CN107324408A - A kind of Ni3S2The synthetic method of micron bar array - Google Patents
A kind of Ni3S2The synthetic method of micron bar array Download PDFInfo
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
A kind of Ni3S2The synthetic method of micron bar array, comprises the following steps：1）Pending nickel foam is cleaned by ultrasonic, fully rinsed, is dried；2）It is 1 to control vanadium source, sulphur source mol ratio:（1~11）, vanadium source and sulphur source are dissolved in appropriate solvent so that vanadium source concentration is 10 ~ 40 mM in resulting solution, is sufficiently stirred for, obtains solution A；3）Solution A is poured into the water heating kettle with polytetrafluoroethyllining lining, by step 1）Water heating kettle is sealed after the nickel foam immersion solution A of pretreatment, solvent thermal reaction is carried out, reaction temperature is 70 ~ 200 DEG C, and the reaction time is 6 ~ 30 h；4）After reaction terminates, reactor is cooled down at room temperature, product is fully rinsed, dried, obtain Ni3S2Micron bar array.The method that the present invention is provided is simple to operate, and reaction condition is gentle, and reaction time is short, the Ni of preparation3S2Product purity is high, and pattern is uniform, and with excellent electrocatalytic hydrogen evolution performance.
Description
Technical field
The invention belongs to electrode material surface processing technology field, and in particular to a kind of Ni3S2The synthesis side of micron bar array
Method.
Background technology
With a large amount of consumption of the non-renewable energy resources such as coal, oil, natural gas, following people endanger the serious energy is faced
Machine.And a kind of cleaning, safety, the reproducible energy are found into current research focus.Hydrogen Energy is carried as a kind of preferable energy
Body, people place high hopes to it.Electrocatalytic decomposition water technology is one of effective way of hydrogen manufacturing, and the key problem of the technology is
Efficient, the cheap water-splitting catalyst of exploitation.At present, noble metal-based catalysts（Such as Pt, Ru or Ir etc.）Be catalytic performance most
Good water-splitting catalyst, but the low shortcoming of expensive, reserves significantly limit the extensive use of such catalyst.
Transient metal sulfide, with rich content, the advantages of with low cost, is that instead of the good of noble metal-based catalysts
Selection.Research shows that Ni base compound materials can effectively improve the reactivity that hydrogen process is produced in water-splitting.Ni3S2Nanostructured is made
It is widely studied, is with a wide range of applications for a kind of efficient production hydrogen catalyst.In addition, by catalyst and conductive substrates
With reference to, can be effectively facilitated electric charge transmission, can significantly strengthen its catalytic activity and stability.
At present, the Ni prepared by methods such as hydro-thermal method, solvent-thermal methods proposed both at home and abroad3S2Material, pattern includes：Sheet,
Flower pattern etc..Chinese invention issued patents the 201610552386.6th disclose a kind of negative electrode of lithium ion battery GO-PANT-Ni3S2
The preparation method of composite, but operating procedure is complicated, and reaction time is longer, technical difficulty is big.Chinese invention bulletin is special
Profit the 201510657154.2nd discloses a kind of Ni of flower pattern3S2The preparation of/graphene three-dimensional combination electrode material, first uses water
Hot method is reacted, then the method for taking tube furnace to calcine obtains a kind of Ni of flower pattern3S2/ graphene three-dimensional combination electrode material,
Severe reaction conditions, and cost is big.Ni3S2nanosheets array supported on Ni foam:A novel ef
cient three-dimensional hydrogen-evolving electrocatalyst in both neutral and
Basic solutions et al. have obtained the Ni of reticular microstructure composition with the method for hydro-thermal3S2Nanometer sheet, but obtained liberation of hydrogen
Overpotential is larger, and catalytic activity is poor.
This patent uses an efficient, simple and inexpensive step solvent-thermal method, is prepared for Ni3S2Micron bar array, effectively
Improve Ni3S2Stability of the material in alkali lye, so as to effectively improve electrolysis water Hydrogen Evolution Performance.
The content of the invention
The present invention is directed to above-mentioned the deficiencies in the prior art, it is therefore intended that propose a kind of Ni3S2The synthesis side of micron bar array
Method.The method that the present invention is provided is simple to operate, and reaction condition is gentle, and reaction time is short, the Ni of preparation3S2Product purity is high, pattern
Uniformly, and with excellent electrocatalytic hydrogen evolution performance.
