CN107317005A - A kind of hybrid metal sulfide electrode and preparation method thereof - Google Patents
A kind of hybrid metal sulfide electrode and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- 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
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- 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
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- H01—ELECTRIC ELEMENTS
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- 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
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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Abstract
The invention discloses a kind of hybrid metal sulfide electrode and preparation method thereof.The hybrid metal sulfide electrode is made up of central core layer and peripheral shell, and perpendicular to conductive substrates formation hierarchical array structure.The preparation method is that the compound containing iron, cobalt or nickel is dissolved in the mixed aqueous solution containing molybdenum and sulphur respectively, using high pressure hydro-thermal method, on conductive substrates material, and single step reaction obtains hybrid metal sulfide electrode.The hierarchy of the electrode is conducive to improving the specific surface area of electrode material and increases active site；Array structure is conducive to improving electric transmission efficiency and the diffusion of electrolyte of electrode material；Regulatable electron energy level is conducive to electronics being efficiently injected into from electrode to electrolyte.These advantages make the high of the corresponding single metal sulfide electrode of the catalytic activity, stability and corresponding device performance ratio of hybrid metal sulfide electrode.Electrode prepared by this method can meet energy conversion and the application requirement of memory device of high efficiency, low cost.
Description
Technical field
The present invention relates to energy conversion and energy stores electrode, a kind of hybrid metal sulfide electrode and its system are particularly belonged to
Preparation Method.
Background technology
In energy conversion device, such as DSSC, photolysis water hydrogen device, photocatalytic degradation of dye device
Part or low-temperature fuel cell, noble metal platinum are widely used in various catalysis electrodes as catalyst material, but its cost it is high with
And the corrosion in various electrolyte solutions hinders commercial application of the platinum in energy conversion device.In energy storage device
In, such as ultracapacitor or lithium ion battery, generally using carbon-based material or lithium salts with layer structure as electrode material.
The key of efficient energy conversion and memory device is the preparation of electrode.Develop low cost new structure has height
The electrode of specific surface area and high electronic conduction ability, it is significant.
Single metal sulfide is compared to, inexpensive hybrid metal sulfide can be by regulating and controlling metal species and change
Bandgap structure and pattern of the metering than adjusting material are learned, the catalytic performance of excellent performance is obtained.Existing hybrid metal sulfide
Synthesis condition and preparation technology it is more complicated, mainly have multi-step synthetic method, such as comprising hydro-thermal reaction, chemical bath deposition and ion
The steps such as exchange reaction.And the hybrid metal sulfide being synthesized does not have direct vertical-growth in being divided in conductive substrates
Level array structure electrode.Therefore, a kind of one-step method is invented directly to grow the hybrid metal sulfide with hierarchical array structure
In in conductive substrates, so as to obtain the electrode of excellent properties, apply in energy conversion and memory device, with important meaning
Justice.
The content of the invention
It is an object of the invention to provide a kind of hybrid metal sulfide electrode and preparation method thereof.The electrode should have
Hierarchical array structure, it is characterized in that hybrid metal sulfide is made up of central core layer and peripheral shell, and perpendicular to conductive substrates
Hierarchical array structure is formed, its central core layer is the sulfide rich in iron, cobalt or nickel, and peripheral shell is receiving rich in molybdenum disulfide
Rice piece.The performance characteristic of the electrode is the specific surface area for the electrode that hierarchy can increase to increase active site；
Array structure can improve the diffusion of electric transmission efficiency and electrolyte；Material can be adjusted by regulating and controlling metal species and stoichiometric proportion
The bandgap structure of material is efficiently injected into so as to obtain suitable energy level distribution and be advantageously implemented electronics to electrode to electrolyte.This
A little advantages make the catalytic activity, stability and corresponding device performance of hybrid metal sulfide electrode all than corresponding single gold
Belong to sulfide high.Methods described should simply and can prepare meet high efficiency, low cost energy conversion with memory device applications requirement
Electrode.
To achieve these goals, the technical solution that provides of the present invention is：
A kind of hybrid metal sulfide electrode, the hybrid metal sulfide is made up of central core layer and peripheral shell, and
Perpendicular to conductive substrates formation hierarchical array structure, its central core layer is the sulfide rich in iron, cobalt or nickel, and peripheral shell is richness
Nanometer sheet containing molybdenum disulfide.
