CN109261168A - A kind of Ni of vanadium modification3S2Nano-bar array electrode material and preparation method thereof - Google Patents
A kind of Ni of vanadium modification3S2Nano-bar array electrode material and preparation method thereof Download PDFInfo
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- CN109261168A CN109261168A CN201811200454.8A CN201811200454A CN109261168A CN 109261168 A CN109261168 A CN 109261168A CN 201811200454 A CN201811200454 A CN 201811200454A CN 109261168 A CN109261168 A CN 109261168A
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Abstract
The present invention provides a kind of Ni of vanadium modification3S2Nano-bar array electrode material, with particles self assemble at squamous surface topography.The preparation method comprises the following steps: by metallic nickel be immersed in containing vanadium source, sulphur source, ammonium fluoride suspension in, carry out solvent thermal reaction；Then, solvent thermal reaction product is calcined, obtains the Ni of the vanadium modification of nano bar-shape3S2Electrode material.Wherein, vanadium source is vanadyl acetylacetonate, sodium metavanadate, sodium vanadate, 12 hydration sodium vanadates, ammonium metavanadate or vanadic anhydride；Sulphur source is thiocarbamide, thioacetamide, vulcanized sodium, sodium oiethyl dithiocarbamate or sulphur simple substance.The presence of the nanorod structure of particles self assemble, secondary units effectively increases the active site of material, compared to bulk catalyst, effectively reduces the resistance of material, can be used as a kind of excellent electro-catalysis production oxygen elctro-catalyst.
Description
Technical field
The invention belongs to electrolysis water catalytic fields, and in particular to a kind of Ni of vanadium modification3S2Nano-bar array electrode material and
Preparation method.
Background technique
Electro-catalysis water-splitting hydrogen producing technology is an emerging technology, meets people currently to the craving of the energy.It solves
There is currently energy crisis and problem of environmental pollution.And during electrolysis water, water oxygen is the rate controlling in water splitting processes
Step restricts the whole process of water-splitting, thus seeks a kind of efficient water-splitting to produce oxygen elctro-catalyst to be to improve water-splitting effect
The core of rate has important research significance.
Currently, transition metal iron, cobalt, nickel-base material are shown excellent since its reserves is big and self-conductive is high
Electro catalytic activity, receive the extensive concern of people.Wherein, Ni3S2Material is ground extensively since the excellent characteristics of itself receives
Study carefully.The Ni prepared reported at present3S2Material morphology includes sheet, flower pattern, rodlike etc..
Chinese invention issued patents the 201310320738.1st disclose a kind of electrolysis aquatic products oxygen composite catalyzing electrode and
Preparation method has been prepared using the method for hydro-thermal with rodlike Ni (OH)2/ Ni3S2Combination electrode, but material overpotential
It is larger, it can not use under conditions of high current, catalytic activity is poor.No. 201610252105.5 public affairs of Chinese invention issued patents
Three nickel of a kind of array type curing-carbon nano-tube combination electrode and its preparation method and application has been opened, has first been carried out instead with hydro-thermal method
It answers, then heat-treating methods obtain a kind of three nickel of array type curing-carbon nano-tube combination electrode material, reaction time is long, instead
It is harsh to answer condition, and cost is big.
And vanadium is widely used in sodium-ion battery and catalysis material preparation due to the variable valence of its own, and
By vanadium-based materials and Ni3S2Research in terms of Material cladding is less, thus study it is a kind of have low in cost, catalytic activity high and
The Ni of the simple vanadium modification of preparation process3S2Electrode material is of great significance.
Summary of the invention
This patent is directed to the deficiency of above-mentioned material, proposes a kind of Ni of vanadium modification3S2Nano-bar array electrode material, preparation
Simple process, reaction are mild and low in cost.Particles self assemble at nanorod electrodes material, the more catalytic active sites of exposure
Point effectively improves the electrolysis elutriation oxygen performance in alkaline electrolyte.To achieve the goals above, the present invention is using following
Technical solution.