To achieve these goals, the technical solution adopted in the present invention is：A kind of Ni3S2The synthesis side of micron bar array
Method, comprises the following steps：
（1）Pending nickel foam is soaked into acetone and is cleaned by ultrasonic, then nickel foam is immersed in 2 ~ 4 mol/L hydrochloric acid
It is cleaned by ultrasonic, finally replaces the nickel foam pre-processed after flushing, vacuum drying with deionized water with ethanol respectively；
（2）It is raw material from vanadium source and sulphur source, weighs certain mass, it is 1 with sulphur source mol ratio to control vanadium source:（1~11）, dissolving
In appropriate solvent so that vanadium source concentration be 10 ~ 40 mM, stir 3 ~ 20 min, obtain homogeneous solution A；
（3）The solution A being stirred is poured into the water heating kettle with polytetrafluoroethyllining lining, by step（1）The foam of pretreatment
Sealing after nickel is put into polytetrafluoroethyllining lining, is subsequently placed in homogeneous reaction instrument and reacts；
（4）After reaction terminates, reactor is cooled down at room temperature, product deionized water and ethanol are alternately rinsed for several times, vacuum
Dry, obtain Ni3S2Micron bar array.
Step（1）Described ultrasonic cleaning is 5 ~ 15 min.
Step（1）Described vacuum drying is 5 ~ 15 h of vacuum drying at 20 ~ 40 DEG C.
Step（2）Described vanadium source is sodium metavanadate, sodium vanadate, 12 hydration sodium vanadates, ammonium metavanadate and five oxidations
One or more in two vanadium.
Step（2）Described sulphur source is in thioacetamide, vulcanized sodium, sodium oiethyl dithiocarbamate and sulphur simple substance
One or more.
Step（2）Described solvent is the one or more in deionized water, absolute ethyl alcohol, methanol, ethylene glycol.
Step（3）Described solvent thermal reaction temperature is 70 ~ 200 DEG C, and the reaction time is 6 ~ 30 h.
Step（4）Described vacuum drying is 5 ~ 15 h of vacuum drying at 20 ~ 40 DEG C.
Compared with prior art, the present invention can obtain following beneficial effect：
（1）This method uses a step solvent thermal reaction and directly synthesizes final product, with low synthesis temperature, this method gram
The high shortcoming of traditional method of calcination temperature has been taken, and has not needed large scale equipment and harsh reaction condition, raw material is cheap and easy to get, cost
Low, yield is high, environmentally friendly without post-processing, can be adapted to large-scale production.
（2）Ni prepared by this method3S2Micron bar length forms the micron bar array of rule, micron in foam nickel base
Rod is assembled by nanometer sheet, and the thickness of piece is about in 30 nm or so.What this nanometer sheet was assembled into bar-shaped considerably increases ratio
Surface area, is conducive to electrolyte and Ni3S2The abundant contact of micron bar array.Meanwhile, the unique three-dimensional porous knot of foam nickel base
Structure, improves the transmittability of electric charge.Then its chemical property can be greatly enhanced.
（3）Product chemistry composition prepared by this method is homogeneous, and purity is high, and pattern is uniform, and it is used as electrolysis water electrode material
When can show excellent chemical property, in 10 mA/cm-2Current density under, its overpotential is about 178 mV, and
Under 0.34 V voltage, 5 h stability can be at least kept.
Brief description of the drawings
Fig. 1 is Ni prepared by embodiment 43S2The X-ray diffraction of micron bar array（XRD）Collection of illustrative plates；
Fig. 2 is Ni prepared by embodiment 43S2The ESEM of 500 times of the amplification of micron bar array（SEM）Photo；
Fig. 3 is Ni prepared by embodiment 43S2The ESEM of 3k times of the amplification of micron bar array（SEM）Photo；
Fig. 4 is Ni prepared by embodiment 43S2The ESEM of 150k times of the amplification of micron bar array（SEM）Photo；
Fig. 5 is Ni prepared by embodiment 43S2The linear sweep voltammetry of micron bar array（LSV）Performance test figure.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment is described in further detail to the present invention, but the present invention is not limited to
Following examples.
