrate trihydrate under the condition of magnetic stirring, and then adding 0.05mol of ammonia water and 0.1mol of sodium hydroxide to form a stable and transparent dark blue solution; the obtained reaction solution is subjected to an electrodeposition method, 0.04A current is passed through a working electrode, the reaction temperature is controlled at 40 ℃, and the electrifying time is 100 s; taking out the precipitate after the reaction is finished, repeatedly washing and drying the precipitate by pure water and ethanol to obtain the superfine AgCuO2And (3) nano materials.
Example 6
AgNO was weighed at room temperature according to a Ag to Cu molar ratio of 1.25:13And Cu (CH)3COO)2·H2Taking 50 ml of pure water, sequentially adding 0.001875mol of silver nitrate and 0.0015mol of copper acetate monohydrate under the condition of magnetic stirring, and then adding 0.05mol of ammonia water and 0.1mol of sodium hydroxide to form a stable and transparent dark blue solution; the obtained reaction solution is subjected to an electrodeposition method, 0.04A current is passed through a working electrode, the reaction temperature is controlled at 40 ℃, and the electrifying time is 100 s; to be reactedTaking out the precipitate after the reaction is finished, repeatedly washing and drying the precipitate by using pure water and ethanol to obtain the superfine AgCuO2And (3) nano materials.
In the above embodiments, the copper source used may be replaced by Cu (NO) while maintaining the total molar amount of the copper source added3)2Or Cu (CH)3COO)2·H2And O is any one or a mixture of two. Likewise, the alkali source may be replaced with either sodium hydroxide or potassium hydroxide or a combination of both.
Example 7
Compared to example 1, most of them are the same except that in this example: the molar ratio of the silver source to the divalent copper source was 1.5: 1.
Example 8
Compared to example 1, most of them are the same except that in this example: the molar ratio of the silver source to the divalent copper source was 1.1: 1.
Example 9
Compared to example 1, most of them are the same except that in this example: the current applied to the working electrode was 0.1A, and the current application time was 80 seconds.
Example 10
Compared to example 1, most of them are the same except that in this example: the current applied to the working electrode was 0.01A, and the current application time was 300 s.
Example 11
Compared to example 1, most of them are the same except that in this example: the temperature of the electrochemical deposition was 50 ℃.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (3)

1. AgCuO with controllable size2The preparation method of the nano material is characterized by comprising the following steps:
(1) uniformly mixing a silver source and a divalent copper source solution, adding ammonia water, stirring, and adding an alkali source to obtain a stable and transparent mixed solution for later use;
(2) taking the mixed solution obtained in the step (1) as an electrolyte solution, electrifying the working electrode by adopting an electrodeposition method, and depositing to obtain AgCuO2Nanosheet, namely, completing;
the silver source is silver nitrate or silver acetate, and the cupric source is cupric nitrate or cupric acetate;
the molar ratio of the silver source to the divalent copper source is 1.1-1.5: 1;
the alkali source is sodium hydroxide and/or potassium hydroxide, and the addition amount of the alkali source meets the condition that the concentration of hydroxide ions in the mixed solution is 1-10 mol/L;
the addition amount of ammonia water meets the following requirements: the concentration of the compound in the mixed solution is 1-10 mol/L;
the electrifying current of the working electrode is 0.01-0.4A, and the electrifying time is 100-200 s;
the temperature of the electrochemical deposition was 40 ℃.
2. AgCuO with controllable size2Nanomaterial prepared by the method of claim 1, wherein the prepared AgCuO2The nano material is a two-dimensional nano sheet, the minimum transverse dimension of the nano material is 80nm, and the thickness of the nano material is 15-30 nm.
3. The AgCuO with controllable size as claimed in claim 22The application of the nano material as a p-type hole transport material in the preparation of solar cells.
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CN106637332A (en) * 2016-11-22 2017-05-10 浙江大学 Method for preparing cathode material AgCuO2 through anodic oxidation electrodeposition

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Electrodeposition of AgCuO2 Nanoplates;Run Liu;《Journal of the Electrochemical society》;20170125;D130-134页 *

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