A kind of preparation method of hybrid metal sulfide electrode, comprises the following steps：
1) hybrid metal precursor water solution is prepared, wherein：Acetylacetone,2,4-pentanedione concentration of iron is 0.01-0.1molL-1, molybdic acid
Na concn is 0.01-0.1molL-1, thiourea concentration be 0.05-0.3molL-1, polyethylene glycol-block- polypropylene glycols-
Block- Polyethylene glycols are 1-5mmolL-1, ammonium hydroxide concentration be 8-12molL-1；
2) by step 1) prepare hybrid metal precursor water solution be placed in ptfe autoclave liner, by conduction
The conducting surface of base material is perpendicularly inward, or parallel downward, is placed in ptfe autoclave liner, closed, high pressure hydro-thermal
Reaction, reaction temperature is 150-200 DEG C, and the reaction time is 10-18 hours, is cooled to room temperature, is washed, ethanol cleaning, is mixed
Close metal sulfide electrode.
Ferric acetyl acetonade in described hybrid metal precursor water solution can use cobalt chloride, cobalt nitrate, cobalt acetate, chlorination
Nickel, nickel nitrate or nickel acetate are substituted.
Sodium molybdate in described hybrid metal precursor water solution can be substituted with ammonium molybdate or ammonium thiomolybdate.
Thiocarbamide in described hybrid metal precursor water solution can be substituted with thioacetamide.
Polyethylene glycol-block- polypropylene glycol-block- polyethylene glycol in described hybrid metal precursor water solution
Mean molecule quantity be 5600-11400；Preferably 8400.
Described conductive substrates material is that titanium foil sheet or net, stainless steel substrates or net, nickel foam, FTO electro-conductive glass or ITO are led
Electric glass.
Compared with prior art, beneficial effects of the present invention：Hybrid metal sulfide electrode prepared by the present invention have with
Lower architectural feature：1) central core layer is the sulfide rich in iron, cobalt or nickel；2) peripheral shell is the nanometer rich in molybdenum disulfide
Piece；3) hybrid metal sulfide is perpendicular to conductive substrates formation hierarchical array structure.The hybrid metal sulfide electrode of the present invention
With following performance characteristic：1) hierarchy is conducive to improving the specific surface area of electrode material and increases active site；2)
Array structure is conducive to improving electric transmission efficiency and the diffusion of electrolyte of electrode material；3) can be by controlling precursor solution
Middle metal species and stoichiometric proportion, so that the electron energy level for regulating and controlling electrode is conducive to effective note of the electronics from electrode to electrolyte
Enter；4) catalytic activity of hybrid metal sulfide electrode, stability and corresponding device performance are all than corresponding single metal sulphur
Compound is high；5) electrode being prepared by the method for the present invention, in DSSC, photoelectric transformation efficiency to be up to
To 9.32%；For in photolysis water hydrogen device, hydrogen production efficiency to be up to 9.50%；For in ultracapacitor, in 2A/g
Under, specific capacitance is up to 850F/g；6) preparation condition of the present invention is gently controllable, and method is easy and effective, and cost is low, is conducive to commercialization
Large-scale production.
Embodiment
Embodiment 1
1) by 0.04molL-1Ferric acetyl acetonade, 0.04molL-1Sodium molybdate, 0.15molL-1Thiocarbamide, 2mmol
L-1Mean molecule quantity is 8400 polyethylene glycol-block- polypropylene glycol-block- polyethylene glycol and 10molL-1Hydroxide
Ammonium is soluble in water, prepares hybrid metal precursor water solution；
2) by step 1) prepare hybrid metal sulfide precursor water solution be placed in ptfe autoclave liner,
Titanium foil sheet is crimped and is close to the inwall of inner liner of reaction kettle, closed, high pressure hydro-thermal reaction, reaction temperature is 200 DEG C, reaction time
For 12 hours, room temperature is cooled to, is washed, ethanol cleaning obtains iron sulfide vulcanization molybdenum electrode.