Embodiment 1
（1）Will（1×5）It is cleaned by ultrasonic 5 min in cm nickel foam immersion acetone soln, nickel foam is immersed in 2 mol/L again
Hydrochloric acid in carry out being cleaned by ultrasonic 5 min, finally replace respectively with ethanol with deionized water and rinsed 3 times, vacuum is dry at 20 DEG C
Nickel foam after being handled after dry 5 h；
（2）12 hydration sodium vanadates and vulcanized sodium are weighed, it is 0.2 mmol to take 12 hydration sodium vanadates, control vanadium source and sulphur source
Mol ratio is 1：1, while being added in 20 ml deionized waters, the min of magnetic agitation 3 obtains homogeneous solution A at room temperature；
（3）The solution A being stirred is poured into the water heating kettle with polytetrafluoroethyllining lining, by step（1）The foam handled well
Sealing after nickel is put into polytetrafluoroethyllining lining, is subsequently placed in homogeneous reaction instrument, and the reaction time is 6 hs at 70 DEG C
It is lower to be reacted；
（4）After reaction terminates, reactor is cooled down at room temperature, product deionized water and ethanol alternately rinse 3 times, then 20
5 h are dried in vacuo at DEG C and obtain Ni3S2Micron bar array.
Embodiment 2
（1）Will（1×5）It is cleaned by ultrasonic 10 min in cm nickel foam immersion acetone soln, nickel foam is immersed in 3 mol/L again
Hydrochloric acid in carry out be cleaned by ultrasonic 15 min, finally respectively with ethanol replace with deionized water rinse 4 times, the vacuum at 20 DEG C
Dry the nickel foam after being handled after 10 h；
（2）Take sodium vanadate and sodium oiethyl dithiocarbamate, sodium vanadate is 0.4 mmol, the mol ratio of vanadium source and sulphur source is 1：
4, while being added in 20 ml ethanol, the min of magnetic agitation 15 obtains homogeneous solution A at room temperature for control；
（3）The solution A being stirred is poured into the water heating kettle with polytetrafluoroethyllining lining, by step（1）The foam handled well
Sealing after nickel is put into polytetrafluoroethyllining lining, is subsequently placed in homogeneous reaction instrument, and the reaction time is 10 h bars at 90 DEG C
Reacted under part；
（4）After reaction terminates, reactor is cooled down at room temperature, product deionized water and ethanol alternately rinse 3 times, then 25
10 h are dried in vacuo at DEG C and obtain Ni3S2Micron bar array.
Embodiment 3
（1）Will（1×5）It is cleaned by ultrasonic 10 min in cm nickel foam immersion acetone soln, nickel foam is immersed in 3 mol/L again
Hydrochloric acid in carry out be cleaned by ultrasonic 15 min, finally respectively with ethanol replace with deionized water rinse 4 times, the vacuum at 25 DEG C
Dry the nickel foam after being handled after 10 h；
（2）Ammonium metavanadate and sulphur simple substance are taken, ammonium metavanadate is 0.8mmol, the mol ratio for controlling vanadium source and sulphur source is 1：6, simultaneously
In the methanol solvate for being added to 20 ml, the min of magnetic agitation 15 obtains homogeneous solution A at room temperature；
（3）The solution A being stirred is poured into the water heating kettle with polytetrafluoroethyllining lining, by step（1）The foam handled well
Sealing after nickel is put into polytetrafluoroethyllining lining, is subsequently placed in homogeneous reaction instrument, and the reaction time is 24 h at 120 DEG C
Under the conditions of reacted；
（4）After reaction terminates, reactor is cooled down at room temperature, product deionized water and ethanol alternately rinse 3 times, then 25
10 h are dried in vacuo at DEG C and obtain Ni3S2Micron bar array.
Embodiment 4
（1）Will（1×5）It is cleaned by ultrasonic 10 min in cm nickel foam immersion acetone soln, nickel foam is immersed in 3 mol/L again
Hydrochloric acid in carry out be cleaned by ultrasonic 15 min, finally respectively with ethanol replace with deionized water rinse 4 times, the vacuum at 30 DEG C
Dry the nickel foam after being handled after 15 h；
（2）Sodium metavanadate and thioacetamide are taken, sodium metavanadate is 0.6 mmol, the mol ratio for controlling vanadium source and sulphur source is 1：9,
It is added to simultaneously in 30 ml deionized water and alcohol mixed solvent, the min of magnetic agitation 15 obtains homogeneous solution at room temperature
A；
（3）The solution A being stirred is poured into the water heating kettle with polytetrafluoroethyllining lining, by step（1）The foam handled well
Sealing after nickel is put into polytetrafluoroethyllining lining, is subsequently placed in homogeneous reaction instrument, and the reaction time is 10 h at 180 DEG C
Under the conditions of reacted；
（4）After reaction terminates, reactor is cooled down at room temperature, product deionized water and ethanol alternately rinse 3 times, then 30
10 h are dried in vacuo at DEG C and obtain Ni3S2Micron bar array.