(1) metallic nickel is successively immersed in acetone, hydrochloric acid and water and ethyl alcohol and is cleaned by ultrasonic, is then dried in vacuo, salt
Acid concentration is 1 ~ 5 mol/L；
(2) a certain amount of vanadium source, sulphur source are dissolved in the solvent of certain volume, vanadium source and sulphur source molar ratio are 1:(1 ~ 6), make
The vanadium source concentration obtained is 2 ~ 20mM, stirs 3 ~ 60min, obtains suspension A；
(3) it being added a certain amount of ammonium fluoride in suspended A, stirs 1 ~ 2 h, obtain solution B, the dosage of ammonium fluoride is 0.001 ~
0.06g；
(4) metallic nickel that will be handled well in the solution B being stirred and step (1), is fitted into autoclave, is subsequently placed in baking
Solvent thermal reaction is carried out in case；
(5) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol are rinsed for several times, so
After be dried in vacuo；
(6) product is calcined in tube furnace under vacuum conditions, obtains the Ni of the vanadium modification of nano bar-shape3S2Electrode material.
Metallic nickel described in step (1) is nickel foam or nickel screen.
Ultrasonic cleaning described in step (1) is 5 ~ 15min.
Vacuum drying described in step (1) is 5 ~ 20 h of vacuum drying at 20 ~ 80 DEG C.
Vanadium source described in step (2) is vanadyl acetylacetonate, sodium metavanadate, sodium vanadate, 12 hydration sodium vanadates, metavanadic acid
One or more of ammonium and vanadic anhydride.
Sulphur source described in step (2) is thiocarbamide, thioacetamide, vulcanized sodium, sodium oiethyl dithiocarbamate and sulphur
One or more of simple substance.
Solvent described in step (2) is one or more of ethylenediamine, dehydrated alcohol, methanol, ethylene glycol.
Solvent thermal reaction temperature described in step (4) is 50 ~ 200 DEG C, and the reaction time is 0.5 ~ 40h.
Vacuum drying described in step (5) is 5 ~ 20h of vacuum drying at 20 ~ 80 DEG C.
Calcination temperature described in step (6) is that calcination time is 0.5 ~ 4 h at 300 ~ 700 DEG C.
Compared with prior art, the present invention can obtain following the utility model has the advantages that
(1) present invention chooses suitable sulphur source and vanadium source, by introducing ammonium fluoride as surfactant, using a step solvent heat
The Ni of vanadium modification is made in method3S2Nano-bar array electrode material.
(2) step solvent thermal process of the present invention, at low cost, reaction time is short, reaction condition is mild, preparation process
Simply, stable product quality and pattern is uniform, it is environmentally friendly, it can be suitble to be mass produced.
(3) Ni of vanadium modification prepared by the present invention3S2Nano-bar array electrode material, the introducing of vanadium change the shape of material
The presence of looks, the nanorod structure of particles self assemble, secondary units effectively increases the active site of material, compared to block
Shape catalyst effectively reduces the resistance of material, can be used as a kind of excellent electro-catalysis production oxygen elctro-catalyst, in 10mA/cm2's
Under current density, overpotential can be down to 160 mV, in 100 mA/cm2Current density under, overpotential can be down to 420
mV。
Detailed description of the invention
Fig. 1 is the Ni of the vanadium modification being grown in nickel foam prepared by the embodiment of the present invention 43S2X-ray diffraction (XRD)
Map；
Fig. 2 is the Ni of the vanadium modification being grown in nickel foam prepared by the embodiment of the present invention 43S22500 times of amplification of scanning electricity
Mirror (SEM) photo；
Fig. 3 is the Ni of the vanadium modification being grown in nickel foam prepared by the embodiment of the present invention 43S230000 times of amplification of scanning
Electronic Speculum (SEM) photo；
Fig. 4 is the Ni of the vanadium modification being grown in nickel foam prepared by the embodiment of the present invention 43S2Linear sweep voltammetry (LSV)
Performance test figure.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the invention will be described in further detail:
Embodiment 1:
(1) nickel foam of (1 × 5) cm is immersed in and is cleaned by ultrasonic 5 min in acetone, nickel foam is immersed in 1 mol/L's again
5 min of ultrasonic cleaning are carried out in hydrochloric acid, are finally replaced flushing 3 times with deionized water with ethyl alcohol respectively, are dried in vacuo at 20 DEG C
The nickel foam that obtains that treated after 5 h；
(2) vanadyl acetylacetonate and thiocarbamide are weighed, taking vanadyl acetylacetonate is 0.04 mmol, controls mole in vanadium source and sulphur source
It than for 1:1, while being added in 20 ml ethylenediamines, 3 min of magnetic agitation obtains suspension A at room temperature；
(3) ammonium fluoride of 0.001 g is added in suspended A, stirs 1h, obtains solution B；
(4) metallic nickel that will be handled well in the solution B being stirred and step (1), is fitted into autoclave, is subsequently placed in baking
It is reacted in case, the reaction time is to carry out solvent thermal reaction under 0.5 h condition at 50 DEG C；
(5) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol are alternately rinsed 3 times,
Then 5 h are dried in vacuo at 20 DEG C；
(6) product is under nitrogen protection atmosphere, and calcination temperature is that 300 DEG C of calcination times are that 0.5h is placed in tube furnace and is forged
It burns, obtains the Ni of vanadium modification3S2Nano-bar array electrode material.
