CN113593918B - Self-assembly preparation method of lamellar cobalt selenide nanosheet array electrode - Google Patents
Self-assembly preparation method of lamellar cobalt selenide nanosheet array electrode Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 47
- QVYIMIJFGKEJDW-UHFFFAOYSA-N cobalt(ii) selenide Chemical compound [Se]=[Co] QVYIMIJFGKEJDW-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000001338 self-assembly Methods 0.000 title claims description 12
- 239000011521 glass Substances 0.000 claims abstract description 126
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000004729 solvothermal method Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 83
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 72
- 239000011669 selenium Substances 0.000 claims description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 26
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 24
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 19
- PMYDPQQPEAYXKD-UHFFFAOYSA-N 3-hydroxy-n-naphthalen-2-ylnaphthalene-2-carboxamide Chemical compound C1=CC=CC2=CC(NC(=O)C3=CC4=CC=CC=C4C=C3O)=CC=C21 PMYDPQQPEAYXKD-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000003760 magnetic stirring Methods 0.000 claims description 16
- 229960001881 sodium selenate Drugs 0.000 claims description 16
- 235000018716 sodium selenate Nutrition 0.000 claims description 16
- 239000011655 sodium selenate Substances 0.000 claims description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 13
- 229940011182 cobalt acetate Drugs 0.000 claims description 10
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 10
- GWTCIAGIKURVBJ-UHFFFAOYSA-L dipotassium;dodecyl phosphate Chemical compound [K+].[K+].CCCCCCCCCCCCOP([O-])([O-])=O GWTCIAGIKURVBJ-UHFFFAOYSA-L 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- LPNYRYFBWFDTMA-UHFFFAOYSA-N potassium tert-butoxide Chemical compound [K+].CC(C)(C)[O-] LPNYRYFBWFDTMA-UHFFFAOYSA-N 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017052 cobalt Inorganic materials 0.000 claims description 8
- 239000010941 cobalt Substances 0.000 claims description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 8
- 238000007603 infrared drying Methods 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 7
- 229910052711 selenium Inorganic materials 0.000 claims description 7
- 229940091258 selenium supplement Drugs 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 125000003916 ethylene diamine group Chemical group 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- 230000006698 induction Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 6
- 239000007772 electrode material Substances 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000003346 selenoethers Chemical class 0.000 description 3
- 238000009827 uniform distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- YBNMDCCMCLUHBL-UHFFFAOYSA-N (2,5-dioxopyrrolidin-1-yl) 4-pyren-1-ylbutanoate Chemical compound C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1CCCC(=O)ON1C(=O)CCC1=O YBNMDCCMCLUHBL-UHFFFAOYSA-N 0.000 description 1
- 229910001370 Se alloy Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses an autonomous assembling preparation method of a sheet-shaped cobalt selenide nanosheet array electrode, which comprises the steps of cleaning FTO glass, and then immersing the FTO glass into a solution for pretreatment to obtain pretreated FTO glass; step 2, forming a seed layer on the pretreated FTO glass; and 3, simultaneously placing the FTO glass obtained in the step 2 in a reaction kettle and immersing the FTO glass in a reaction kettle solution, carrying out solvothermal reaction, cooling and taking out, washing for 3-5 times by using absolute ethyl alcohol, and drying to obtain the lamellar cobalt selenide nanosheet array electrode. The invention can prepare the nanosheet layered Co growing preferentially under the template-free condition by selecting a proper seed layer for induction in an autonomous assembly mode and combining a solvothermal method of a specific process x Se array and forming electrode plates; preparation of Co x The Se nanosheet array solar electrode has preferred growth orientation, and can remarkably improve the performance of the cell.
Description
Technical Field
The invention belongs to the technical field of preparation methods of electrode materials of solar cells, and particularly relates to an automatic assembly preparation method of a sheet-shaped cobalt selenide nanosheet array electrode.
Background
As the VI group element, Se has stronger metallicity, and the metal selenide shows excellent conductive performance; in addition, Se has larger atomic radius and lower ionization energy than S of the same family, so that the metal selenide shows unique catalytic property, and Cu x Se, PbSe and Co x Se and other metal selenides are the most widely researched counter electrode materials at present, cobalt selenide has excellent electrochemical activity, and the light absorption coefficient is as high as 10 5 The band gap is only 1.5-1.7 eV, and a nano structure with a large specific surface area is easy to synthesize, so the nano structure becomes a hot spot concerned for an electrode material.
By regulating and controlling the grain size of the cobalt selenide, a stronger quantum confinement effect can be shown, and the catalytic activity can be further enhanced.
