CN109225270A - A kind of Ni3S2@NiV-LDH heterojunction structure bifunctional electrocatalyst, Preparation method and use - Google Patents
A kind of Ni3S2@NiV-LDH heterojunction structure bifunctional electrocatalyst, Preparation method and use Download PDFInfo
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Abstract
The present invention provides a kind of Ni3S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst: clean conducting base is immersed in NiV-LDH precursor solution, hydro-thermal reaction obtains NiV-LDH/NF nano-chip arrays；NiV-LDH/NF nano-chip arrays are immersed in the homogeneous solution containing sulphur source, hydro-thermal reaction obtains Ni3S2@NiV-LDH heterojunction structure bifunctional electrocatalyst.The present invention also provides this Ni3S2@NiV-LDH heterojunction structure bifunctional electrocatalyst.The present invention directly prepares electrode material, avoids the active site for enabling material sufficiently expose its surface using binder, while solving the problems, such as that existing elctro-catalyst can not show excellent properties and stability on OER and HER simultaneously.
Description
Technical field
The invention belongs to elctro-catalyst technical fields, and in particular to a kind of Ni3S2The difunctional electro-catalysis of@NiV-LDH heterojunction structure
Agent, Preparation method and use.
Background technique
The exhaustion of traditional fossil energy and being on the rise for problem of environmental pollution force people to seek a kind of novel alternative
The energy.Hydrogen Energy be it is a kind of cleaning, efficiently, non-polluting energy sources.In view of the reserves of water on the earth are extremely abundant, water decomposition generates hydrogen
Gas and oxygen, therefore water electrolysis hydrogen production oxygenerating technology has been favored by people.Electrolysis water process is divided into two half-reactions: liberation of hydrogen is anti-
Should and oxygen evolution reaction, metal oxide containing precious metals (IrO2、RuO2) and precious metals pt be considered as that most effective water decomposition OER and HER is urged
Agent, but their expensive prices and less reserves constrain and produce and be widely applied on a large scale.
Recently, layered double hydroxide (abbreviation LDH) is a kind of material with special layer structure, solely due to it
The interchangeability of anion between the Modulatory character and laminate of special two-dimensional layered structure, laminate element composition and content, in OER
Attract attention and apply, but its HER performance it is poor or almost without, and during the test powder sample be easy curling, lead
Its performance is caused to be affected, Ni3S2It is a kind of metallic state sulfide, there is good electric conductivity, introduces Ni3S2Nano material energy
Enough improve the electric conductivity of material.
This patent uses efficient, simple and inexpensive hydro-thermal method, is prepared for Ni3S2@NiV-LDH heterojunction structure electrode material
Material, effectively raises the aqueous energy of electro-catalysis complete solution of material.
Summary of the invention
Present invention introduces conducting bases, directly prepare electrode material, avoid enabling material sufficiently to expose using binder
The active site on its surface, while solving existing elctro-catalyst and can not show excellent properties and steady on OER and HER simultaneously
Qualitative problem proposes a kind of Ni3S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst.
(1) conducting base is immersed in acetone soln and is cleaned by ultrasonic 5 ~ 20min, is then transferred in the hydrochloric acid of 2 ~ 4mol/L
5 ~ 20min of ultrasonic cleaning is carried out, finally replaces flushing 2 ~ 3 times with ultrapure water with ethyl alcohol respectively, then be dried in vacuo at 25 ~ 35 DEG C
10~14h；
(2) precursor solution, the nickel salt for being (0.05 ~ 0.2) mol/L comprising concentration in the precursor solution are configured, concentration is
The vanadic salts of (0.0125 ~ 0.1) mol/L, the ammonium fluoride and concentration that concentration is (0.01 ~ 0.1) mol/L are (0.125 ~ 0.35) mol/
The aqueous solution of the urea of L, 20 ~ 40min of magnetic agitation obtains clear solution A at room temperature.At clear solution A and step (1)
The conducting base managed is transferred in high temperature and pressure hydro-thermal kettle, 6 ~ 18h is then reacted at 90 ~ 150 DEG C, wherein reaction-filling ratio is answered
The control is 20 ~ 80%.Hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, the conducting base that then will be cooled down after reaction
It takes out, collects product after 3 washings and 3 alcohol are alternately cleaned, and at 25 ~ 35 DEG C, be dried in vacuo 3 ~ 5h.