Fig. 1 is Ni manufactured in the present embodiment3S2The XRD spectrum of micron bar array, as can be seen from Figure 1 x-ray powder spread out
Penetrate peak can index be Ni3S2, and almost occur without other impurities peak, therefore the high purity N i that embodiment 4 has been synthesized3S2。
Fig. 2 ~ 4 are Ni manufactured in the present embodiment3S2SEM photograph of the micron bar array under different amplification, from Fig. 2's
The pattern of the SEM it can be seen from the figure thats sample is the micron bar array being grown in nickel foam.
Fig. 5 is Ni manufactured in the present embodiment3S2Micron bar array LSV performance curves, from Fig. 3 linear sweep voltammetry figure
As can be seen that the sample is 10 mA/cm in current density2When, it is 178 mV with low overpotential, and in 0.34 V electricity
Pressure, can at least keep 5 h stability.Show with efficient electrocatalytic hydrogen evolution activity.
Embodiment 5
（1）Will（1×5）It is cleaned by ultrasonic 15 min in cm nickel foam immersion acetone soln, nickel foam is immersed in 4 mol/L again
Hydrochloric acid in carry out ultrasonic cleaning 10min, finally replace respectively with ethanol with deionized water and rinsed 4 times, vacuum is dry at 40 DEG C
Nickel foam after being handled after dry 15 h；
（2）Vanadic anhydride and thioacetamide are taken, vanadic anhydride is 0.8 mmol, and the mol ratio for controlling vanadium source and sulphur source is
1：11, while being added in 40 ml ethylene glycol solvent, the min of magnetic agitation 20 obtains homogeneous solution A at room temperature；
（3）The solution A being stirred is poured into the water heating kettle with polytetrafluoroethyllining lining, by step（1）The foam handled well
Sealing after nickel is put into polytetrafluoroethyllining lining, is subsequently placed in homogeneous reaction instrument, and the reaction time is 30 h at 200 DEG C
Under the conditions of reacted；
（4）After reaction terminates, reactor is cooled down at room temperature, product deionized water and ethanol alternately rinse 3 times, then 40
15 h are dried in vacuo at DEG C and obtain Ni3S2Micron bar array.
Claims (9)
1. a kind of Ni3S2The synthetic method of micron bar array, it is characterised in that comprise the following steps：
（1）Pending nickel foam is cleaned by ultrasonic, fully rinsed, is dried, the nickel foam pre-processed；
（2）It is 1 to control vanadium source, sulphur source mol ratio:（1~11）, vanadium source and sulphur source are dissolved in appropriate solvent so that institute
It is 10 ~ 40 mM to obtain vanadium source concentration in solution, is sufficiently stirred for, obtains solution A；
（3）The solution A being stirred is poured into the water heating kettle with polytetrafluoroethyllining lining, by step（1）The foam of pretreatment
Water heating kettle is sealed after nickel immersion solution A, solvent thermal reaction is then carried out, reaction temperature is 70 ~ 200 DEG C, and the reaction time is 6 ~ 30
h；
（4）After reaction terminates, product is fully rinsed in cooling, is dried, is obtained Ni3S2Micron bar array.
2. a kind of Ni according to claim 13S2The synthetic method of micron bar array, it is characterised in that the step（1）
Ultrasonic cleaning, nickel foam is first soaked in organic solvent for ultrasonic cleaning, then that nickel foam is soaked in pickle into ultrasound is clear
Wash.
3. a kind of Ni according to claim 23S2The synthetic method of micron bar array, it is characterised in that the step（1）
Ultrasonic cleaning, the organic solvent used for acetone, pickle be 2 ~ 4 mol/L hydrochloric acid, 5 ~ 15min of ultrasonic time.
4. a kind of Ni according to claim 13S2The synthetic method of micron bar array, it is characterised in that the step（1）、
Step（4）In abundant flushing, flushing is replaced with deionized water using alcohols solvent.
5. a kind of Ni according to claim 13S2The synthetic method of micron bar array, it is characterised in that the step（1）、
Step（4）In drying, drying condition be 20 ~ 40 DEG C at be dried in vacuo 5 ~ 15 h.
6. a kind of Ni according to claim 13S2The synthetic method of micron bar array, it is characterised in that the vanadium source is inclined
One or more in sodium vanadate, sodium vanadate, 12 hydration sodium vanadates, ammonium metavanadate and vanadic anhydride.
7. a kind of Ni according to claim 13S2The synthetic method of micron bar array, it is characterised in that the sulphur source is sulphur
For the one or more in acetamide, vulcanized sodium, sodium oiethyl dithiocarbamate and sulphur simple substance.
