CN114752960B - Defective CoS-Co 3 S 4 Preparation method of heterojunction micron sheet - Google Patents
Defective CoS-Co 3 S 4 Preparation method of heterojunction micron sheet Download PDFInfo
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- CN114752960B CN114752960B CN202210487607.1A CN202210487607A CN114752960B CN 114752960 B CN114752960 B CN 114752960B CN 202210487607 A CN202210487607 A CN 202210487607A CN 114752960 B CN114752960 B CN 114752960B
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- 230000002950 deficient Effects 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 230000007547 defect Effects 0.000 claims abstract description 8
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000010335 hydrothermal treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 description 10
- 238000011160 research Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal cobalt sulfide Chemical class 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/30—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
The invention relates to a defect CoS-Co 3 S 4 Preparation method of heterojunction micro-sheet, specifically CoCl 2 ·6H 2 O, KSCN as precursor, hydrothermal synthesis of defective CoS-Co 3 S 4 Heterojunction micro-sheet, defective CoS-Co 3 S 4 The heterojunction microchip can efficiently and electrically catalyze water oxidation.
Description
Technical Field
The invention relates to a defect CoS-Co 3 S 4 A preparation method of heterojunction micro-tablets belongs to the field of material preparation.
Background
The transition metal cobalt sulfide has CoS and CoS 2 、Co 2 S 3 、Co 3 S 4 、Co 9 S 8 And the like, which have unique physicochemical properties. Cobalt sulfide has been a hot spot for research because of its excellent properties in the fields of photocatalysis, electrocatalysis, thermocatalysis, etc. Cobalt sulfide has limited its application in electrocatalytic water oxidation reactions due to the disadvantages of slow surface electron transfer rate, low conductivity, etc. Therefore, the surface structure of cobalt sulfide is regulated and controlled through interface engineering, so that the cobalt sulfide catalyzes water oxidation, and the cobalt sulfide is a hot spot for recent researches.
The controllable synthesis of micro-nano cobalt sulfide and the construction of heterostructures are important methods for modulating the electronic structure of the cobalt sulfide surface. For example: kuila et al synthesized CoS using sodium molybdate, urea, cobalt oxalate x @MoS 2 Heterojunction which catalyzes water to decompose and has better performance than noble metal RuO 2 Pt/C catalyst (Chemerectrochem 2019,6, 430-438). Lin et al constructed CoS/MoS 2 And Co 3 S 4 /MoS 2 /Ni 2 P nano tube, which is applied to catalyzing water hydrogen evolution reaction, finds Co 3 S 4 /MoS 2 /Ni 2 The P nano tube has higher activity, the initial voltage is 60mV, (Journal of Materials Chemistry A,2017,5, 25410-25419). Li et al constructed carbon-coated CoS 2 -FeS 2 Heterojunction nanosheets which exhibit high catalytic activity in catalyzing hydrogen evolution reaction and oxygen evolution reaction, have a voltage of 1.66V at the time of catalyzing water decomposition, and have a current density of 10mA/cm 2 (Dalton Transactions,2020, 49, 13352-13358). At present, the research on constructing heterojunction by cobalt sulfide and other elements is more, and the heterojunction is constructed by single element cobalt sulfideLess research has been carried out and there are few reports on the reactions that catalyze the oxidation of water.
The water oxidation reaction is a half reaction of the electrolytic water reaction, and the overpotential is currently high. Reducing overpotential is a hotspot of current research. Therefore, the cobalt sulfide material is modulated to expose more active sites, so that the cobalt sulfide material has important scientific value for efficiently catalyzing water oxidation.
The invention comprises the following steps:
the present invention aims to provide a defective CoS-Co 3 S 4 A preparation method of heterojunction micro-sheets and application thereof in electrocatalytic water oxidation.
Based on the above object, the technical scheme of the invention is as follows:
1) Defective CoS-Co 3 S 4 Heterojunction microchip: 0.2 to 0.5g of CoCl 2 ·6H 2 O, 0.2-0.4 g KSCN is dissolved in 40-80 mL water, the obtained liquid is treated by hydrothermal treatment for 10-18 h at 230-250 ℃ in a reaction kettle, cooled to room temperature, and the product is centrifuged and dried to obtain the defect CoS-Co 3 S 4 Heterojunction micro-sheets.
2) Defect CoS-Co 3 S 4 The heterojunction microchip is used for catalyzing water oxidation, and the current density is 10mA/cm when the voltage is 1.55V 2 。
The invention has the following advantages:
1) By CoCl 2 ·6H 2 O, KSCN is used as a precursor, and defective CoS-Co is hydrothermally synthesized 3 S 4 Heterojunction micro-sheet effectively expands defect CoS-Co 3 S 4 A preparation method of heterojunction micro-tablets.
2) The invention has the characteristics of simple and efficient method.
Description of the drawings:
FIG. 1 is a defective CoS-Co 3 S 4 XRD characterization results of heterojunction micro-sheets.
Detailed Description
The following examples serve to further illustrate the invention but are not intended to limit it.