(3) suitable thioacetamide (TAA) is weighed to be added in the deionized water of 20 ~ 40ml, at this time the concentration of TAA be (1 ~
2) mol/l, then the conducting base by step (2) after dry and TAA solution are transferred to together in high temperature and pressure hydro-thermal kettle, then
0.5 ~ 2h is reacted at 100 ~ 200 DEG C, wherein reaction-filling ratio should be controlled 20 ~ 80%.
The conducting base of the step (1) is any one of nickel foam or carbon cloth.
It is Nickelous nitrate hexahydrate, six hydration nickel sulfate or Nickel dichloride hexahydrate that the nickel salt of the step (2), which is the nickel source,
One of.
The vanadic salts of the step (2) is vanadium chloride.
Beneficial effect of the invention are as follows:
(1) Ni that the present invention prepares3S2@NiV-LDH heterojunction structure is completed by simple hydro-thermal reaction, and step is simple, instead
Short between seasonable, environmentally friendly, repeatability is strong.
(2) Ni proposed by the present invention3S2The preparation method of@NiV-LDH composite construction, grows nanometer sheet on conducting base
Array structure is directly prepared into electrode material, can be directly used for electrocatalysis characteristic test.
Detailed description of the invention
Fig. 1 is Ni prepared by the embodiment of the present invention 53S2X-ray diffraction (XRD) map of@NiV-LDH/NF composite construction；
Fig. 2 is Ni prepared by the embodiment of the present invention 53S2Scanning electron microscope (SEM) photo of@NiV-LDH/NF composite construction；
Fig. 3 is Ni prepared by the embodiment of the present invention 53S2Transmission electron microscope (TEM) photo of@NiV-LDH/NF composite construction；
Fig. 4 is Ni prepared by the embodiment of the present invention 53S2The HER performance map of@NiV-LDH/NF composite material；
Fig. 5 is Ni prepared by the embodiment of the present invention 53S2The OER performance map of@NiV-LDH/NF composite material.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the invention will be described in further detail:
Embodiment 1:
Conducting base is nickel foam, and nickel salt is Nickelous nitrate hexahydrate.
(1) conducting base is immersed in acetone soln and is cleaned by ultrasonic 10min, is then transferred in the hydrochloric acid of 2mol/L and carries out
It is cleaned by ultrasonic 10min, finally replaces flushing 3 times with ultrapure water with ethyl alcohol respectively, then be dried in vacuo 10h at 35 DEG C；
(2) precursor solution, the Nickelous nitrate hexahydrate for being 0.05mol/L comprising concentration in the precursor solution are configured, concentration is
The vanadium chloride of 0.0125mol/L, ammonium fluoride and concentration that concentration is 0.05mol/L are the aqueous solution of the 0.125) urea of mol/L,
Magnetic agitation 20min obtains clear solution A at room temperature.Clear solution A and step (1) conducting base handled well are transferred to height
In warm high pressure water heating kettle, 18h is then reacted at 100 DEG C, wherein reaction-filling ratio should be controlled 40%.Hydro-thermal reaction terminates,
Reaction kettle is naturally cooled into room temperature, then takes out the conducting base cooled down after reaction, by 3 washings and 3 alcohol alternatings
Product is collected after cleaning, and at 35 DEG C, be dried in vacuo 3h.
(3) suitable thioacetamide (TAA) is weighed to be added in the deionized water of 20ml, the concentration of TAA is 2mol/l at this time,
Then the conducting base by step (2) after dry and TAA solution are transferred to together in high temperature and pressure hydro-thermal kettle, then at 100 DEG C
Lower reaction 2h, wherein reaction-filling ratio should be controlled 40%.
Embodiment 2:
Conducting base is nickel foam, and nickel salt is Nickelous nitrate hexahydrate.
