CN108439549A - A kind of preparation of array structure transition metal selenides electrode and its application in electrolysis water - Google Patents
A kind of preparation of array structure transition metal selenides electrode and its application in electrolysis water Download PDFInfo
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- CN108439549A CN108439549A CN201810297329.7A CN201810297329A CN108439549A CN 108439549 A CN108439549 A CN 108439549A CN 201810297329 A CN201810297329 A CN 201810297329A CN 108439549 A CN108439549 A CN 108439549A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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Abstract
A kind of preparation of array structure transition metal selenides electrode and its application in electrolysis water belong to electrode technology field.The first step optimizes nickel sheet (NF) substrate by simply pre-processing, second step is in nickel sheet substrate surface original position homoepitaxial metal-organic framework materials (Mn/Fe/Co/Ni/Cu MOF) nano-array, obtain NF MOFs materials, NF M are finally made in MOFs nano-array surface in situ selenizings in third stepxSeyNano-array electrode material.NF‑MxSeyAs electrolytic water electric it is great have lower starting point, larger current density, excellent electrocatalytic decomposition it is aqueous can and higher stability, can be applicable to the new energy such as electrolysis water storage and conversion equipment.
Description
Technical field
The invention belongs to convert new energy to be stored in conversion art electro-catalysis development technique field.It is organic that technology is related to metal
Framework material (MOFs) is constructed and its prepares array structure transition metal selenides (NF-M for template selenizing derivativexSey) electrode.
Background technology
It is continuously increased with the rapid development of industrial production with population, using coal, oil, natural gas as the change of main representative
Stone fuel is largely consumed in recent decades, while causing inevitable environmental pollution and energy shortage.Therefore, it finds a kind of
Clean regenerative resource increasingly becomes current era growth requirement.In numerous materials, hydrogen as it is a kind of it is environmentally protective,
Efficiently, the clean energy resource rich in energy is the substitute of the following potential fossil energy.Reproducible feature can solve very well
Certainly energy crisis and environmental crisis two large problems.Except that clean energy resource can be used as to use, hydrogen also has in industries such as oil, chemical industry
Important application, such as hydrogen is as raw and semifinished materials industries and ammonification.Currently, hydrogen preparation method has developed many kinds, electrolysis water with
Numerous methods are compared with the advantages such as at low cost, high yield, high-purity, pollution-free；Meanwhile the oxygen that anode generates can also be made
The fields such as medicine are applied to for good resource, there is huge source benefit and economic benefit, therefore, water electrolysis hydrogen production method very may be used
The core methed of the following industries can be become.Electrolysis water includes two half-cell reactions, and respectively cathode hydrogen evolution reacts
(HyDrogen Evolution Reaction, HER) and Oxygen anodic evolution reaction (OxyGen Evolution Reaction,
OER).Since OER kineticses are more sluggish, carried out to accelerate reaction, catalyst is often introduced into this half-cell
In reaction, during the reaction, energy expenditure and hydrogen generation efficiency and catalyst material are closely related, so studying and developing one
The new and effective electrolysis water catalyst of kind is significant for electrolysis water conversion new energy process.
Metal-organic framework materials (Metal-organic frameworks, MOFs) system is by metal ion and organic ligand
The holey inorganic-organic hybridization functional material to be formed is acted on by coordinate bond.Compared to traditional material, MOFs has hole
Rate height, large specific surface area, pore structure are controllable, the advantages that being readily synthesized.In recent years, MOFs in gas absorption, molecular recognition, urge
The various fields such as change, separation are widely applied and are paid close attention to.Wherein, porous MOFs and its derivative show in electro-catalysis field
Go out preferable performance, is especially studied extensively in the reaction of electrocatalytic decomposition water, there is potential using value.This mainly by
In MOFs compared to traditional material, various structures in the synthesis process, adjustability is strong, it can be achieved that targeting synthesis, and building-up process
It is simpler.Nevertheless, there are still some problems in terms of synthesis by MOFs, if powder is easily reunited, active site cannot be abundant
Exposure etc., this is unfavorable for mass transfer and electron transmission, inhibits its development and application.Therefore, a kind of new method is studied and develops,
Preparation structure composition is various, loose porous, large specific surface area, active site is abundant, adjustability is high, has excellent in performance functional group
MOFs and its derivative be used for electrochemical decomposition water, can effectively improve electrochemical source of current density and electrochemical decomposition water effect
Rate.
Invention content
The object of the present invention is to provide a kind of preparation methods of array structure transition metal selenides electrode.