Example 1
Defective CoS-Co 3 S 4 The preparation process of the heterojunction micro-sheet is as follows: 0.2g CoCl 2 ·6H 2 O,0.2g KSCN is dissolved in 40mL water, the obtained liquid is subjected to hydrothermal treatment for 10 hours at 230 ℃ in a reaction kettle, cooled to room temperature, and the product is centrifuged and dried to obtain the defect CoS-Co 3 S 4 Heterojunction micro-sheets.
Example 2
0.5g CoCl 2 ·6H 2 O,0.4g of KSCN is dissolved in 80mL of water, the obtained liquid is subjected to hydrothermal treatment in a reaction kettle at 250 ℃ for 18h, cooled to room temperature, and the product is obtained through centrifugation and drying.
Example 3
0.3g CoCl 2 ·6H 2 O,0.3g of KSCN is dissolved in 60mL of water, the obtained liquid is subjected to hydrothermal treatment in a reaction kettle at 240 ℃ for 12h, cooled to room temperature, and the product is obtained through centrifugation and drying.
Example 4
mu.L of the homogeneous slurry of example 1 was applied dropwise to 1X 1cm 2 On the foam nickel electrode, the three-electrode system catalyzes the water oxidation after drying, and when the voltage is 1.55V, the current density is 10mA/cm 2 。
Claims (2)
1. Defective CoS-Co 3 S 4 Preparation method of heterojunction micro-sheet, specifically CoCl 2 ·6H 2 O, KSCN as precursor, hydrothermal synthesis of defective CoS-Co 3 S 4 Heterojunction micro-sheet, defective CoS-Co 3 S 4 The heterojunction micro-sheet can efficiently and electrically catalyze water oxidation; defective CoS-Co 3 S 4 The heterojunction microchip is prepared by the following steps: 0.2 to 0.5g of CoCl 2 ·6H 2 O, 0.2-0.4 g KSCN is dissolved in 40-80 mL water, the obtained liquid is treated by hydrothermal treatment for 10-18 h at 230-250 ℃ in a reaction kettle, cooled to room temperature, and the product is centrifuged and dried to obtain the defect CoS-Co 3 S 4 Heterojunction micro-sheets.
2. A method according to claim 1, characterized in that:
defect CoS-Co 3 S 4 Heterojunction micrometersThe sheet is used for catalyzing water oxidation, and the current density is 10mA/cm when the voltage is 1.55V 2 。
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210487607.1A CN114752960B (en) | 2022-05-06 | 2022-05-06 | Defective CoS-Co 3 S 4 Preparation method of heterojunction micron sheet |
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|---|---|---|---|
| CN202210487607.1A CN114752960B (en) | 2022-05-06 | 2022-05-06 | Defective CoS-Co 3 S 4 Preparation method of heterojunction micron sheet |
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| Publication Number | Publication Date |
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| CN114752960A CN114752960A (en) | 2022-07-15 |
| CN114752960B true CN114752960B (en) | 2023-10-24 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112564A (en) * | 2018-09-11 | 2019-01-01 | 青岛科技大学 | A kind of carbon load pyrite FeS2Application of the nanoparticle in electrocatalytic decomposition water hydrogen manufacturing |
| CN112481633A (en) * | 2020-08-26 | 2021-03-12 | 青岛科技大学 | Carbon-coated CoS2-FeS2Preparation method of heterojunction nanosheet |
| KR20210043930A (en) * | 2019-10-14 | 2021-04-22 | 서울대학교산학협력단 | Method for manufacturing cobalt sulfide with sulfur vacancy defect and cobalt sulfide manufactured thereby |
| CN113060770A (en) * | 2021-02-25 | 2021-07-02 | 南京师范大学 | Preparation method of heterojunction CoO/CoS porous nanorod, obtained material and application |
| CN113832493A (en) * | 2021-09-26 | 2021-12-24 | 青岛科技大学 | Fe with defect sites7S8/FeS2Preparation method of heterojunction nanosheet |
-
2022
- 2022-05-06 CN CN202210487607.1A patent/CN114752960B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112564A (en) * | 2018-09-11 | 2019-01-01 | 青岛科技大学 | A kind of carbon load pyrite FeS2Application of the nanoparticle in electrocatalytic decomposition water hydrogen manufacturing |
| KR20210043930A (en) * | 2019-10-14 | 2021-04-22 | 서울대학교산학협력단 | Method for manufacturing cobalt sulfide with sulfur vacancy defect and cobalt sulfide manufactured thereby |
| CN112481633A (en) * | 2020-08-26 | 2021-03-12 | 青岛科技大学 | Carbon-coated CoS2-FeS2Preparation method of heterojunction nanosheet |
| CN113060770A (en) * | 2021-02-25 | 2021-07-02 | 南京师范大学 | Preparation method of heterojunction CoO/CoS porous nanorod, obtained material and application |
| CN113832493A (en) * | 2021-09-26 | 2021-12-24 | 青岛科技大学 | Fe with defect sites7S8/FeS2Preparation method of heterojunction nanosheet |
Non-Patent Citations (1)
| Title |
|---|
| Hierarchical Co3S4/CoS/MoS2 leaf-like nanoflakes array derived from Co-ZIF-L as an advanced anode for flexible supercapacitor;Fen Qiao等;Journal of Alloys and Compounds;第870卷;159393，第1-11页 * |
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