(1) nickel foam of 1cm x 5cm is immersed in acetone soln and is cleaned by ultrasonic 10min, is then transferred to 2mol/L's
Ultrasonic cleaning 10min is carried out in hydrochloric acid, finally replaces flushing 3 times with ultrapure water with ethyl alcohol respectively, then be dried in vacuo at 35 DEG C
10h；
(2) precursor solution, the Nickelous nitrate hexahydrate for being 0.1mol/L comprising concentration in the precursor solution are configured, concentration is
The vanadium chloride of 0.04mol/L, the aqueous solution for the urea that the ammonium fluoride and concentration that concentration is 0.05mol/L are 0.2mol/L, in room
The lower magnetic agitation 20min of temperature obtains clear solution A.Clear solution A and step (1) conducting base handled well are transferred to high temperature height
It presses in water heating kettle, 14h is then reacted at 120 DEG C, wherein reaction-filling ratio should be controlled 40%.Hydro-thermal reaction terminates, will be anti-
It answers kettle to naturally cool to room temperature, then takes out the conducting base cooled down after reaction, alternately cleaned by 3 washings and 3 alcohol
After collect product, and at 35 DEG C, be dried in vacuo 3h.
(3) suitable thioacetamide (TAA) is weighed to be added in the deionized water of 30ml, the concentration of TAA is 2mol/l at this time,
Then the conducting base by step (2) after dry and TAA solution are transferred to together in high temperature and pressure hydro-thermal kettle, then at 120 DEG C
Lower reaction 1h, wherein reaction-filling ratio should be controlled 60%.
Embodiment 3:
Conducting base is nickel foam, and nickel salt is Nickel dichloride hexahydrate.
(1) nickel foam of 1cm x 5cm is immersed in acetone soln and is cleaned by ultrasonic 5min, is again immersed in nickel foam
Ultrasonic cleaning 5min is carried out in the hydrochloric acid of 2mol/L, finally replaces flushing 3 times, the vacuum at 30 DEG C with ultrapure water with ethyl alcohol respectively
The nickel foam that obtains that treated after dry 10；
(2) precursor solution, the Nickel dichloride hexahydrate for being 0.1mol/L comprising concentration in the precursor solution are configured, concentration is
The vanadium chloride of 0.05mol/L, the aqueous solution for the urea that the ammonium fluoride and concentration that concentration is 0.05mol/L are 0.2mol/L, in room
The lower magnetic agitation 20min of temperature obtains clear solution A.Clear solution A and step (1) nickel foam handled well are transferred to high temperature and pressure
In water heating kettle, 10h is then reacted at 140 DEG C, wherein reaction-filling ratio should be controlled 30%.Hydro-thermal reaction terminates, and will react
Kettle naturally cools to room temperature, then takes out the conducting base cooled down after reaction, after 3 washings and 3 alcohol are alternately cleaned
Product is collected, and at 35 DEG C, is dried in vacuo 3h.
(3) suitable thioacetamide (TAA) is weighed to be added in the deionized water of 30ml, the concentration of TAA is 2mol/l at this time,
Then the conducting base by step (2) after dry and TAA solution are transferred to together in high temperature and pressure hydro-thermal kettle, then at 140 DEG C
Lower reaction 0.5h, wherein reaction-filling ratio should be controlled 60%.
Embodiment 4:
Conducting base is nickel foam, and nickel salt is six hydration nickel sulfate.
(1) nickel foam of 1cm x 5cm is immersed in acetone soln and is cleaned by ultrasonic 5min, is again immersed in nickel foam
Ultrasonic cleaning 5min is carried out in the hydrochloric acid of 2mol/L, finally replaces flushing 3 times, the vacuum at 30 DEG C with ultrapure water with ethyl alcohol respectively
The nickel foam that obtains that treated after dry 10；
(2) precursor solution, the six hydration nickel sulfate for being 0.1167mol/L comprising concentration in the precursor solution, concentration are configured
For the vanadium chloride of 0.067mol/L, the urea that the ammonium fluoride and concentration that concentration is 0.05mol/L are 0.2167mol/L it is water-soluble
Liquid, magnetic agitation 20min obtains clear solution A at room temperature.Clear solution A and step (1) nickel foam handled well are transferred to
In high temperature and pressure hydro-thermal kettle, 15h is then reacted at 150 DEG C, wherein reaction-filling ratio should be controlled 40%.Hydro-thermal reaction knot
Reaction kettle is naturally cooled to room temperature by beam, then takes out the conducting base cooled down after reaction, is handed over by 3 washings and 3 alcohol
For collecting product after cleaning, and at 35 DEG C, it is dried in vacuo 3h.
