CN112853423A - Cuprous oxide film with high photoelectrochemical property and preparation method thereof - Google Patents

Cuprous oxide film with high photoelectrochemical property and preparation method thereof Download PDF

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CN112853423A
CN112853423A CN202110025207.4A CN202110025207A CN112853423A CN 112853423 A CN112853423 A CN 112853423A CN 202110025207 A CN202110025207 A CN 202110025207A CN 112853423 A CN112853423 A CN 112853423A
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cuprous oxide
oxide film
solution
electrode
film
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王龙成
吴光杰
张永飞
喻志奎
康硕
金达莱
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Zhejiang University of Technology ZJUT
Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment

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Abstract

The invention discloses a cuprous oxide film with high photoelectrochemical property and a preparation method thereof. Selecting soluble copper salt, lactate solution and sodium hydroxide solution as raw materials to prepare deposition solution; performing thin film deposition on the conductive glass by using a three-electrode electrochemical cell; inserting the three electrodes into the deposition solution, and keeping the temperature at 50-70 ℃ for 30 minutes; adjusting the pH range to 9.0-12.0, and controlling the deposition time to 20-60 minutes; cleaning and drying the obtained film; then, the film is decarburized for 1 hour under the ventilation condition of 120-150 ℃, and then the film is annealed and sintered for 2 hours at 250-400 ℃. The cuprous oxide film prepared by the method is uniform, compact and crack-free, and has high photoelectrochemical properties.