The SILAR method has been reported to be capable of deposition by successive ionic layersCan synthesize Cu on FTO 1.8 A Se counter electrode; a hydrothermal method can also be adopted to prepare a transparent binary Co-Se alloy counter electrode and hollow spherical CoSe; co is also successfully prepared by a solvothermal synthesis method 9 Se 8 a/CoSe counter electrode.
Cobalt selenide is generally classified into CoSe having semiconductor characteristics and Co having metal alloy properties 0.85 Se, non-stoichiometric integer ratio of Co due to overlap of Se 4p and Co 3d spintronic orbitals 0.85 Se has remarkable catalytic property and conductivity; thus, Co 0.85 Se has been widely studied as an electrode material, Co 0.85 The Se electrode is usually prepared by a sol-gel method or a hydrothermal method, and the final form is Co 0.85 Se thin film, but has a problem that the specific surface area is low and the growth cannot be preferred.
Disclosure of Invention
In view of this, the main object of the present invention is to provide an independent assembly method for preparing a lamellar cobalt selenide nanosheet array electrode.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the embodiment of the invention provides an automatic assembly preparation method of a sheet-shaped cobalt selenide nanosheet array electrode, which is implemented according to the following steps:
step 1, cleaning FTO glass, and then immersing the FTO glass into a solution for pretreatment to obtain pretreated FTO glass;
and 3, simultaneously placing the FTO glass obtained in the step 2 in a reaction kettle and immersing the FTO glass in a reaction kettle solution, carrying out solvothermal reaction, cooling and taking out, washing for 3-5 times by using absolute ethyl alcohol, and drying to obtain the lamellar cobalt selenide nanosheet array electrode.
In the above scheme, the step 1 specifically comprises: potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) With potassium tert-butoxide (C) 4 H 9 OK), dissolving in the mixed solution of deionized water and ethanol, and magnetically stirring until the mixed solution is transparentAnd then immersing the cleaned FTO glass into the solution for pretreatment for 30 minutes to obtain the pretreated FTO glass.
In the above scheme, the step 1 is specifically implemented according to the following steps:
step 1.1, preparing a mixed solution of deionized water and ethanol according to a volume ratio of 2-5: 1, and then adding potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) Magnetically stirring for 20-40 minutes to form a uniform solution;
step 1.2 to the solution formed in step 1.1 potassium tert-butoxide (C) was added slowly 4 H 9 OK), stirring, and adjusting the pH value to be 11-12;
step 1.3, ultrasonically cleaning the FTO glass in dilute nitric acid, deionized water and absolute ethyl alcohol respectively, wherein the FTO glass is cleaned for 2-4 times in 20-40 minutes every time, so as to obtain clean FTO glass;
step 1.4, placing the clean FTO glass into the solution obtained in the step 1.2;
and step 1.5, preserving heat for 20-40 minutes at 115-185 ℃, and maintaining magnetic stirring at a rotating speed of 500-600 r/min to obtain the pretreated FTO glass.
In the above scheme, the step 2 specifically comprises: putting the FTO glass pretreated in the step 1 into cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving in citric acid (C) 6 H 8 O 7 ) And slowly hydrolyzing the mixture in deionized water at a low temperature, and then processing the mixture at a high temperature to generate the FTO glass with the seed layer.
In the above scheme, the step 2 is specifically implemented according to the following steps:
step 2.1, under the ice-bath condition, cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving in deionized water to prepare a solution with the molar concentration of Co ions of 0.35-0.65 mol/L; a pH value of
Step 2.2, adding citric acid (C) into the solution of step 2.1 6 H 8 O 7 ) Adjusting the pH value to 4-5;
2.3, placing the FTO glass pretreated in the step 1 in the liquid obtained in the step 2.2, and slowly raising the temperature to 30-50 ℃ at a temperature raising speed of 0.35-0.65 ℃ per minute;
and 2.4, directly taking out the FTO glass obtained in the step 2.3, drying the FTO glass in an infrared drying oven at the temperature of 210-390 ℃ for 40-80 minutes, taking out the FTO glass, and washing the FTO glass with ionized water for 3-5 times to obtain the FTO glass with the seed layer.