Embodiment 2:
(1) nickel foam of (1 × 5) cm is immersed in and is cleaned by ultrasonic 5 min in acetone, nickel foam is immersed in 1 mol/L's again
5 min of ultrasonic cleaning are carried out in hydrochloric acid, are finally replaced flushing 3 times with deionized water with ethyl alcohol respectively, are dried in vacuo at 30 DEG C
The nickel foam that obtains that treated after 8 h；
(2) sodium metavanadate and thioacetamide are weighed, taking sodium metavanadate is 0.06 mmol, controls the molar ratio in vanadium source and sulphur source
It for 1:2, while being added in 20 ml dehydrated alcohols, 10 min of magnetic agitation obtains suspension A at room temperature；
(3) ammonium fluoride of 0.004 g is added in suspended A, stirs 1 h, obtains solution B；
(4) metallic nickel that will be handled well in the solution B being stirred and step (1), is fitted into autoclave, is subsequently placed in baking
It is reacted in case, the reaction time is to carry out solvent thermal reaction under 5 h conditions at 100 DEG C；
(5) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol are alternately rinsed 3 times,
Then 8 h are dried in vacuo at 30 DEG C；
(6) product is under nitrogen protection atmosphere, and calcination temperature is that 400 DEG C of calcination times are that 1h is placed in tube furnace and is calcined,
Obtain the Ni of vanadium modification3S2Nano-bar array electrode material.
Embodiment 3:
(1) nickel screen of (1 × 5) cm is immersed in the hydrochloric acid for being cleaned by ultrasonic 10 min in acetone, nickel screen being immersed in 3 mol/L again
In carry out ultrasonic cleaning 15 min, finally respectively with ethyl alcohol replace with deionized water rinse 3 times, be dried in vacuo 10 at 40 DEG C
The nickel foam that obtains that treated after h；
(2) sodium vanadate and vulcanized sodium are weighed, taking sodium vanadate is 0.08 mmol, and the molar ratio for controlling vanadium source and sulphur source is 1:3, together
When be added in 20 ml methanol, 15 min of magnetic agitation obtains suspension A at room temperature；
(3) ammonium fluoride of 0.006 g is added in suspended A, stirs 2 h, obtains solution B；
(4) metallic nickel that will be handled well in the solution B being stirred and step (1), is fitted into autoclave, is subsequently placed in baking
It is reacted in case, the reaction time is to carry out solvent thermal reaction under 10 h conditions at 120 DEG C；
(5) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol are alternately rinsed 3 times,
Then 3 h are dried in vacuo at 20 DEG C；
(6) product is under nitrogen protection atmosphere, and calcination temperature is that 500 DEG C of calcination times are that 2h is placed in tube furnace and is calcined,
Obtain the Ni of vanadium modification3S2Nano-bar array electrode material.
Embodiment 4:
(1) nickel screen of (1 × 5) cm is immersed in the hydrochloric acid for being cleaned by ultrasonic 15 min in acetone, nickel screen being immersed in 4 mol/L again
In carry out ultrasonic cleaning 15 min, finally respectively with ethyl alcohol replace with deionized water rinse 3 times, be dried in vacuo 15 at 60 DEG C
The nickel foam that obtains that treated after h；
(2) ammonium metavanadate and sodium oiethyl dithiocarbamate are weighed, taking ammonium metavanadate is 0.2 mmol, controls vanadium source and sulphur source
Molar ratio be 1:4, while being added in 20 ml dehydrated alcohols, 30 min of magnetic agitation obtains suspension A at room temperature；
(3) ammonium fluoride of 0.04 g is added in suspended A, stirs 2 h, obtains solution B；
(4) metallic nickel that will be handled well in the solution B being stirred and step (1), is fitted into autoclave, is subsequently placed in baking
It is reacted in case, the reaction time is to carry out solvent thermal reaction under 20 h conditions at 160 DEG C；
(5) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol are alternately rinsed 3 times,
Then 15 h are dried in vacuo at 60 DEG C；
(6) product is under nitrogen protection atmosphere, and calcination temperature is that 600 DEG C of calcination times are that 4 h are placed in tube furnace and are calcined,
Obtain the Ni of vanadium modification3S2Nano-bar array electrode material.