Description

Cuprous oxide film with high photoelectrochemical property and preparation method thereof
Technical Field
The invention belongs to the field of photoelectric functional materials, and particularly relates to a cuprous oxide film with high photoelectrochemical properties and a preparation method thereof.
Background
In the face of gradual depletion of petrochemical energy and gradual deterioration of human ecosystem, the global energy consumption structure needs to be changed, and the traditional energy is gradually changed to renewable energy. The cost reduction and the photoelectric conversion efficiency improvement are two major problems of the solar cell, and the search for a novel solar cell material which is cheap, has good stability and good photovoltaic characteristics is an effective method for developing the low-cost solar cell. [ Von pilatory et a1. solar power technology and application, 6(2009): 173-.
Cu2O is a direct forbidden band semiconductor material with excellent performance and visible light response, has potential application value in the photoelectric field, has the characteristics of rich raw materials, low cost, no toxicity, no pollution, high theoretical photoelectric conversion efficiency and the like, and has good practical application value in a novel light absorption layer of a thin-film solar cell. In recent years, the photoelectrochemical Properties (PEC) of semiconductor materials have become a research hotspot, and how to improve the photoelectrochemical properties of semiconductor materials has become a research target of a plurality of researchers. (Yandriren. solar cell material, 2(2006):110-]。
The cuprous oxide film has wide application, and is particularly indispensable in semiconductor optoelectronic devices. The difference of the preparation process and the setting parameters has important influence on the structure and the performance of the prepared film material. At present, in order to improve and regulate the performance of the cuprous oxide film, various Cu films are researched and developed2The preparation method of the 0 film comprises a sol-gel method, chemical vapor deposition, a magnetron sputtering method, a thermal oxidation method, an anodic oxidation method, a vacuum evaporation method and a pulse laser deposition method. The film prepared by the prior art has poor uniformity and high cost.
Disclosure of Invention
In order to solve the problems in the background technology, the invention provides a cuprous oxide film with high photoelectrochemical performance and a preparation method thereof. And heating at a ventilation position to perform decarburizing treatment on the film, and then annealing at high temperature to obtain the cuprous oxide film.
The technical scheme adopted by the invention is as follows:
cuprous oxide film with high photoelectrochemical property
The cuprous oxide film is a layer of film deposited on the conductive surface of the conductive glass substrate and has the chemical formula of Cu2O。
The carrier concentration of the cuprous oxide film is as high as 2.34 multiplied by 1018cm-3And has high photoelectrochemical performance.
Preparation method of cuprous oxide film with high photoelectrochemical property
The method comprises the following steps:
step 1) dissolving soluble copper salt in deionized water, and stirring to prepare a copper salt solution; dissolving soluble lactate in deionized water, and stirring to prepare a lactate solution;
step 2) putting the copper salt solution and the lactate solution obtained in the step 1) into a constant-temperature water bath, mixing and stirring, controlling the temperature of the solution at 50-70 ℃, and dropwise adding 2mol/L sodium hydroxide solution into the mixed solution to adjust the pH value, thereby preparing an electrodeposition solution;
step 3) performing thin film deposition on the conductive glass substrate by using a three-electrode electrochemical cell consisting of a working electrode, a counter electrode and a reference electrode: inserting a three-electrode consisting of a working electrode, a counter electrode and a reference electrode into the electrodeposition solution in the step 2), keeping the temperature for 30 minutes, and depositing on conductive glass to obtain a cuprous oxide film; the working electrode is conductive glass;
step 4), washing the film deposited on the conductive glass by using deionized water, and drying;
step 5) performing carbon removal treatment on the dried film for 1 hour under a ventilation condition; the carbon removal treatment is to remove carbon elements of the film under the ventilation condition;
step 6) heat treatment: annealing and sintering the film for 2 hours at the temperature of 250-400 ℃.
The soluble copper salt in the step 1) is anhydrous copper sulfate or copper sulfate pentahydrate, and the soluble lactate is sodium lactate or lactic acid solution.
The molar concentration of the copper salt solution in the step 1) is 0.1-0.4 mol/L, and the molar concentration of the lactate solution is 1.0-2.0 mol/L.
In the step 2), the volume ratio of the copper salt solution to the lactate solution is 1: 3.
In the step 2), the pH is adjusted to 9.0-12.0.
In the three-electrode electrochemical cell in the step 3), the working electrode is conductive glass, the counter electrode is a platinum electrode, a gold electrode or a graphite electrode, and the reference electrode is an Ag/AgCl/saturated KCl solution reference electrode.
In the step 3), the voltage between the working electrode and the reference electrode is adjusted to be-0.85V-1.4V, and the deposition time is controlled to be 20 minutes-60 minutes.
In the step 5), the temperature of the carbon removal treatment is controlled between 120 ℃ and 150 ℃.
For Cu of the invention2And (3) carrying out heat treatment at different temperatures on the thin film, so that the crystallinity of the cuprous oxide thin film is optimized through the heat treatment, the defects of the cuprous oxide thin film are reduced, and the photoelectric property of the cuprous oxide solar cell is improved.