(3) it weighs suitable TAA to be added in the deionized water of 20ml, the concentration of TAA is 2mol/l at this time, then by step 2
The NiV-LDH/NF nano-chip arrays and TAA solution prepared are transferred to together in high temperature and pressure hydro-thermal kettle, then at 100 DEG C
2h is reacted, wherein reaction-filling ratio should be controlled 40%.
Embodiment 5:
Conducting base is nickel foam, and nickel salt is Nickel dichloride hexahydrate.
(1) nickel foam of 1cm x 5cm is immersed in acetone soln and is cleaned by ultrasonic 5min, is again immersed in nickel foam
Ultrasonic cleaning 5min is carried out in the hydrochloric acid of 2mol/L, finally replaces flushing 3 times, the vacuum at 30 DEG C with ultrapure water with ethyl alcohol respectively
The nickel foam that obtains that treated after dry 10；
(2) precursor solution, the Nickel dichloride hexahydrate for being 0.1mol/L comprising concentration in the precursor solution are configured, concentration is
The vanadium chloride of 0.025mol/L, the aqueous solution for the urea that the ammonium fluoride and concentration that concentration is 0.05mol/L are 0.25mol/L,
Magnetic agitation 20min obtains clear solution A at room temperature.Clear solution A and step (1) nickel foam handled well are transferred to high temperature height
It presses in water heating kettle, 10h is then reacted at 150 DEG C, wherein reaction-filling ratio should be controlled 40%.Hydro-thermal reaction terminates, will be anti-
It answers kettle to naturally cool to room temperature, then takes out the conducting base cooled down after reaction, alternately cleaned by 3 washings and 3 alcohol
After collect product, and at 35 DEG C, be dried in vacuo 3h.
(3) it weighs suitable TAA to be added in the deionized water of 20ml, the concentration of TAA is 2mol/l at this time, then by step 2
The NiV-LDH/NF nano-chip arrays and TAA solution prepared are transferred to together in high temperature and pressure hydro-thermal kettle, then at 160 DEG C
0.5h is reacted, wherein reaction-filling ratio should be controlled 40%.
Fig. 1 is Ni manufactured in the present embodiment3S2X-ray diffraction (XRD) map of@NiV-LDH/NF composite construction.This reality
It applies in a characteristic peak for product X RD map and nickel foam, Ni occurs3S2And the characteristic peak of NiV-LDH, illustrate to have obtained target production
Object.
Fig. 2 is Ni manufactured in the present embodiment3S2Scanning electron microscope (SEM) photo of@NiV-LDH/NF composite construction.Photo is aobvious
Show, foam nickel surface has grown the array structure being stacked by nanometer sheet.
Fig. 3 is Ni manufactured in the present embodiment3S2Transmission electron microscope (TEM) photo of@NiV-LDH/NF composite construction.Photo is aobvious
Show, nano particle is embedded in nanometer sheet.
Fig. 4 is Ni manufactured in the present embodiment3S2The HER performance map of@NiV-LDH/NF composite material.Fig. 4 shows the composite wood
Material has good electrocatalytic hydrogen evolution performance, is 10mA/cm in current density2When, overpotential 200mV.
Fig. 5 is Ni manufactured in the present embodiment3S2The OER performance map of@NiV-LDH/NF composite material.Fig. 5 shows the composite wood
There is material good electro-catalysis to analyse oxygen performance, be 50mA/cm in current density2When, overpotential 350mV.