The Ni of vanadium modification manufactured in the present embodiment3S2Electrode material, as can be seen from Figure 1 X-ray powder diffraction peak occurs
Position be expressed as Ni3S2Characteristic peak, remove Ni3S2Characteristic peak outside, without apparent diffraction maximum, show that having synthesized vanadium repairs
The Ni of decorations3S2Electrode material.
It can be seen that the pattern of the sample is nanometer stick array from 2500 times of SEM figures of amplification of Fig. 2.
From 30000 times of SEM figures of amplification of Fig. 3 it can be seen that the material be by particles self assemble at nanometer stick array,
Stick diameter is evenly distributed about in 300 ~ 600nm or so.
It is 10mA/cm that the sample be can be seen that from the linear sweep voltammetry figure of Fig. 4 in current density2When, it has low
Overpotential, down to 160 mV, in 100 mA/cm2Current density under, overpotential can be down to 420 mV, and material has good
Good electro-catalysis oxygen evolution activity.
Embodiment 5:
(1) nickel foam of (1 × 5) cm is immersed in and is cleaned by ultrasonic 5 min in acetone, nickel foam is immersed in 5 mol/L's again
15 min of ultrasonic cleaning are carried out in hydrochloric acid, finally replace flushing 3 times with deionized water with ethyl alcohol respectively, and vacuum is dry at 80 DEG C
The nickel foam that obtains that treated after dry 20 h；
(2) vanadic anhydride and thioacetamide are weighed, taking vanadic anhydride is 0.4 mmol, controls mole in vanadium source and sulphur source
It than for 1:6, while being added in 20 ml ethylene glycol, 60 min of magnetic agitation obtains suspension A at room temperature；
(3) ammonium fluoride of 0.06 g is added in suspended A, stirs 2 h, obtains solution B；
(4) metallic nickel that will be handled well in the solution B being stirred and step (1), is fitted into autoclave, is subsequently placed in baking
It is reacted in case, the reaction time is to carry out solvent thermal reaction under 40 h conditions at 200 DEG C；
(5) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol are alternately rinsed 3 times,
Then 20 h are dried in vacuo at 80 DEG C；
(6) product is under nitrogen protection atmosphere, and calcination temperature is that 700 DEG C of calcination times are that 3 h are placed in tube furnace and are calcined,
Obtain the Ni of vanadium modification3S2Nano-bar array electrode material.
Claims (9)
1. a kind of Ni of vanadium modification3S2Nano-bar array electrode material, which is characterized in that the Ni of the vanadium modification3S2Nanometer rods battle array
Arrange have particles self assemble at squamous surface.
2. a kind of Ni of vanadium modification3S2The preparation method of nano-bar array electrode material, which comprises the following steps:
By metallic nickel be immersed in containing vanadium source, sulphur source, ammonium fluoride suspension in, carry out solvent thermal reaction；Then, by solvent heat
Reaction product carries out vacuum calcining, obtains the Ni of the vanadium modification of nano bar-shape3S2Electrode material.
3. a kind of Ni of vanadium modification according to claim 23S2The preparation method of nano-bar array electrode material, feature
It is, the vanadium source is vanadyl acetylacetonate, sodium metavanadate, sodium vanadate, 12 hydration sodium vanadates, ammonium metavanadate and five oxygen
Change one or more of two vanadium.
4. a kind of Ni of vanadium modification according to claim 23S2The preparation method of nano-bar array electrode material, feature
It is, the sulphur source is one of thiocarbamide, thioacetamide, vulcanized sodium, sodium oiethyl dithiocarbamate and sulphur simple substance
Or it is several.