A kind of array structure transition metal selenides electrode material, which is characterized in that transition metal selenides is with array junctions
The form of structure is grown in nickel sheet (NF) substrate, and the transition metal of transition metal selenides is preferably：Manganese, iron, cobalt, nickel, copper etc.
One or more of.Transition metal selenides is nano bar-shape structure；Preferred vertical is grown,
A kind of preparation method of array structure transition metal selenides electrode material of the present invention, is broadly divided into three steps：The
One step simply pre-processes nickel sheet (NF) substrate；Second step is in nickel sheet substrate surface original position homoepitaxial transition metal organic backbone
Material array obtains NF-MOFs materials；Third is walked in MOFs nanometer rods or/and piece surface in situ selenizing, and array junctions are finally made
Structure transition metal selenides electrode material.
The synthetic method of the above-mentioned a variety of transition metal selenides array electrode materials of the present invention, specifically includes following steps：
The first step carries out ultrasonic pretreatment to nickel sheet (NF) substrate respectively with hydrochloric acid, acetone, ethyl alcohol and water successively；By nickel sheet
It is put into hydrochloric acid, concentration of hydrochloric acid 4-8M, stops after being ultrasonically treated 10-15 minutes；Acetone, second alcohol and water are respectively taken identical super
Sonication mode；
Second step grows MOFs nanometer rods/piece by hydro-thermal method in NF substrates；The pretreated NF of the first step is immersed
Carry out hydro-thermal reaction in mother liquor B, mother liquor B be 2,5-Dihydroxyterephthalic acid, transition metal salt, n,N-Dimethylformamide with
The mixed liquor of water, and ethanol in proper amount or isopropanol is added；Wherein 0.5- is corresponded to per 0.1-0.5g 2,5- dihydric para-phthalic acids
1.0g transition metal salts (transition metal salt preferably four chloride hydrate manganese, Iron dichloride tetrahydrate, cabaltous nitrate hexahydrate, six hydrations
One or more of nickel nitrate, Gerhardite) corresponding 20-45ml n,N-Dimethylformamide and water mixed solution,
Further the volume ratio of N,N-dimethylformamide, water, ethyl alcohol or isopropanol is (1-15):1:1；And it is anti-to move into polytetrafluoroethylene (PTFE)
It answers and reacts 9-24h in kettle, temperature is maintained at 85-135 DEG C；There is the NF of transition metal M OFs to use respectively growth in situ after reaction
Ethyl alcohol, n,N-Dimethylformamide washing are multiple, finally obtain NF-MOF composite materials；
The synthetic NF-MOF of selenium powder and previous step is placed in magnetic boat by third step simultaneously, and magnetic boat is put into tube furnace
In, using nitrogen protection, heating temperature is 300-400 DEG C, and preferably 350 DEG C, the time is 0.5-3 hours, preferably 1.5 hours.
Every 0.5-1.0g transition metal salts in further preferred second step correspond to the selenium powder 0.1-0.3g in third step.
Gained NF-MxSeyThe application of nano-array material decomposes water as electrode.
Nano-array electrode material NF-MxSeyThe application that can be used as electrode is further used for efficient electrocatalytic decomposition water, phase
There are a variety of advantages for traditional electrolyte water catalyst material, the stability of selenides nano-array electrode material is stronger, contains
A variety of transition metal, structure composition are various, loose porous, active site is abundant, large specific surface area, adjustability are high, plasticity is strong.
The present invention is prepared for the ordered nano array electrode material NF-M of regular patternxSeyIt, should as electrolysis water electrode
Method is simple with synthetic method, building-up process is controllable, can synthesize a variety of selenides, synthetic method is with universality, composition
The advantages such as various, it is often more important that, which has very big specific surface area and abundant active site, and then in OER
With lower starting point, larger current density, the aqueous energy of excellent electrocatalytic decomposition and higher stability, can be applicable to
The new energy such as electrolysis water store and conversion equipment.Preparation method of the present invention is simple for process, easy to implement, yield is high, is conducive to batch
Prepare high performance electrode material.NF-MxSeyAs electrolytic water electric it is great have lower starting point, larger current density,
The aqueous energy of excellent electrocatalytic decomposition and higher stability, can be applicable to the storage of the new energy such as electrolysis water and conversion equipment.
Description of the drawings
The scanning electron microscope schematic diagram of NF-Co-MOF in 1 for Fig. 1.
NF-CoSe in 1 for Fig. 22The scanning electron microscope schematic diagram of composite material.
The scanning electron microscope schematic diagram of NF-Ni-MOF in 2 for Fig. 3.
NF-NiSe in 2 for Fig. 42The scanning electron microscope schematic diagram of composite material.