Claims (10)
1. a kind of Ni3S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst, which is characterized in that including walking as follows
It is rapid:
Clean conducting base is immersed in NiV-LDH precursor solution, hydro-thermal reaction obtains NiV-LDH/NF nanometer sheet battle array
Column；NiV-LDH/NF nano-chip arrays are immersed in the homogeneous solution containing sulphur source, hydro-thermal reaction obtains Ni3S2@NiV-LDH
Heterojunction structure bifunctional electrocatalyst.
2. a kind of Ni according to claim 13S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst,
Be characterized in that, the NiV-LDH precursor solution be comprising concentration be 0.05 ~ 0.2mol/L nickel source, 0.0125 ~ 0.1mol/
The aqueous solution of the urea in the vanadium source of L, 0.01 ~ 0.1mol/L ammonium fluoride and 0.125 ~ 0.35mol/L.
3. a kind of Ni according to claim 23S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst,
It is characterized in that, the nickel source is one of Nickelous nitrate hexahydrate, six hydration nickel sulfate or Nickel dichloride hexahydrate.
4. a kind of Ni according to claim 23S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst,
It is characterized in that, the vanadium source is vanadium chloride.
5. a kind of Ni according to claim 13S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst,
It is characterized in that, the conducting base is nickel foam or carbon cloth.
6. a kind of Ni according to claim 13S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst,
It is characterized in that, the sulphur source is thioacetamide TAA.
7. a kind of Ni according to claim 13S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst,
Be characterized in that, prepare the hydro-thermal reaction of NiV-LDH/NF nano-chip arrays reaction temperature be 90 ~ 150 DEG C, the reaction time be 6 ~
18h, reaction-filling is than control 20 ~ 80%；The reaction temperature of sulphur source and the hydro-thermal reaction of NiV-LDH/NF nano-chip arrays is
100 ~ 200 DEG C, the reaction time is 0.5 ~ 2h, and reaction-filling is than control 20 ~ 80%.
8. a kind of Ni according to claim 13S2The preparation method of@NiV-LDH heterojunction structure bifunctional electrocatalyst,
It is characterized in that, specific steps include:
1) conducting base is immersed in acetone soln and is cleaned by ultrasonic 5 ~ 20min, is then transferred in the hydrochloric acid of 2 ~ 4mol/L and carries out
Be cleaned by ultrasonic 5 ~ 20min, finally respectively with ethyl alcohol replace with ultrapure water rinse 2 ~ 3 times, then at 25 ~ 35 DEG C be dried in vacuo 10 ~
14h；
2) precursor solution, the nickel salt for being 0.05 ~ 0.2mol/L comprising concentration in the precursor solution, concentration 0.0125 are configured
The vanadic salts of ~ 0.1mol/L, the water for the urea that the ammonium fluoride and concentration that concentration is 0.01 ~ 0.1mol/L are 0.125 ~ 0.35mol/L
Solution, 20 ~ 40min of magnetic agitation obtains clear solution A at room temperature；The conductive base that clear solution A and step 1) are handled well
Body is transferred in high temperature and pressure hydro-thermal kettle, and 6 ~ 18h is then reacted at 90 ~ 150 DEG C, wherein reaction-filling ratio should control 20 ~
80%；Hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes out the conducting base cooled down after reaction, by 3
Secondary washing and 3 alcohol collect product after alternately cleaning, and at 25 ~ 35 DEG C, are dried in vacuo 3 ~ 5h；
3) it weighs suitable thioacetamide TAA to be added in the deionized water of 20 ~ 40ml, the concentration of TAA is 1 ~ 2mol/ at this time
L, then the conducting base by step 2 after dry and TAA solution are transferred to together in high temperature and pressure hydro-thermal kettle, then 100 ~
0.5 ~ 2h is reacted at 200 DEG C, wherein reaction-filling ratio should be controlled 20 ~ 80%.
9. a kind of Ni of any one of claim 1 ~ 8 the method preparation3S2@NiV-LDH heterojunction structure bifunctional electrocatalyst.
10. a kind of Ni as claimed in claim 93S2@NiV-LDH heterojunction structure bifunctional electrocatalyst is as electro-catalysis complete solution water
Catalyst purposes.
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