In the above scheme, the reaction kettle solution in step 3 is specifically prepared according to the following steps:
step 3.1, weighing cobalt chloride (CoCl) respectively 2 ) Is cobalt source, sodium selenate (Na) 2 SeO 3 ) Is a selenium source, and the molar ratio of Co to Se is 0.55-1.15: 1;
step 3.2 with ethylenediamine (C) 2 H 8 N 2 ) And toluene (C) 8 H 10 ) As a solvent, the volume ratio of ethylenediamine to methylbenzene is 3-5: 1;
and 3.3, dissolving the weighed cobalt chloride and sodium selenate into 140-240 ml of mixed solution of ethylenediamine and methylbenzene, and magnetically stirring for 1-2 hours at the temperature of 20-30 ℃ until a transparent solution, namely a reaction kettle solution, is formed, wherein the rotating speed of the magnetic stirring is 500-600 r/min.
In the above scheme, the step 3 is specifically implemented according to the following steps:
step 3.4, transferring the reaction kettle solution obtained in the step 3.3 into a hydrothermal reaction kettle, and immersing the FTO glass with the seed layer obtained in the step 2 into the reaction kettle solution to be placed at an angle of 30-60 degrees;
step 3.5, sealing the reaction kettle, placing the reaction kettle in a high-temperature oven, heating to 210-310 ℃, and preserving heat for 13-20 hours at the heating rate of 0.5-1.5 ℃ per minute;
step 3.6, cooling the hydrothermal kettle to room temperature, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying in a vacuum drying oven; the temperature is 60-100 ℃ and the time is 0.7-1.4 hours, and Co can be obtained x Se nanosheet array electrode.
In the above scheme, the lining of the hydrothermal reaction kettle is polytetrafluoroethylene.
Compared with the prior art, the method selects a proper seed layer for induction by an autonomous assembly mode and combines the specific seed layerThe solvent thermal method of the process can prepare the nanosheet layered Co growing preferentially under the condition of no template x Se array and forming electrode plates; preparation of Co x The Se nanosheet array solar electrode has preferred growth orientation, and can remarkably improve the performance of the cell.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and do not limit the invention. In the drawings:
FIG. 1 is a Co prepared by the self-assembly preparation method of the lamellar cobalt selenide nanosheet array electrode provided in embodiment 1 of the present invention 0.85 A topography of the Se nanosheet array solar cell electrode;
FIG. 2 is a Co prepared by the self-assembly preparation method of the lamellar cobalt selenide nanosheet array electrode provided in embodiment 2 of the present invention 0.55 A topography of the Se nanosheet array solar cell electrode;
FIG. 3 is a Co self-assembled Co nanosheet array electrode prepared by the method of embodiment 3 of the present invention 1.15 A topography of the Se nanosheet array solar cell electrode;
FIG. 4 is a Co self-assembled Co nanosheet array electrode prepared by the method of embodiment 4 of the present invention 0.65 A topography of a Se nanosheet array solar cell electrode.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in the process, article, or apparatus that comprises the element.
The embodiment of the invention provides an automatic assembly preparation method of a sheet-shaped cobalt selenide nanosheet array electrode, which is implemented according to the following steps:
step 1, cleaning FTO glass, and then immersing the FTO glass into a solution for pretreatment to obtain pretreated FTO glass;
specifically, potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) With potassium tert-butoxide (C) 4 H 9 OK), dissolving in a mixed solution of deionized water and ethanol, magnetically stirring to obtain a transparent solution, and then immersing the cleaned FTO glass in the solution for pretreatment for 30 minutes to obtain the pretreated FTO glass.
specifically, the FTO glass pretreated in the step 1 is put into cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving in citric acid (C) 6 H 8 O 7 ) And slowly hydrolyzing the mixture in deionized water at a low temperature, and then processing the mixture at a high temperature to generate the FTO glass with the seed layer.
And 3, simultaneously placing the FTO glass obtained in the step 2 in a reaction kettle and immersing the FTO glass in a reaction kettle solution, carrying out solvothermal reaction, cooling, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying to obtain the lamellar cobalt selenide nanosheet array electrode.
Further, the step 1 is specifically implemented according to the following steps:
step 1.1, preparing a mixed solution of deionized water and ethanol according to a volume ratio of 2-5: 1, and then adding potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) Magnetically stirring for 20-40 minutes to form a uniform solution;
step 1.2 to the solution formed in step 1.1, potassium tert-butoxide (C) was added slowly 4 H 9 OK), stirring, and adjusting the pH value to be 11-12;
step 1.3, ultrasonically cleaning the FTO glass in dilute nitric acid, deionized water and absolute ethyl alcohol respectively, wherein the FTO glass is cleaned for 2-4 times in 20-40 minutes every time, so as to obtain clean FTO glass;
step 1.4, placing the clean FTO glass into the solution obtained in step 1.2;
and step 1.5, preserving heat for 20-40 minutes at 115-185 ℃, and maintaining magnetic stirring at a rotating speed of 500-600 r/min to obtain the pretreated FTO glass.