The a variety of NF-M of Fig. 5xSeyThe performance schematic diagram of composite material electrocatalytic decomposition water.
Specific implementation mode
With reference to embodiment, the invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
The first step uses hydrochloric acid, acetone, second alcohol and water ultrasound to handle specific method to nickel sheet (NF) in 10 minutes respectively：It configures
The NF for shearing shape is positioned in the hydrochloric acid solution by the aqueous hydrochloric acid solution of 4-8M concentration, 10-15 minutes ultrasonic, with phase Tongfang
Method is cleaned by ultrasonic using acetone, second alcohol and water successively.The NF after the completion of cleaning is dried later, in case using in next step.
NF is immersed mother liquor B and carries out hydro-thermal reaction by second step, mother liquor B be 0.15g 2,5-Dihydroxyterephthalic acid and
0.7g cabaltous nitrate hexahydrates are dissolved in 20ml N,N-dimethylformamides and water and alcohol mixed solution.Wherein N, N- dimethyl methyl
Amide is 1 with the volume ratio of water and ethyl alcohol:1:1, and move into hydrothermal temperature in the reaction kettle of 100ml and be maintained at 100 DEG C, when
Between 15 hours.It is washed with ethyl alcohol, N,N-dimethylformamide after reaction and repeatedly obtains NF-Co-MOF composite materials.
The synthetic NF-Co-MOF composite materials of 0.1-0.3g selenium powders and previous step are placed in magnetic boat by third step simultaneously,
And magnetic boat is placed in tube furnace, using nitrogen protection, reaction temperature is 350 DEG C, and the time is 1.5 hours, finally obtains NF-
CoSe2Nano-array electrode material.
Embodiment 2
The first step uses hydrochloric acid, acetone, second alcohol and water ultrasound to pre-process specific method to nickel sheet (NF) in 10 minutes respectively：Configuration
The aqueous hydrochloric acid solution of good 4-8M concentration, the NF for shearing shape is positioned in the hydrochloric acid solution, and 10-15 minutes ultrasonic, use is identical
Method is cleaned by ultrasonic using acetone, second alcohol and water successively.The NF after the completion of cleaning is dried later, in case making in next step
With.
NF is immersed mother liquor B and carries out hydro-thermal reaction by second step, mother liquor B be 0.15g 2,5-Dihydroxyterephthalic acid and
0.7g Nickelous nitrate hexahydrates are dissolved in 20ml N,N-dimethylformamides and water and alcohol mixed solution.Wherein N, N- dimethyl methyl
Amide is 1 with the volume ratio of water and ethyl alcohol:1:1, and move into hydrothermal temperature in the reaction kettle of 100ml and be maintained at 100 DEG C, when
Between 15 hours.It is washed with ethyl alcohol, N,N-dimethylformamide after reaction and repeatedly obtains NF-Ni-MOF composite materials.
The synthetic NF-Ni-MOF composite materials of 0.1-0.3g selenium powders and previous step are placed in magnetic boat by third step simultaneously,
And magnetic boat is placed in tube furnace, using nitrogen protection, reaction temperature is 350 DEG C, and the time is 1.5 hours, finally obtains NF-
NiSe2Nano-array electrode material.
The test result of material obtained by above-described embodiment, specifically sees below：
(1) material morphology characterizes：
NF-Co-MOF, the NF-CoSe are taken respectively2, NF-Ni-MOF and NF-NiSe2One fritter of electrode material selects Cai
Department's SIGMA 500/VP model field emission scanning electron microscopes characterize it.Structure and morphology figure is shown in Fig. 1, Fig. 2, Fig. 3, figure
4。
(2) material electrochemical performance characterizes：
This test electro-chemical test instrument used is German ZAHNER electrochemical workstations.Fig. 5 is NF-MxSeyCompound electric
The i-v curve of (sweep speed 5mv/s) is tested in pole in 1.0M potassium hydroxide solutions.
Claims (9)
1. a kind of array structure transition metal selenides electrode material, which is characterized in that transition metal selenides is with array structure
Form be grown in nickel sheet (NF) substrate.
2. a kind of array structure transition metal selenides electrode material described in accordance with the claim 1, which is characterized in that transition gold
Belong to selenides transition metal be preferably：One or more of manganese, iron, cobalt, nickel, copper etc..
3. a kind of array structure transition metal selenides electrode material described in accordance with the claim 1, which is characterized in that transition gold
It is nanometer rods or/and laminated structure to belong to selenides；Vertical nickel sheet (NF) growth.