Control of Cu in solution by adjusting pH of deposition solution+/O2-Because the oxygen atom densities of different crystal faces of cuprous oxide are different, the preferential growth of the cuprous oxide film is changed from (100) crystal face to (111) crystal face, and the shape of the film sequentially shows the change of a four-sided pyramid, a three-sided prism and a three-sided pyramid. The increase of the pH value increases the number of free particles in the electrolyte solution, improves the conductivity of the solution, reduces concentration polarization and obtains better crystallization performance of particles.
The invention has the beneficial effects that:
the cuprous oxide film is prepared by adopting constant-potential cathode electrochemical deposition, and is obtained by ventilation heating, carbon removal and high-temperature annealing calcination, and the film material is uniform, compact, free of cracking and high in purity; through the adjustment of reaction parameters, the cuprous oxide film can be uniformly grown on the substrate material, so that the reaction materials can be reduced, the subsequent coating process is omitted, and the production cost is greatly reduced. In addition, the electrochemical deposition method has the advantages of uniform film formation, controllable deposition thickness, simple equipment and operation, mild reaction conditions and small environmental pollution, and is a brand-new, clean, mild and environment-friendly method.
The invention has higher photoelectrochemical property; cu deposition at different pH values 20 film and Cu before and after Heat treatment2The 0 film can rapidly generate cathode photocurrent under the condition of illumination, and has good photoelectric conversion characteristics. Along with the increase of the pH value and the increase of the heat treatment temperature, the crystal growth driving force is increased, the defects are reduced, the crystal form is more complete, the recombination of photon-generated carriers is reduced, the transmission of the photon-generated carriers is facilitated, and the Cu is improved20 thin film photocurrent.
Drawings
FIG. 1 is a schematic diagram of a structure of a cuprous oxide film deposited on a conductive glass substrate: 1. and (3) depositing a cuprous oxide film, 2, and a conductive glass substrate.
FIG. 2 is an XRD spectrum of the cuprous oxide film of example 1, (a) XRD spectra of cuprous oxide films prepared at different annealing temperature values; (b) is an XRD spectrogram of the cuprous oxide film prepared under the condition of different pH values.
FIG. 3 is a spectrum of cuprous oxide film of example 1.
FIG. 4 is an electron micrograph of a cuprous oxide film of example 1.
FIG. 5(a) Cu prepared at different annealing temperatures2The Mott-Schottky curve of the 0 film, FIG. 5(b), is a plot of annealing temperature versus carrier concentration and flat band potential.
FIG. 6(a) Cu prepared at different pH values2The Mott-Schottky curve for the 0 film, FIG. 6(b), is a plot of pH as a function of carrier concentration and flat band potential.
Fig. 7 is a graph of the transient photocurrent intensity of the cuprous oxide film in example 1 as a function of annealing temperature.
Detailed Description
As shown in FIG. 1, the present invention is applied to a conductive glass substrate 2One side is deposited with a cuprous oxide film 1. The chemical formula of the cuprous oxide film is Cu2And O, the flat band potential of the film material moves to the positive direction along with the increase of PH and annealing temperature, and the film material has higher photoelectrochemical property.
Example 1:
a cuprous oxide film with high photoelectrochemical property is prepared by dissolving 25g of blue copperas pentahydrate in 250mL of deionized water, and stirring to prepare a copper sulfate solution with the molar concentration of 0.4 mol/L. 50mL of sodium lactate is dissolved in 250mL of deionized water and stirred to prepare a sodium lactate solution with the molar concentration of 1.4 mol/L. 10mL of copper sulfate and 10mL of sodium lactate solution are mixed and stirred, 1mol/L of sodium hydroxide solution is dripped into the mixture to adjust the pH value to 10, and the temperature of the solution is controlled at 60 ℃ by constant temperature water bath. And depositing the cuprous oxide film by using a three-electrode electrochemical cell. The working electrode is conductive glass. The counter electrode is a high-purity platinum electrode. The reference electrode is an Ag/AgCl/KCl saturated solution electrode. The three electrodes were inserted into the prepared electrodeposition solution and the temperature was maintained for 30 minutes. The voltage between the working electrode and the reference electrode is adjusted to-1.2V, and the deposition time is controlled to 30 minutes. And washing the deposited film with deionized water, and drying. The film was then decarburized by heating to 120 ℃ in a vent for 1 hour, and then annealed and sintered at 250 ℃, 300 ℃, 350 ℃, 400 ℃ for 2 hours.
As can be seen from fig. 2(a), the heat treatment increases the activation energy of the particles inside or on the surface of the crystal, increases the diffusion driving force, improves the crystallization performance of the crystal, and reduces the recombination of photo-generated electron-hole pairs, thereby increasing the carrier concentration. The sample tends to grow (111), the positions of diffraction peaks of XRD patterns of the samples with different annealing temperatures are not changed, only the intensity of the diffraction peaks is changed, and the samples with different annealing temperatures have only the change of crystallinity and no change of phase, and are Cu2O。
As can be seen from FIG. 2(b), the pH value has a great influence on the crystallinity of cuprous oxide, and when the pH value of the deposition solution is low, Cu 20 the intensity of the diffraction peak of the film is lower, indicating that Cu2The 0 film is relatively poor in quality and small in crystallinity. When depositing p of the solutionWhen H value increases, Cu2The diffraction peak of the 0 film is obviously enhanced, which shows that Cu2The crystallization properties and quality of the 0 film increase with increasing pH. Meanwhile, the pH value of the solution also has certain influence on the crystal orientation of the film, the (111) crystal face of the cuprous oxide film preferentially grows along with the increase of the pH value, and the diffraction peak intensity of the (111) crystal face is gradually enhanced along with the increase of the pH value.