The step 2 is specifically implemented according to the following steps:
step 2.1, under the ice-bath condition, cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving the mixture in deionized water to prepare a solution with the molar concentration of Co ions of 0.35-0.65 mol/L;
step 2.2, adding citric acid (C) into the solution of step 2.1 6 H 8 O 7 ) Adjusting the pH value to 4-5;
2.3, placing the FTO glass pretreated in the step 1 into the liquid obtained in the step 2.2, and slowly raising the temperature to 30-50 ℃ at a temperature raising speed of 0.35-0.65 ℃ per minute;
and 2.4, directly taking out the FTO glass obtained in the step 2.3, drying the FTO glass in an infrared drying oven at the temperature of 210-390 ℃ for 40-80 minutes, taking out the FTO glass, and washing the FTO glass with ionized water for 3-5 times to obtain the FTO glass with the seed layer.
The step 3 is specifically implemented according to the following steps:
step 3.1, weighing cobalt chloride (CoCl) respectively 2 ) Is cobalt source, sodium selenate (Na) 2 SeO 3 ) Is a selenium source, and the molar ratio of Co to Se is 0.55-1.15: 1;
step 3.2 with ethylenediamine (C) 2 H 8 N 2 ) And toluene (C) 8 H 10 ) The solvent is ethylene diamine and toluene, and the volume ratio of ethylene diamine to toluene is 3-5: 1;
3.3, dissolving weighed cobalt chloride and sodium selenate into 140-240 ml of mixed solution of ethylenediamine and methylbenzene, and magnetically stirring for 1-2 hours at the temperature of 20-30 ℃ until a transparent solution, namely a reaction kettle solution, is formed, wherein the rotating speed of magnetic stirring is 500-600 r/min;
step 3.4, transferring the reaction kettle solution obtained in the step 3.3 into a hydrothermal reaction kettle, and immersing the FTO glass with the seed layer obtained in the step 2 into the reaction kettle solution to be placed at an angle of 30-60 degrees;
step 3.5, sealing the reaction kettle, placing the reaction kettle in a high-temperature oven, heating to 210-310 ℃, and preserving heat for 13-20 hours at the heating rate of 0.5-1.5 ℃ per minute;
step 3.6, cooling the hydrothermal kettle to room temperature, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying in a vacuum drying oven; the temperature is 60-100 ℃ and the time is 0.7-1.4 hours, thus obtaining Co x Se nanosheet array electrode.
The inner liner of the hydrothermal reaction kettle is made of polytetrafluoroethylene.
Example 1
Example 1 of the present invention provides a lamellar Co 0.85 The self-assembly preparation method of the Se nanosheet array solar cell electrode is implemented according to the following steps:
step 1, preparing a mixed solution of deionized water and ethanol according to a volume ratio of 3:1, and then adding potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) Magnetically stirring for 30 minutes to form a uniform solution;
step 3, ultrasonically cleaning the FTO glass in dilute nitric acid, deionized water and absolute ethyl alcohol respectively, wherein the FTO glass is ultrasonically cleaned for 3 times within 30 minutes each time to obtain clean FTO glass;
step 4, placing the clean FTO glass into the solution obtained in the step 2;
step 5, preserving the heat for 30 minutes at 150 ℃, and maintaining the magnetic stirring at the rotating speed of 550r/min to obtain pretreated FTO glass;
step 6, under the ice-bath condition, cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving in deionized water to prepare a solution with the molar concentration of Co ions being 0.5 mol/L;
step 7, adding citric acid (C) into the solution obtained in step 6 6 H 8 O 7 ) Adjusting the pH value to 4;
step 8, placing the FTO glass pretreated in the step 5 into the liquid obtained in the step 2.2, and slowly raising the temperature to 40 ℃ at a temperature raising speed of 0.5 ℃ per minute;
step 9, directly taking out the FTO glass obtained in the step 8, drying the FTO glass in an infrared drying oven at the temperature of 300 ℃ for 60 minutes, taking out the FTO glass, and washing the FTO glass with ionized water for 4 times to obtain the FTO glass with a seed layer;
step 10, weighing cobalt chloride (CoCl) respectively 2 ) Is cobalt source, sodium selenate (Na) 2 SeO 3 ) Is a selenium source, and the molar ratio of Co to Se is 0.85: 1;
step 11, using ethylenediamine (C) 2 H 8 N 2 ) And toluene (C) 8 H 10 ) Is a solvent, and the volume ratio of ethylenediamine to toluene is 4: 1;
step 12, dissolving weighed cobalt chloride and sodium selenate into 200ml of mixed solution of ethylenediamine and methylbenzene, and magnetically stirring for 1.5 hours at the temperature of 20-30 ℃ until a transparent solution, namely a reaction kettle solution, is formed, wherein the rotating speed of magnetic stirring is 550 r/min;
step 13, transferring the reaction kettle solution obtained in the step 12 into a hydrothermal reaction kettle, and immersing the FTO glass with the seed layer obtained in the step 9 into the reaction kettle solution to be placed at an angle of 45 degrees;
step 14, sealing the reaction kettle, placing the reaction kettle in a high-temperature oven, heating to 260 ℃, and preserving heat for 16 hours, wherein the heating rate is 1 DEG/min;
step 15, cooling the hydrothermal kettle to room temperature, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying in a vacuum drying oven; the temperature is 80 ℃ and the time is 1 hour, thus obtaining Co 0.85 Se nanosheet array electrode.