The iron sulfide vulcanizes molybdenum electrode and is made up of central core layer and peripheral shell, and perpendicular to titanium foil sheet formation classification battle array
Array structure, its central core layer is rich in iron sulfide, and peripheral shell is rich in molybdenum sulfide.The iron sulfide vulcanization molybdenum electrode of acquisition is used for
In DSSC to electrode.When light intensity is 100mWcm-2When, the cell photoelectric current density is 16.50mA
cm-2, open-circuit voltage is 0.75V, and fill factor, curve factor is 0.65, and photoelectric transformation efficiency reaches 8.04%, quick to the dyestuff of electrode with platinum
The photoelectric transformation efficiency 8.10% for changing solar cell is suitable.
Embodiment 2
1) by 0.03molL-1Cobalt chloride, 0.03molL-1Sodium molybdate, 0.12molL-1Thiocarbamide, 2mmolL-1It is flat
Average molecular weight is 8400 polyethylene glycol-block- polypropylene glycol-block- polyethylene glycol and 8molL-1Ammonium hydroxide is dissolved in
In water, hybrid metal precursor water solution is prepared；
2) by step 1) prepare hybrid metal sulfide precursor water solution be placed in ptfe autoclave liner,
The conduction of FTO electro-conductive glass is placed in reactor parallel to the substrate of inner liner of reaction kettle down, closed, high pressure hydro-thermal is anti-
Should, reaction temperature is 180 DEG C, and the reaction time is 15 hours, is cooled to room temperature, is washed, ethanol cleaning, obtains cobalt sulfide@vulcanizations
Molybdenum electrode.
The cobalt sulfide vulcanizes molybdenum electrode and is made up of central core layer and peripheral shell, and perpendicular to the formation point of FTO electro-conductive glass
Level array structure, its central core layer is rich in cobalt sulfide, and peripheral shell is rich in molybdenum sulfide.The cobalt sulfide of acquisition is vulcanized into molybdenum electrode
For in DSSC to electrode.When light intensity is 100mWcm-2When, the cell photoelectric current density is
17.35mA·cm-2, open-circuit voltage is 0.79V, and fill factor, curve factor is 0.68, and photoelectric transformation efficiency reaches 9.32%, higher than platinum to electricity
The photoelectric transformation efficiency 8.10% of the DSSC of pole.
Embodiment 3
1) by 0.03molL-1Nickel chloride, 0.06molL-1Ammonium molybdate, 0.20molL-1Thiocarbamide, 2mmolL-1It is flat
Average molecular weight is 8400 polyethylene glycol-block- polypropylene glycol-block- polyethylene glycol and 10molL-1Ammonium hydroxide is dissolved in
In water, hybrid metal precursor water solution is prepared；
2) by step 1) prepare hybrid metal sulfide precursor water solution be placed in ptfe autoclave liner,
Titanium foil sheet is crimped and is close to the inwall of inner liner of reaction kettle, closed, high pressure hydro-thermal reaction, reaction temperature is 180 DEG C, reaction time
For 15 hours, room temperature is cooled to, is washed, ethanol cleaning obtains nickel sulfide vulcanization molybdenum electrode.
The nickel sulfide vulcanizes molybdenum electrode and is made up of central core layer and peripheral shell, and perpendicular to titanium foil sheet formation classification battle array
Array structure, its central core layer is rich in nickel sulfide, and peripheral shell is rich in molybdenum sulfide.The nickel sulfide vulcanization molybdenum electrode of acquisition is used for
In DSSC to electrode.When light intensity is 100mWcm-2When, the cell photoelectric current density is 17.05mA
cm-2, open-circuit voltage is 0.77V, and fill factor, curve factor is 0.66, and photoelectric transformation efficiency reaches 8.66%, higher than dyestuff of the platinum to electrode
The photoelectric transformation efficiency 8.10% of sensitization solar battery.