4. a kind of method of array structure transition metal selenides electrode material of claim 1-3 any one of them is prepared,
It is characterized in that, includes the following steps：It is broadly divided into three steps：The first step simply pre-processes nickel sheet (NF) substrate；Second step is in nickel
Piece substrate surface original position homoepitaxial transition metal organic framework material array obtains NF-MOFs materials；Third step is received in MOFs
Array structure transition metal selenides electrode material is finally made in rice stick or/and piece surface in situ selenizing.
5. according to the method for claim 4, which is characterized in that specifically include following steps：
The first step carries out ultrasonic pretreatment to nickel sheet (NF) substrate respectively with hydrochloric acid, acetone, ethyl alcohol and water successively；Nickel sheet is put into
In hydrochloric acid, concentration of hydrochloric acid 4-8M stops after being ultrasonically treated 10-15 minutes；Acetone, second alcohol and water are respectively taken at identical ultrasound
Reason mode；
Second step grows MOFs nanometer rods/piece by hydro-thermal method in NF substrates；The pretreated NF of the first step is immersed into mother liquor B
Middle carry out hydro-thermal reaction, mother liquor B are 2,5-Dihydroxyterephthalic acid, transition metal salt, n,N-Dimethylformamide and water
Mixed liquor, and ethanol in proper amount or isopropanol is added；Wherein 0.5-1.0g is corresponded to per 0.1-0.5g 2,5- dihydric para-phthalic acids
Transition metal salt corresponds to the mixed solution of 20-45ml n,N-Dimethylformamide and water, n,N-Dimethylformamide, water, ethyl alcohol
Or the volume ratio of isopropanol is (1-15):1:1；And move into and react 9-24h in ptfe autoclave, temperature is maintained at 85-
135℃；There is the NF of transition metal M OFs to be washed respectively with ethyl alcohol, N,N-dimethylformamide the growth in situ after reaction more
It is secondary, finally obtain NF-MOF composite materials；
The synthetic NF-MOF of selenium powder and previous step is placed in magnetic boat by third step simultaneously, and magnetic boat is put into tube furnace, is adopted
With nitrogen protection, heating temperature is 300-400 DEG C, and the time is 0.5-3 hours.
6. according to the method for claim 5, which is characterized in that transition metal salt preferably four chloride hydrate manganese, four hydration chlorine
Change one or more of ferrous iron, cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, Gerhardite.
7. according to the method for claim 5, which is characterized in that every 0.5-1.0g transition metal salts in second step correspond to the
Selenium powder 0.1-0.3g in three steps.
8. according to the method for claim 5, which is characterized in that it is preferably 350 DEG C that third, which walks temperature, and the time is 1.5 hours.
9. a kind of application of array structure transition metal selenides electrode material of claim 1-3 any one of them, as electricity
Extremely decompose water.
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| CN109360971A (en) * | 2018-11-26 | 2019-02-19 | 重庆文理学院 | A kind of preparation method of microspheroidal manganese selenide/carbon composite |
| CN109888237A (en) * | 2019-03-07 | 2019-06-14 | 肇庆市华师大光电产业研究院 | A kind of anode material of lithium-ion battery and preparation method thereof |
| CN110449156A (en) * | 2019-07-18 | 2019-11-15 | 山东大学 | Growth in situ is Prussian blue in a kind of metallic substrates or the derivative elctro-catalyst and preparation method thereof of Prussian blue similar object |
| CN110655654A (en) * | 2019-09-18 | 2020-01-07 | 常州大学 | Preparation of two-dimensional layered cobalt-based metal organic framework (Co-MOF) electrode material and research on oxygen evolution performance |
| CN110841713A (en) * | 2019-10-17 | 2020-02-28 | 杭州电子科技大学 | Copper-cobalt bimetallic-organic framework material based on 2, 5-dihydroxy terephthalic acid ligand and preparation method and application thereof |
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| CN113363079B (en) * | 2020-03-04 | 2022-11-15 | 华东理工大学 | Hollow Cu 7 Se 4 -Cu x Co 1-x Se 2 Nanosphere composite material and preparation method and application thereof |
| CN112058309A (en) * | 2020-08-14 | 2020-12-11 | 华南理工大学 | Fusiform MnFeNi-MOF-74 material growing in situ on foamed nickel and preparation method and application thereof |
| CN112877680A (en) * | 2021-01-11 | 2021-06-01 | 延安大学 | Composite electrode material and preparation method and application thereof |
| CN113930782A (en) * | 2021-09-24 | 2022-01-14 | 南京信息工程大学 | Preparation method and application of self-supporting electrode |
| CN113930782B (en) * | 2021-09-24 | 2023-06-20 | 南京信息工程大学 | Preparation method and application of self-supporting electrode |
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