Fig. 3 is an EDS spectrum of a cuprous oxide film showing the presence of two elements, oxygen and copper, primarily. The atomic number ratio of copper to oxygen is about 2: 1, the obtained film is a cuprous oxide film.
Fig. 4 is a low power electron micrograph of a cuprous oxide film. From the three photographs of FIG. 4(a), (b) and (c), it can be seen that the film particles are uniform, and the film material is uniform and dense without cracks.
Fig. 5 is a graph of the effect of annealing temperature on cuprous oxide films. Calculating the carrier concentration and the flat band potential of the cuprous oxide film according to the slope and intercept of the Mott-Schottky curve of FIG. 5(a), thereby obtaining the relation chart of FIG. 5 (b); as can be seen from FIG. 5(b), Cu is present as the heat treatment temperature is increased20 film has an increased carrier concentration of 6.5X 1017cm-3Increased to 2.34 × 1018cm-3The flat band potential increases from 0.183V to 0.255V as the carrier concentration increases moving in the forward direction. When not heat-treated, Cu2The organic matter generated during deposition and not removed in the 0 thin film affects the electron transfer and reduces the carrier concentration. With the increase of the heat treatment temperature, the organic substances pass through CO or CO2The film is discharged in a mode of reducing carrier transmission resistance, in addition, the activity of crystal particles is improved through heat treatment, the diffusion driving force is improved, the crystallization performance of crystals is improved, and the recombination center of carriers is reduced, so that the carrier concentration is improved. The heat treatment improves the discharge of crystal organic matter and the crystallization performance of the crystal, and improves the carrier concentration.
Fig. 6 is a graph of the effect of pH on cuprous oxide films. Calculating the carrier concentration and the flat band potential of the cuprous oxide film according to the slope and intercept of the Mott-Schottky curve of FIG. 6(a), thereby obtaining the relation chart of FIG. 6 (b); as can be seen from fig. 6(b), as the pH value increases,Cu2the carrier concentration of 0 thin film is increased from 3.71X 1017cm-3Increased to 1.18 × 1018cm-3I.e. the flat band potential changes positively. As can be seen from the graph, the flat band potentials were 0.163V,0.183V,0.184V,0.194V and 0.25V, respectively, in accordance with the change in the carrier concentration as the pH value was increased.
As can be seen from FIG. 7, the product obtained in this example is excellent in photoelectrochemical properties, Cu2The 0 film can rapidly generate cathode photocurrent under the condition of illumination, and has good photoelectric conversion characteristics; with the increase of annealing temperature, the defects of the electrochemical performance of the crystal with improved crystallization performance are reduced, the recombination of photon-generated carriers is reduced, the carrier concentration is increased, and Cu is caused2The photocurrent of the 0 film increased.
Example 2:
a cuprous oxide film with high photoelectrochemical property is prepared by dissolving 25g of blue copperas pentahydrate in 250mL of deionized water, and stirring to prepare a copper sulfate solution with the molar concentration of 0.4 mol/L. 50mL of sodium lactate is dissolved in 250mL of deionized water and stirred to prepare a sodium lactate solution with the molar concentration of 1.4 mol/L. 10mL of copper sulfate and 10mL of sodium lactate solution are mixed and stirred, 1mol/L of sodium hydroxide solution is added dropwise to adjust the pH value to 12.0, and the temperature of the solution is controlled at 60 ℃ by a thermostatic water bath. And depositing the cuprous oxide film by using a three-electrode electrochemical cell. The working electrode is conductive glass. The counter electrode is a high-purity platinum electrode. The reference electrode is an Ag/AgCl/KCl saturated solution electrode. The three electrodes were inserted into the prepared electrodeposition solution and the temperature was maintained for 30 minutes. The voltage between the working electrode and the reference electrode is adjusted to-0.8V, and the deposition time is controlled to be 60 minutes. And washing the deposited film with deionized water, and drying. The film was then decarburized by heating to 120 ℃ in a vent for 1 hour, and then annealed and sintered at 250 ℃, 300 ℃, 350 ℃, 400 ℃ for 2 hours. The specific test results of the prepared europium-doped yttrium oxide film are similar to the test results of example 1.
Example 3:
a cuprous oxide film with high photoelectrochemical property is prepared by dissolving 7.5g of blue vitriod in 250mL of deionized water, stirring to prepare a blue vitriod solution with the molar concentration of 0.2 mol/L. 25mL of sodium lactate is dissolved in 250mL of deionized water and stirred to prepare a sodium lactate solution with the molar concentration of 0.7 mol/L. 10mL of copper sulfate and 10mL of sodium lactate solution are mixed and stirred, 1mol/L of sodium hydroxide solution is added dropwise to adjust the pH value to 12.0, and the temperature of the solution is controlled at 70 ℃ by a thermostatic water bath. And depositing the cuprous oxide film by using a three-electrode electrochemical cell. The working electrode is conductive glass. The counter electrode is a high-purity platinum electrode. The reference electrode is an Ag/AgCl/KCl saturated solution electrode. The three electrodes were inserted into the prepared electrodeposition solution and the temperature was maintained for 60 minutes. The voltage between the working electrode and the reference electrode is adjusted to-0.4V, and the deposition time is controlled to 30 minutes. And washing the deposited film with deionized water, and drying. The film was then decarburized by heating to 120 ℃ in a vent for 1 hour, and then annealed and sintered at 250 ℃, 300 ℃, 350 ℃, 400 ℃ for 2 hours. The specific test results of the prepared europium-doped yttrium oxide film are similar to the test results of example 1.