Embodiment 4
1) by 0.05molL-1Nickel nitrate, 0.08molL-1Ammonium thiomolybdate, 0.10molL-1Thiocarbamide, 2mmol
L-1Mean molecule quantity is 8400 polyethylene glycol-block- polypropylene glycol-block- polyethylene glycol and 12molL-1Hydroxide
Ammonium is dissolved in water, prepares hybrid metal precursor water solution；
2) by step 1) prepare hybrid metal sulfide precursor water solution be placed in ptfe autoclave liner,
Nickel foam is crimped and is close to the inwall of inner liner of reaction kettle, closed, high pressure hydro-thermal reaction, reaction temperature is 180 DEG C, reaction time
For 18 hours, room temperature is cooled to, is washed, ethanol cleaning obtains nickel sulfide vulcanization molybdenum electrode.
The nickel sulfide vulcanizes molybdenum electrode and is made up of central core layer and peripheral shell, vertically and around the formation point of foam nickel wire
Level array structure, its central core layer is rich in nickel sulfide, and peripheral shell is rich in molybdenum sulfide.The nickel sulfide of acquisition is vulcanized into molybdenum electrode
For in ultracapacitor, under 2A/g, specific capacitance to be up to 850F/g.
Embodiment 5
1) by 0.05molL-1Cobalt acetate, 0.05molL-1Ammonium molybdate, 0.12molL-1Thioacetamide,
2mmol·L-1Mean molecule quantity is 8400 polyethylene glycol-block- polypropylene glycol-block- polyethylene glycol and 10molL-1
Ammonium hydroxide is soluble in water, prepares hybrid metal precursor water solution；
2) by step 1) prepare hybrid metal sulfide precursor water solution be placed in ptfe autoclave liner,
Nickel foam is crimped and is close to the inwall of inner liner of reaction kettle, closed, high pressure hydro-thermal reaction, reaction temperature is 180 DEG C, reaction time
For 18 hours, room temperature is cooled to, is washed, ethanol cleaning obtains cobalt sulfide vulcanization molybdenum electrode.
The cobalt sulfide vulcanizes molybdenum electrode and is made up of central core layer and peripheral shell, vertically and around the formation point of foam nickel wire
Level array structure, its central core layer is rich in cobalt sulfide, and peripheral shell is rich in molybdenum sulfide.The cobalt sulfide of acquisition is vulcanized into molybdenum electrode
For in photolysis water hydrogen device, hydrogen production efficiency to reach 9.50%.
Claims (7)
1. a kind of hybrid metal sulfide electrode, it is characterised in that the hybrid metal sulfide is by central core layer and outer casing
Layer is constituted, and perpendicular to conductive substrates formation hierarchical array structure, its central core layer is the sulfide rich in iron, cobalt or nickel, outside
Casing layer is the nanometer sheet rich in molybdenum disulfide.
2. a kind of preparation method of hybrid metal sulfide electrode as claimed in claim 1, it is characterised in that including following step
Suddenly：
1) hybrid metal precursor water solution is prepared, wherein：Acetylacetone,2,4-pentanedione concentration of iron is 0.01-0.1molL-1, sodium molybdate it is dense
Spend for 0.01-0.1molL-1, thiourea concentration be 0.05-0.3molL-1, polyethylene glycol-block- polypropylene glycols-block-
Polyethylene glycol is 1-5mmolL-1, ammonium hydroxide concentration be 8-12molL-1；
2) by step 1) prepare hybrid metal precursor water solution be placed in ptfe autoclave liner, by conductive substrates
The conducting surface of material is perpendicularly inward, or parallel downward, is placed in ptfe autoclave liner, closed, high pressure hydro-thermal reaction,
Reaction temperature is 150-200 DEG C, and the reaction time is 10-18 hours, is cooled to room temperature, is washed, ethanol cleaning, obtains hybrid metal
Sulfide electrode.
3. a kind of preparation method of hybrid metal sulfide electrode as claimed in claim 2, it is characterised in that described acetyl
Acetone iron can be substituted with cobalt chloride, cobalt nitrate, cobalt acetate, nickel chloride, nickel nitrate or nickel acetate.
4. a kind of preparation method of hybrid metal sulfide electrode as claimed in claim 2, it is characterised in that described molybdic acid
Sodium can be substituted with ammonium molybdate or ammonium thiomolybdate.
5. a kind of preparation method of hybrid metal sulfide electrode as claimed in claim 2, it is characterised in that described thiocarbamide
It can be substituted with thioacetamide.
