CN112456473B - Preparation method of two-phase NiSe 2/carbon nanotube composite - Google Patents
Preparation method of two-phase NiSe 2/carbon nanotube composite Download PDFInfo
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- CN112456473B CN112456473B CN202011519464.5A CN202011519464A CN112456473B CN 112456473 B CN112456473 B CN 112456473B CN 202011519464 A CN202011519464 A CN 202011519464A CN 112456473 B CN112456473 B CN 112456473B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 25
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- 239000010411 electrocatalyst Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000001075 voltammogram Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- -1 carbon nano tube compound Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- 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
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- 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
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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Engineering & Computer Science (AREA)
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- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention discloses a preparation method of a two-phase NiSe 2/carbon nanotube composite, which comprises the steps of precursor preparation, hydrothermal reaction and the like. The prepared compound has excellent electro-catalytic hydrogen evolution performance.
Description
Technical Field
The invention relates to a preparation method of a two-phase NiSe 2/carbon nanotube composite.
Technical Field
Hydrogen is considered an environmentally friendly clean energy source. The product of burning hydrogen is only water, unlike traditional fuels which emit greenhouse gases or polluting gases such as carbon dioxide and sulfur dioxide. Therefore, the hydrogen is more environment-friendly as a new energy source. The electrocatalytic decomposition of water can prepare high-purity hydrogen, and is one of the effective methods for preparing hydrogen at present. Noble metals have been the most active catalysts in this field. However, the cost of precious metals is prohibitively high, and researchers have been continually searching for new non-precious metal electrocatalysts to reduce costs in recent years.
Hydrogen evolution overpotentials for single non-noble metal electrocatalysts tend to be higher, and much research has focused on preparing composites of multiple electrocatalysts to reduce overpotentials. However, the preparation of these complexes is often complicated. Therefore, it is a problem to be solved to develop a simple process for preparing a composite photocatalyst having excellent properties.
Disclosure of Invention
The invention aims to provide a two-phase NiSe 2/carbon nanotube composite with simple process and excellent performance.
The preparation method of the two-phase NiSe 2/carbon nanotube composite comprises the following steps: soaking 500mg of carbon nano tube in a mixed solution of nitric acid and sulfuric acid, wherein the mass specifications of the nitric acid and the sulfuric acid are 70% and 96% respectively, and the volume ratio of the nitric acid to the sulfuric acid is 1: 1; placing the mixed solution in an oil bath at 90 ℃ for 1 hour; after cooling to room temperature, the liquid was filtered off with filter paper; dispersing the carbon nanotubes in the filter paper in deionized water; centrifugally cleaning for 5 times; drying in an oven for 24 hours to obtain a precursor I; 43.4mg of precursor I, 0.1579g of selenium powder and 0.0946g of sodium borohydride are weighed and dissolved in 30mL of dimethylformamide to be continuously stirred for 20 minutes; 0.2377g of nickel nitrate was added; stirring for 20 min; transferring the solution into a 50 ml reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, then centrifugally cleaning for 2 times by using deionized water, and then centrifugally cleaning for 1 time by using ethanol; vacuum drying at 60 deg.C for 12 hr; a two-phase NiSe 2/carbon nanotube composite was obtained.
Compared with the prior art, the sample provided by the invention has the following advantages: the prepared electro-catalyst has excellent performance and simple preparation process.
Drawings
Fig. 1 is XRD patterns of the example sample and the comparative example sample.
Fig. 2 is a linear voltammogram of example and comparative samples.
Detailed Description
The following describes the implementation of the present invention in detail with reference to specific embodiments.
The preparation method of the two-phase NiSe 2/carbon nanotube composite comprises the following steps: soaking 500mg of carbon nano tube in a mixed solution of nitric acid and sulfuric acid, wherein the mass specifications of the nitric acid and the sulfuric acid are 70% and 96% respectively, and the volume ratio of the nitric acid to the sulfuric acid is 1: 1; placing the mixed solution in an oil bath at 90 ℃ for 1 hour; after cooling to room temperature, the liquid was filtered off with filter paper; dispersing the carbon nanotubes in the filter paper in deionized water; centrifugally cleaning for 5 times; drying in an oven for 24 hours to obtain a precursor I; 43.4mg of precursor I, 0.1579g of selenium powder and 0.0946g of sodium borohydride are weighed and dissolved in 30mL of dimethylformamide to be continuously stirred for 20 minutes; 0.2377g of nickel nitrate was added; stirring for 20 min; transferring the solution into a 50 ml reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, centrifugally cleaning with deionized water for 2 times, and centrifugally cleaning with ethanol for 1 time; vacuum drying at 60 deg.C for 12 hr; a two-phase NiSe 2/carbon nanotube composite was obtained.