Claims (10)

1. A cuprous oxide film with high photoelectrochemical property is characterized in that: the cuprous oxide film is a layer of film deposited on the conductive surface of the conductive glass substrate and has the chemical formula of Cu2O。
2. The method for preparing cuprous oxide film with high photoelectrochemical property according to claim 1, wherein said cuprous oxide film has carrier concentration up to 2.34 x 1018cm-3。
3. The preparation method of the cuprous oxide film with high photoelectrochemical property, which is disclosed by any one of claims 1-2, is characterized by comprising the following steps:
step 1) dissolving soluble copper salt in deionized water, and stirring to prepare a copper salt solution; dissolving soluble lactate in deionized water, and stirring to prepare a lactate solution;
step 2) putting the copper salt solution and the lactate solution obtained in the step 1) into a constant-temperature water bath, mixing and stirring, controlling the temperature of the solution at 50-70 ℃, and dropwise adding 2mol/L sodium hydroxide solution into the mixed solution to adjust the pH value, thereby preparing an electrodeposition solution;
step 3) performing thin film deposition on the conductive glass substrate by using a three-electrode electrochemical cell consisting of a working electrode, a counter electrode and a reference electrode: inserting a three-electrode consisting of a working electrode, a counter electrode and a reference electrode into the electrodeposition solution in the step 2), keeping the temperature for 30 minutes, and depositing on conductive glass to obtain a cuprous oxide film; the working electrode is conductive glass;
step 4), washing the film deposited on the conductive glass by using deionized water, and drying;
step 5) performing carbon removal treatment on the dried film for 1 hour under a ventilation condition;
step 6) heat treatment: annealing and sintering the film for 2 hours at the temperature of 250-400 ℃.
4. The method for preparing cuprous oxide film with high photoelectrochemical properties according to claim 3, wherein said soluble copper salt in step 1) is anhydrous cupric sulfate or cupric sulfate pentahydrate, and said soluble lactate is sodium lactate or lactic acid solution.
5. The method for preparing a cuprous oxide film with high photoelectrochemical properties according to claim 3, wherein the molar concentration of the copper salt solution in step 1) is 0.1-0.4 mol/L, and the molar concentration of the lactate solution is 1.0-2.0 mol/L.
6. The method for preparing a cuprous oxide film with high photoelectrochemical properties according to claim 3, wherein in step 2), the volume ratio of the copper salt solution to the lactate solution is 1: 3.
7. A method for preparing cuprous oxide film with high photoelectrochemical properties according to claim 3, wherein in step 2), pH is adjusted to 9.0-12.0.
8. The preparation method of the cuprous oxide film with high photoelectrochemical property according to claim 3, wherein the cuprous oxide film comprises the following steps: in the three-electrode electrochemical cell in the step 3), the working electrode is conductive glass, the counter electrode is a platinum electrode, a gold electrode or a graphite electrode, and the reference electrode is an Ag/AgCl/saturated KCl solution reference electrode.
9. The method for preparing a cuprous oxide film with high photoelectrochemical properties according to claim 3, wherein in step 3), the voltage between the working electrode and the reference electrode is adjusted to be-0.85V-1.4V, and the deposition time is controlled to be 20 minutes-60 minutes.
10. The method for preparing a cuprous oxide film with high photoelectrochemical properties according to claim 3, wherein in step 5), the temperature of decarbonization treatment is controlled to be 120-150 ℃.
CN202110025207.4A 2021-01-08 2021-01-08 Cuprous oxide film with high photoelectrochemical property and preparation method thereof Pending CN112853423A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102321901A (en) * 2011-09-21 2012-01-18 浙江理工大学 Heat treatment method for increasing n-type cuprous oxide film carrier concentration
CN104152964A (en) * 2014-08-12 2014-11-19 浙江大学 Method for manufacturing sodium yttrium fluoride-4 and cuprous oxide composite solar thin film

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102321901A (en) * 2011-09-21 2012-01-18 浙江理工大学 Heat treatment method for increasing n-type cuprous oxide film carrier concentration
CN104152964A (en) * 2014-08-12 2014-11-19 浙江大学 Method for manufacturing sodium yttrium fluoride-4 and cuprous oxide composite solar thin film

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Application publication date: 20210528