6. a kind of preparation method of hybrid metal sulfide electrode as claimed in claim 2, it is characterised in that the poly- second two
The mean molecule quantity of alcohol-block- polypropylene glycol-block- polyethylene glycol is 5600-11400.
7. a kind of preparation method of hybrid metal sulfide electrode as claimed in claim 2, it is characterised in that described conduction
Base material is titanium foil sheet or net, stainless steel substrates or net, nickel foam, FTO electro-conductive glass or ITO electro-conductive glass.
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| CN108565128A (en) * | 2018-04-02 | 2018-09-21 | 桂林电子科技大学 | A kind of preparation method and application of Cu-Mo-S nuclear-shell structured nano-composite materials |
| CN108598410A (en) * | 2018-04-20 | 2018-09-28 | 河北工业大学 | A kind of preparation method of lithium-sulfur cell sandwich material |
| CN109235024A (en) * | 2018-09-04 | 2019-01-18 | 北京邮电大学 | A kind of heterogeneous nano-chip arrays structure of nickel sulfide-molybdenum sulfide and preparation method thereof of carbon cloth load |
| CN109972160A (en) * | 2019-04-23 | 2019-07-05 | 重庆文理学院 | A kind of preparation method of novel double-function catalyzing electrolysis water electrode |
| CN110391089A (en) * | 2019-08-27 | 2019-10-29 | 信阳学院 | A kind of MoS2@CoS2The preparation method of composite material |
| CN111020626A (en) * | 2019-12-09 | 2020-04-17 | 北京工业大学 | Preparation method and application of nickel-molybdenum oxide with 3D nanosheet-nanorod mixed structure |
| CN112863887A (en) * | 2020-12-28 | 2021-05-28 | 沈阳工业大学 | Preparation method of high-performance cabbage-shaped heterostructure electrode material |
| CN113380558A (en) * | 2021-06-21 | 2021-09-10 | 贵州化工建设有限责任公司 | Slag pretreatment method and preparation method of supercapacitor electrode material |
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| CN108390062A (en) * | 2018-02-08 | 2018-08-10 | 陕西科技大学 | A kind of preparation method and applications of sodium-ion battery cathode stainless (steel) wire load molybdenum disulfide nano sheet |
| CN108565128A (en) * | 2018-04-02 | 2018-09-21 | 桂林电子科技大学 | A kind of preparation method and application of Cu-Mo-S nuclear-shell structured nano-composite materials |
| CN108598410A (en) * | 2018-04-20 | 2018-09-28 | 河北工业大学 | A kind of preparation method of lithium-sulfur cell sandwich material |
| CN109235024A (en) * | 2018-09-04 | 2019-01-18 | 北京邮电大学 | A kind of heterogeneous nano-chip arrays structure of nickel sulfide-molybdenum sulfide and preparation method thereof of carbon cloth load |
| CN109235024B (en) * | 2018-09-04 | 2021-04-20 | 北京邮电大学 | Carbon cloth loaded nickel sulfide-molybdenum sulfide heterogeneous nanosheet array structure and preparation method thereof |
| CN109972160A (en) * | 2019-04-23 | 2019-07-05 | 重庆文理学院 | A kind of preparation method of novel double-function catalyzing electrolysis water electrode |
| CN110391089A (en) * | 2019-08-27 | 2019-10-29 | 信阳学院 | A kind of MoS2@CoS2The preparation method of composite material |
| CN111020626A (en) * | 2019-12-09 | 2020-04-17 | 北京工业大学 | Preparation method and application of nickel-molybdenum oxide with 3D nanosheet-nanorod mixed structure |
| CN112863887A (en) * | 2020-12-28 | 2021-05-28 | 沈阳工业大学 | Preparation method of high-performance cabbage-shaped heterostructure electrode material |
| CN112863887B (en) * | 2020-12-28 | 2022-02-08 | 沈阳工业大学 | Preparation method of high-performance cabbage-shaped heterostructure electrode material |
| CN113380558A (en) * | 2021-06-21 | 2021-09-10 | 贵州化工建设有限责任公司 | Slag pretreatment method and preparation method of supercapacitor electrode material |
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