8. a kind of Ni according to claim 13S2The synthetic method of micron bar array, it is characterised in that the step（2）
In solvent be deionized water, absolute ethyl alcohol, methanol, ethylene glycol in one or more.
9. a kind of Ni according to claim 13S2The synthetic method of micron bar array, it is characterised in that the step（3）
Reaction unit be homogeneous reaction instrument.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325539A (en) * | 2018-03-15 | 2018-07-27 | 陕西科技大学 | A kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2The synthetic method of elctro-catalyst |
| CN109055972A (en) * | 2018-07-20 | 2018-12-21 | 曲阜师范大学 | Mn adulterates Ni3S2Nano-array liberation of hydrogen catalyst and its preparation method and application |
| CN109136886A (en) * | 2018-10-17 | 2019-01-04 | 中国石油大学(华东) | One kind preparing Ni in pure nickel plate surface3S2The method of super-hydrophobic coat |
| CN109225270A (en) * | 2018-09-30 | 2019-01-18 | 陕西科技大学 | A kind of Ni3S2@NiV-LDH heterojunction structure bifunctional electrocatalyst, Preparation method and use |
| CN109267089A (en) * | 2018-09-30 | 2019-01-25 | 陕西科技大学 | A kind of Ni of the V doping of nanoforest shape3S2/ NF self-supporting electrode and preparation method thereof |
| CN109261168A (en) * | 2018-10-16 | 2019-01-25 | 陕西科技大学 | A kind of Ni of vanadium modification3S2Nano-bar array electrode material and preparation method thereof |
| CN109280933A (en) * | 2018-09-28 | 2019-01-29 | 陕西科技大学 | A kind of NiV2S4Elctro-catalyst and preparation method thereof |
| CN109628951A (en) * | 2018-10-31 | 2019-04-16 | 中山大学 | A kind of nickel sulfide Electrocatalytic Activity for Hydrogen Evolution Reaction agent and the preparation method and application thereof |
| CN110459745A (en) * | 2019-08-11 | 2019-11-15 | 五邑大学 | A kind of Ni3S2@VO2The preparation method of nanocomposite |
| CN110656349A (en) * | 2019-09-29 | 2020-01-07 | 安徽师范大学 | Fe-doped nickel oxalate nanorod growing in situ on foamed nickel, preparation method and application thereof |
| 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 |
| CN111468140A (en) * | 2020-06-02 | 2020-07-31 | 陕西科技大学 | Ni3S2Preparation method of NiV-L DH heterogeneous nanocone electrocatalyst |
| CN112279315A (en) * | 2019-07-23 | 2021-01-29 | 湖北大学 | Environment-friendly nickel sulfide array material and preparation method thereof |
| CN113026052A (en) * | 2021-03-25 | 2021-06-25 | 台州学院 | Acicular Se-doped Ni3S2And method for preparing the same |
| CN114551908A (en) * | 2022-01-25 | 2022-05-27 | 东风汽车集团股份有限公司 | Preparation method of gas diffusion layer with anti-bipolar capability |
| CN114807956A (en) * | 2022-04-11 | 2022-07-29 | 西南石油大学 | Preparation method of in-situ growth nano array catalyst applied to hydrogen sulfide hydrogen production |
-
2017
- 2017-08-16 CN CN201710700020.3A patent/CN107324408A/en active Pending
Non-Patent Citations (5)
| Title |
|---|
| BIN YANG ET AL.: "The growth and assembly of the multidimensional hierarchical Ni3S2 for aqueous asymmetric supercapacitors", 《CRYSTENGCOMM》 * |
| CANBIN OUYANG ET AL.: "Hierarchically Porous Ni3S2 Nanorod Array Foam as Highly Efficient Electrocatalyst for Hydrogen Evolution Reaction and Oxygen Evolution Reaction", 《ELECTROCHIMICA ACTA》 * |
| JUN SONG CHEN ET AL.: "Self-supported phase-pure Ni3S2 sheet-on-rod nanoarrays with enhanced pseudocapacitive properties and high energy density", 《JOURNAL OF POWER SOURCES》 * |
| XIONGWEI ZHONG ET AL.: "Efficient coupling of a hierarchical V2O5@Ni3S2 hybrid nanoarray for pseudocapacitors and hydrogen production", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| YUANJU QU ET AL.: "Facile Synthesis of Vanadium-Doped Ni3S2 Nanowire Arrays as Active Electrocatalyst for Hydrogen Evolution Reaction", 《ACS APPL. MATER. INTERFACES》 * |
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