As shown in FIG. 1, it can be seen that Co prepared by the present invention 0.85 Se electrode with obvious nano-sheet shapeAre clearly and uniformly distributed.
Example 2
Example 2 of the present invention provides a lamellar Co 0.55 The self-assembly preparation method of the Se nanosheet array solar cell electrode is implemented according to the following steps:
step 1, preparing a mixed solution of deionized water and ethanol according to a volume ratio of 2:1, and then adding potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) Magnetically stirring for 20 minutes to form a uniform solution;
step 3, ultrasonically cleaning the FTO glass in dilute nitric acid, deionized water and absolute ethyl alcohol respectively, wherein the FTO glass is ultrasonically cleaned for 2 times for 20 minutes each time to obtain clean FTO glass;
step 4, placing the clean FTO glass into the solution obtained in the step 2;
step 5, preserving the heat for 20 minutes at 115 ℃, and maintaining magnetic stirring at the rotating speed of 500-600 r/min to obtain pretreated FTO glass;
step 6, under the ice-bath condition, cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving in deionized water to prepare a solution with the molar concentration of Co ions being 0.35 mol/L;
step 7, adding citric acid (C) into the solution obtained in step 6 6 H 8 O 7 ) Adjusting the pH value to 4-5;
step 8, placing the FTO glass pretreated in the step 5 into the liquid obtained in the step 2.2, and slowly raising the temperature to 30 ℃ at a temperature raising speed of 0.35 ℃ per minute;
step 9, directly taking out the FTO glass obtained in the step 8, drying the FTO glass in an infrared drying oven at the temperature of 210 ℃ for 40 minutes, taking out the FTO glass, and washing the FTO glass for 3 times by using ionized water to obtain the FTO glass with the seed layer;
step 10, weighing cobalt chloride (CoCl) respectively 2 ) Is cobalt source, sodium selenate (Na) 2 SeO 3 ) As a source of seleniumThe molar ratio of Co to Se is 0.55: 1;
step 11, using ethylenediamine (C) 2 H 8 N 2 ) And toluene (C) 8 H 10 ) Is a solvent, and the volume ratio of ethylenediamine to toluene is 3: 1;
step 12, dissolving weighed cobalt chloride and sodium selenate into 140ml of mixed solution of ethylenediamine and toluene, and magnetically stirring for 1h at the temperature of 20 ℃ until a transparent solution, namely a reaction kettle solution, is formed, wherein the magnetic stirring speed is 500 r/min;
step 13, transferring the reaction kettle solution obtained in the step 12 into a hydrothermal reaction kettle, and immersing the FTO glass with the seed layer obtained in the step 9 into the reaction kettle solution to be placed at an angle of 30 degrees;
step 14, sealing the reaction kettle, placing the reaction kettle in a high-temperature oven, heating to 210 ℃, and keeping the temperature for 13 hours, wherein the heating rate is 0.5 ℃ per minute;
step 15, cooling the hydrothermal kettle to room temperature, taking out, washing with absolute ethyl alcohol for 3 times, and drying in a vacuum drying oven; the temperature is 60 ℃ and the time is 0.7 hour, and then the Co can be obtained 0.55 Se nanosheet array electrode.
As shown in FIG. 2, it can be seen that Co prepared by the present invention 0.55 The Se nanosheet array solar cell electrode has obvious nanosheet shape, clear shape and uniform distribution.