To illustrate the technical effects of the example samples, comparative example samples were prepared as follows: soaking 500mg of carbon nano tube in a mixed solution of nitric acid and sulfuric acid, wherein the mass specifications of the nitric acid and the sulfuric acid are 70% and 96% respectively, and the volume ratio of the nitric acid to the sulfuric acid is 1: 1; placing the mixed solution in an oil bath at 90 ℃ for 1 hour; after cooling to room temperature, the liquid was filtered off with filter paper; dispersing the carbon nano tubes in the filter paper in deionized water; centrifugally cleaning for 5 times; drying in an oven for 24 hours to obtain a precursor I; 0.1579g of selenium powder and 0.0946g of sodium borohydride are weighed and dissolved in 30mL of dimethylformamide to be continuously stirred for 20 minutes; 0.2377g of nickel nitrate was added; stirring for 20 min; transferring the solution into a 50 ml reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, centrifugally cleaning with deionized water for 2 times, and centrifugally cleaning with ethanol for 1 time; vacuum drying at 60 deg.C for 12 hr; obtaining a precursor II; dispersing all precursors II and 43.4mg precursors I in deionized water, and stirring for 30 minutes by ultrasonic waves to fully mix the precursors; centrifuging for 1 time, and vacuum drying at 60 deg.C for 12 hr; obtaining the single-phase NiSe 2/carbon nano tube compound.
In order to illustrate the technical effects of the present example, the example samples and the comparative example samples were characterized. Fig. 1 is an XRD spectrum of both. Wherein a broad peak around 26 ° corresponds to the carbon nanotube. For the example samples, it can be seen that the diffraction peaks of the samples match the standard data for cubic NiSe2 (PDF # 65-1843, space group Pa-3) and orthorhombic NiSe2 (PDF # 18-0886, space group Pnmn), indicating that the samples are two-phase NiSe 2/carbon nanotube composites. While for the comparative sample, the diffraction peak matches the standard data for cubic NiSe2 (PDF # 65-1843, space group Pa-3), indicating that the sample is a single-phase NiSe 2/carbon nanotube composite.
The samples of examples and comparative examples were tested for their electrocatalytic hydrogen evolution overpotential using a 0.5M sulfuric acid solution as the electrolyte. FIG. 2 is a linear voltammogram of the example sample and the comparative example sample, from which the electrocatalytic hydrogen evolution overpotential (10 mA/cm) of the example sample can be seen2Time) was 143mV, while the electrocatalytic hydrogen evolution overpotential (10 mA/cm) of the comparative example sample2When the voltage is higher than the threshold voltage), the voltage is 156 mV. The result shows that the two-phase NiSe 2/carbon nanotube composite has more excellent electrocatalytic hydrogen evolution performance.
It should be noted that the above description is only a preferred embodiment of the present invention, and the present invention is not limited to the above examples. It is to be understood that other modifications and variations, which may be directly derived or suggested to one skilled in the art without departing from the basic concept of the invention, are to be considered as included within the scope of the invention.
Claims (3)
1. Two-phase NiSe2The preparation method of the carbon nanotube composite is characterized by comprising the following steps: soaking 500mg of carbon nano tube in a mixed solution of nitric acid and sulfuric acid, wherein the mass specifications of the nitric acid and the sulfuric acid are 70% and 96% respectively, and the volume ratio of the nitric acid to the sulfuric acid is 1: 1; placing the mixed solution in an oil bath at 90 ℃ for 1 hour; after cooling to room temperature, the liquid was filtered off with filter paper; dispersing the carbon nano tubes in the filter paper in deionized water; centrifugally cleaning for 5 times; drying in an oven for 24 hours to obtain a precursor I; 43.4mg of precursor I, 0.1579g of selenium powder and 0.0946g of sodium borohydride are weighed and dissolved in 30mL of dimethylformamide to be continuously stirred for 20 minutes; 0.2377g of nickel nitrate was added; stirring for 20 min; transferring the solution into a 50 ml reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, centrifugally cleaning with deionized water for 2 times, and centrifugally cleaning with ethanol for 1 time; vacuum drying at 60 deg.C for 12 hr; two-phase NiSe is obtained2A carbon nanotube composite.
2. The two-phase NiSe prepared by the method of claim 12A carbon nanotube composite.
3. The two-phase NiSe of claim 22The application of the carbon nanotube composite in the field of electrocatalytic hydrogen evolution.
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| CN114774975B (en) * | 2022-05-03 | 2023-06-23 | 台州学院 | Preparation method of two-phase nickel selenide compound |
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| CN106710885A (en) * | 2016-12-16 | 2017-05-24 | 吴中区穹窿山天仲高分子材料技术研究所 | Nickel selenide/carbon nanotube composite nanometer material and preparation and application thereof |
| CN108479813A (en) * | 2018-04-18 | 2018-09-04 | 成都新柯力化工科技有限公司 | A kind of water electrolysis hydrogen production coats the preparation method of seleno catalyst with carbon nanotube |
| CN110548525B (en) * | 2019-09-21 | 2022-02-25 | 台州学院 | Preparation method of carbon nanotube composite nickel-selenium nanosheet electrocatalyst |
| CN111398395B (en) * | 2020-05-22 | 2022-06-24 | 河南工业大学 | Preparation method of dual-signal electrochemical aptamer sensor for vomitoxin detection |
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