5. a kind of Ni of vanadium modification according to claim 23S2The preparation method of nano-bar array electrode material, feature
It is, the vanadium source and sulphur source molar ratio are 1:(1 ~ 6)；Vanadium source concentration is 2 ~ 20 mM in the suspension.
6. a kind of Ni of vanadium modification according to claim 23S2The preparation method of nano-bar array electrode material, feature
It is, the solvent thermal reaction, reaction temperature is 50 ~ 200 DEG C, and the reaction time is 0.5 ~ 40 h.
7. a kind of Ni of vanadium modification according to claim 23S2The preparation method of nano-bar array electrode material, feature
It is, the vacuum calcining, calcination temperature is 300 ~ 700 DEG C, and calcination time is 0.5 ~ 4 h.
8. a kind of Ni of vanadium modification according to claim 23S2The preparation method of nano-bar array electrode material, feature
It is, the solvent of the suspension is one or more of ethylenediamine, dehydrated alcohol, methanol or ethylene glycol.
9. according to a kind of described in any item Ni of vanadium modification of claim 2 ~ 83S2The preparation side of nano-bar array electrode material
Method, which is characterized in that specific steps include:
1) metallic nickel is successively immersed in acetone, hydrochloric acid and water and ethyl alcohol and is cleaned by ultrasonic, is then dried in vacuo, concentration of hydrochloric acid
For 1 ~ 5 mol/L；
2) a certain amount of vanadium source, sulphur source are dissolved in the solvent of certain volume, vanadium source and sulphur source molar ratio are 1:(1 ~ 6), make
The vanadium source concentration obtained is 2 ~ 20 mM, stirs 3 ~ 60 min, obtains suspension A；
3) ammonium fluoride of dosage of surfactant is added in suspended A, stirs 1 ~ 2 h, obtains solution B；
4) it by the solution B being stirred and the metallic nickel handled well in step 1), is fitted into autoclave, is subsequently placed in baking oven
Middle carry out solvent thermal reaction；
5) to which after reaction, reaction kettle is cooled down at room temperature, for several times, then product deionized water and ethyl alcohol rinse
It is dried in vacuo；
6) product is calcined in tube furnace under vacuum conditions, obtains the Ni of the vanadium modification of nano bar-shape3S2Electrode material.
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| CN110219014A (en) * | 2019-07-09 | 2019-09-10 | 陕西科技大学 | A kind of V:Ni of squid palpus out shape3S2The preparation method of/NF bifunctional electrodes |
| CN110459745A (en) * | 2019-08-11 | 2019-11-15 | 五邑大学 | A kind of Ni3S2@VO2The preparation method of nanocomposite |
| CN110492069A (en) * | 2019-08-11 | 2019-11-22 | 中山市华舜科技有限责任公司 | Synthetic method of Zn@ metal organic framework composite electrode material |
| CN111330598A (en) * | 2020-04-14 | 2020-06-26 | 陕西科技大学 | Ni3S2NiV-LDH nanosheet electrocatalyst modified by nanospheres and preparation method thereof |
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| CN110219014A (en) * | 2019-07-09 | 2019-09-10 | 陕西科技大学 | A kind of V:Ni of squid palpus out shape3S2The preparation method of/NF bifunctional electrodes |
| CN110459745A (en) * | 2019-08-11 | 2019-11-15 | 五邑大学 | A kind of Ni3S2@VO2The preparation method of nanocomposite |
| CN110492069A (en) * | 2019-08-11 | 2019-11-22 | 中山市华舜科技有限责任公司 | Synthetic method of Zn@ metal organic framework composite electrode material |
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| CN111659421A (en) * | 2020-06-16 | 2020-09-15 | 陕西科技大学 | V-doped Ni3S2Nano-sheet/nano-rod composite structure electrocatalyst and preparation method thereof |
| CN111659421B (en) * | 2020-06-16 | 2022-09-13 | 陕西科技大学 | V-doped Ni 3 S 2 Nano-sheet/nano-rod composite structure electrocatalyst and preparation method thereof |
| CN113058622A (en) * | 2021-03-26 | 2021-07-02 | 安徽大学 | Nickel sulfide/molybdenum disulfide composite nano array for photoelectrocatalysis killing of drug-resistant bacteria and preparation method thereof |
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Application publication date: 20190125 |