Example 3
Example 3 of the present invention provides a lamellar Co 1.15 The self-assembly preparation method of the Se nanosheet array solar cell electrode is implemented according to the following steps:
step 1, preparing a mixed solution of deionized water and ethanol according to a volume ratio of 5:1, and then adding potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) Magnetically stirring for 40 min to form homogeneous solution;
step 3, ultrasonically cleaning the FTO glass in dilute nitric acid, deionized water and absolute ethyl alcohol respectively for 4 times within 40 minutes each time to obtain clean FTO glass;
step 4, placing the clean FTO glass into the solution obtained in the step 2;
step 5, preserving the heat for 40 minutes at 185 ℃, and maintaining magnetic stirring at the rotating speed of 600r/min to obtain pretreated FTO glass;
step 6, under the ice-bath condition, cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving in deionized water to prepare a solution with the molar concentration of Co ions being 0.65 mol/L;
step 7, adding citric acid (C) into the solution obtained in step 6 6 H 8 O 7 ) Adjusting the pH value to 5;
step 8, placing the FTO glass pretreated in the step 5 into the liquid obtained in the step 2.2, and slowly raising the temperature to 50 ℃ at a temperature raising speed of 0.65 ℃ per minute;
step 9, directly taking out the FTO glass obtained in the step 8, drying the FTO glass in an infrared drying oven at 390 ℃ for 80 minutes, taking out the FTO glass, and washing the FTO glass for 5 times by using ionized water to obtain the FTO glass with a seed layer;
step 10, weighing cobalt chloride (CoCl) respectively 2 ) Is cobalt source, sodium selenate (Na) 2 SeO 3 ) Is a selenium source, and the molar ratio of Co to Se is 1.15: 1;
step 11, using ethylenediamine (C) 2 H 8 N 2 ) And toluene (C) 8 H 10 ) Is a solvent, and the volume ratio of ethylenediamine to toluene is 5: 1;
step 12, dissolving weighed cobalt chloride and sodium selenate into 240ml of mixed solution of ethylenediamine and methylbenzene, and magnetically stirring for 1-2 hours at the temperature of 20-30 ℃ until a transparent solution, namely a reaction kettle solution, is formed, wherein the rotating speed of magnetic stirring is 500-600 r/min;
step 13, transferring the reaction kettle solution obtained in the step 12 into a hydrothermal reaction kettle, and immersing the FTO glass with the seed layer obtained in the step 9 into the reaction kettle solution to be placed at an angle of 60 degrees;
step 14, sealing the reaction kettle, placing the reaction kettle in a high-temperature oven, heating to 310 ℃, and preserving heat for 20 hours at the heating rate of 1.5 ℃ per minute;
step 15, cooling the hydrothermal kettle to room temperature, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying in a vacuum drying oven; the temperature is 100 ℃, the time is 1.4 hours, and Co can be obtained 1.15 Se nanosheet array electrode.
As shown in FIG. 3, it can be seen that Co prepared by the present invention 1.15 The Se nanosheet array solar cell electrode has obvious nanosheet shape, clear shape and uniform distribution.
Example 4
Example 4 of the present invention provides a lamellar Co 0.65 The self-assembly preparation method of the Se nanosheet array solar cell electrode is implemented according to the following steps:
step 1, preparing a mixed solution of deionized water and ethanol according to a volume ratio of 2.5:1, and then adding potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) Magnetically stirring for 25 minutes to form a uniform solution;
step 3, ultrasonically cleaning the FTO glass in dilute nitric acid, deionized water and absolute ethyl alcohol respectively, wherein ultrasonic cleaning is carried out for 25 minutes each time and cleaning is carried out for 3 times, so as to obtain clean FTO glass;
step 4, placing the clean FTO glass into the solution obtained in the step 2;
step 5, preserving the heat for 25 minutes at 140 ℃, and maintaining magnetic stirring at the rotating speed of 500-600 r/min to obtain pretreated FTO glass;
step 6, under the ice-bath condition, cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving in deionized water to prepare a solution with the molar concentration of Co ions of 0.4 mol/L;
step 7, adding citric acid (C) into the solution obtained in step 6 6 H 8 O 7 ) Adjusting the pH value to 4-5;
step 8, placing the FTO glass pretreated in the step 5 into the liquid obtained in the step 2.2, and slowly raising the temperature to 35 ℃ at a temperature raising speed of 0.4 ℃ per minute;
step 9, directly taking out the FTO glass obtained in the step 8, drying the FTO glass in an infrared drying oven at the temperature of 240 ℃ for 50 minutes, taking out the FTO glass, and washing the FTO glass with ionized water for 4 times to obtain the FTO glass with a seed layer;
step 10, weighing cobalt chloride (CoCl) respectively 2 ) Is cobalt source, sodium selenate (Na) 2 SeO 3 ) Is a selenium source, and the molar ratio of Co to Se is 0.65: 1;
step 11, using ethylenediamine (C) 2 H 8 N 2 ) And toluene (C) 8 H 10 ) Is a solvent, and the volume ratio of ethylenediamine to toluene is 3: 1;
step 12, dissolving weighed cobalt chloride and sodium selenate into 160ml of mixed solution of ethylenediamine and toluene, and magnetically stirring for 1.5 hours at 25 ℃ until a transparent solution, namely a reaction kettle solution, is formed, wherein the magnetic stirring speed is 530 r/min;
step 13, transferring the reaction kettle solution obtained in the step 12 into a hydrothermal reaction kettle, and immersing the FTO glass with the seed layer obtained in the step 9 into the reaction kettle solution to be placed at an angle of 40 degrees;
step 14, sealing the reaction kettle, placing the reaction kettle in a high-temperature oven, heating to 240 ℃, and keeping the temperature for 15 hours, wherein the heating rate is 0.8 ℃ per minute;
step 15, cooling the hydrothermal kettle to room temperature, taking out, washing with absolute ethyl alcohol for 3 times, and drying in a vacuum drying oven; the temperature is 75 ℃ and the time is 0.9 hour, and then the Co can be obtained 0.65 Se nanosheet array electrode.
As shown in FIG. 4, it can be seen that Co prepared by the present invention 0.65 The Se nanosheet array solar cell electrode has obvious nanosheet shape, clear shape and uniform distribution.
Example 5
Example 5 of the present invention provides a lamellar Co 1.10 The self-assembly preparation method of the Se nanosheet array solar cell electrode is implemented according to the following steps:
step 1, preparing a mixed solution of deionized water and ethanol according to a volume ratio of 4:1, and then addingInto potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) Magnetically stirring for 35 minutes to form a uniform solution;
step 3, ultrasonically cleaning the FTO glass in dilute nitric acid, deionized water and absolute ethyl alcohol respectively, wherein the FTO glass is cleaned for 3 times after being ultrasonically cleaned for 35 minutes each time, so as to obtain clean FTO glass;
step 4, placing the clean FTO glass into the solution obtained in the step 2;
step 5, preserving the heat for 35 minutes at 160 ℃, and maintaining magnetic stirring at the rotating speed of 580r/min to obtain pretreated FTO glass;
step 6, under the ice-bath condition, cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving in deionized water to prepare a solution with the molar concentration of Co ions being 0.55 mol/L;
step 7, adding citric acid (C) into the solution in the step 6 6 H 8 O 7 ) Adjusting the pH value to 4-5;
step 8, placing the FTO glass pretreated in the step 5 into the liquid obtained in the step 2.2, and slowly raising the temperature to 46 ℃ at a temperature raising speed of 0.55 ℃ per minute;
step 9, directly taking out the FTO glass obtained in the step 8, drying the FTO glass in an infrared drying oven at 350 ℃ for 70 minutes, taking out the FTO glass, and washing the FTO glass with ionized water for 4 times to obtain the FTO glass with a seed layer;
step 10, weighing cobalt chloride (CoCl) respectively 2 ) Is cobalt source, sodium selenate (Na) 2 SeO 3 ) Is a selenium source, and the molar ratio of Co to Se is 1.10: 1;
step 11, using ethylenediamine (C) 2 H 8 N 2 ) And toluene (C) 8 H 10 ) The volume ratio of ethylenediamine to toluene is 4.5: 1;
step 12, dissolving weighed cobalt chloride and sodium selenate into 230ml of mixed solution of ethylenediamine and toluene, and magnetically stirring the mixture for 1 time at the temperature of 25 ℃ until a transparent solution, namely a reaction kettle solution, is formed, wherein the magnetic stirring speed is 580 r/min;
step 13, transferring the reaction kettle solution obtained in the step 12 into a hydrothermal reaction kettle, and immersing the FTO glass with the seed layer obtained in the step 9 into the reaction kettle solution to be placed at an angle of 55 degrees;
step 14, sealing the reaction kettle, placing the reaction kettle in a high-temperature oven, heating to 300 ℃, and preserving heat for 18 hours at the heating rate of 1.2 ℃ per minute;
step 15, cooling the hydrothermal kettle to room temperature, taking out, washing with absolute ethyl alcohol for 5 times, and drying in a vacuum drying oven; the temperature is 90 ℃ and the time is 1.2 hours, and then Co can be obtained 1.10 Se nanosheet array electrode.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (4)
1. An automatic assembly preparation method of a lamellar cobalt selenide nanosheet array electrode is characterized by comprising the following steps:
step 1, cleaning FTO glass, and then immersing the FTO glass into a solution for pretreatment to obtain pretreated FTO glass;
the step 1 is specifically implemented according to the following steps:
step 1.1, preparing a mixed solution of deionized water and ethanol according to a volume ratio of 2-5: 1, and then adding potassium monododecyl phosphate (C) 12 H 25 OPO 3 K 2 ) Magnetically stirring for 20-40 minutes to form a uniform solution;
step 1.2 to the solution formed in step 1.1, potassium tert-butoxide (C) was added slowly 4 H 9 OK), stirring, and adjusting the pH value to be 11-12;
step 1.3, ultrasonically cleaning the FTO glass in dilute nitric acid, deionized water and absolute ethyl alcohol respectively, wherein the FTO glass is cleaned for 2-4 times in 20-40 minutes every time, so as to obtain clean FTO glass;
step 1.4, placing the clean FTO glass into the solution obtained in step 1.2;
step 1.5, preserving heat for 20-40 minutes at 115-185 ℃, and maintaining magnetic stirring at a rotating speed of 500-600 r/min to obtain pretreated FTO glass;
step 2, forming a seed layer on the pretreated FTO glass;
the step 2 is specifically implemented according to the following steps:
step 2.1, under the ice-bath condition, cobalt acetate (C) 4 H 6 CoO 4 ) Dissolving in deionized water to prepare a solution with the molar concentration of Co ions of 0.35-0.65 mol/L;
step 2.2, adding citric acid (C) into the solution of step 2.1 6 H 8 O 7 ) Adjusting the pH value to 4-5;
2.3, placing the FTO glass pretreated in the step 1 into the liquid obtained in the step 2.2, and slowly raising the temperature to 30-50 ℃ at a temperature raising speed of 0.35-0.65 ℃ per minute;
step 2.4, directly taking out the FTO glass obtained in the step 2.3, drying the FTO glass in an infrared drying oven at the temperature of 210-390 ℃ for 40-80 minutes, taking out the FTO glass, and washing the FTO glass for 3-5 times by using ionized water to obtain the FTO glass with a seed layer;
and 3, simultaneously placing the FTO glass obtained in the step 2 in a reaction kettle and immersing the FTO glass in a reaction kettle solution, carrying out solvothermal reaction, cooling and taking out, washing for 3-5 times by using absolute ethyl alcohol, and drying to obtain the lamellar cobalt selenide nanosheet array electrode.
2. The self-assembly preparation method of the lamellar cobalt selenide nanosheet array electrode according to claim 1, wherein the reaction kettle solution in step 3 is specifically prepared according to the following steps:
step 3.1, weighing cobalt chloride (CoCl) respectively 2 ) Is cobalt source, sodium selenate (Na) 2 SeO 3 ) Is a selenium source, and the molar ratio of Co to Se is 0.55-1.15: 1;
step 3.2 with ethylenediamine (C) 2 H 8 N 2 ) And toluene (C) 8 H 10 ) The solvent is ethylene diamine and toluene, and the volume ratio of ethylene diamine to toluene is 3-5: 1;
and 3.3, dissolving the weighed cobalt chloride and sodium selenate into 140-240 ml of mixed solution of ethylenediamine and methylbenzene, and magnetically stirring for 1-2 hours at the temperature of 20-30 ℃ until a transparent solution, namely a reaction kettle solution is formed, wherein the rotating speed of the magnetic stirring is 500-600 r/min.
3. The self-assembly preparation method of the lamellar cobalt selenide nanosheet array electrode as claimed in claim 2, wherein the step 3 is specifically implemented according to the following steps:
step 3.4, transferring the reaction kettle solution obtained in the step 3.3 into a hydrothermal reaction kettle, and immersing the FTO glass with the seed layer obtained in the step 2 into the reaction kettle solution to be placed at an angle of 30-60 degrees;
step 3.5, sealing the reaction kettle, placing the reaction kettle in a high-temperature oven, heating to 210-310 ℃, and preserving heat for 13-20 hours at the heating rate of 0.5-1.5 ℃ per minute;
step 3.6, cooling the hydrothermal kettle to room temperature, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying in a vacuum drying oven; the temperature is 60-100 ℃ and the time is 0.7-1.4 hours, and Co can be obtained x Se nanosheet array electrode.
4. The self-assembly preparation method of the lamellar cobalt selenide nanosheet array electrode according to claim 3, wherein the lining of the hydrothermal reaction kettle is polytetrafluoroethylene.
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