CN109772367A - A kind of preparation method of fabricated in situ transition metal oxide-Ni-based sulfide composite material - Google Patents
A kind of preparation method of fabricated in situ transition metal oxide-Ni-based sulfide composite material Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of fabricated in situ transition metal oxide-Ni-based sulfide composite material, and key step includes: In-situ sulphiding more empty nickel foam synthesis Ni3S2- NF and fabricated in situ CeO2/Ni3S2- NF composite material.Second step specifically includes: Ni3S2- NF material is placed in the water heating kettle of 40ml stand-by with ethyl alcohol cleaning-drying；15ml ethyl alcohol is measured, the six nitric hydrate ceriums of 0.011g, the methenamine of 0.021g is weighed, is placed in the beaker of 50ml, stirring 2h obtains as clear as crystal solution；Obtained solution is poured into containing Ni3S2It in the water heating kettle of-NF material, is sealed and placed in hydro-thermal case after 30min is stirred at room temperature, takes out cooled to room temperature after water heating kettle after keeping 160 DEG C of at least 6h of temperature；It is placed on vacuum drying oven drying by the washing of obtained material 3 times, finally in sheet Ni3S2Upper original position load C eO2Nano particle obtains CeO2/Ni3S2- NF composite material.CeO prepared by the present invention2/Ni3S2- NF heterojunction structure catalysis material, with single Ni3S2、CeO2And nickel foam is compared, which there is excellent electro-catalysis to hydrolyze Hydrogen Evolution Performance.
Description
Technical field
The invention belongs to the preparation technical fields of nano electro-catalytic hydrolyzed material, and in particular to one kind is in three-dimensional porous foams
Fabricated in situ CeO on nickel2/Ni3S2The preparation method of composite material.
Background technique
With the continuous development of human society, then bring is that traditional fossil energy consumption increasingly increases, due to these
The non-renewable and its combustion product of the energy can cause very big pollution and destruction to environment, so a kind of cleaning of demand can be again
Raw high efficient energy sources become human society and continue to develop faced a major challenge.Hydrogen is as a kind of new energy, because of its energy
Metric density is high, combustion product is pollution-free and it is recyclable the advantages that, be considered potential and replace traditional fossil energy.At present
The method of hydrogen making is mainly the steam reformation of methane in industry, and the byproducts such as carbon dioxide are had in such hydrogen production process
Generation, keep the hydrogen purity finally obtained lower, in addition, raw material used in the process is still non-renewable fossil energy
Therefore other cleanings, efficient method if hydrogen will realize large-scale production and application as a kind of new energy, are sought in source
It is highly desirable.Being electrolysed aquatic products hydrogen is considered as one of optimal production hydrogen mode, and electrolysis aquatic products hydrogen is in current industrial technology
It is carried out in highly developed proton exchange membrane electrolysis cells, outside in alive situation, anode is happens is that oxygen evolution reaction, phase
The cathode answered is happens is that hydrogen evolution reaction, and the hydrogen purity of generation is high, and its raw material is the most abundant water of global content, but
Be electrolysis water it is thermodynamically non-spontaneous process, needs applied voltage to do work so that such process carries out, in order to enable
Energy needed for electro-catalysis hydrolyzes and solar battery efficiency matching, need to reduce the activation of reaction using catalyst in cathode
Can, to reduce required energy consumption and then improve the rate of entire reaction system.Generally acknowledged at present hydrolyzing for electro-catalysis produces hydrogen activity
Best catalysis material is transition metal platinum, but the global reserves of metal platinum are very limited, and price is extremely expensive so that its big rule
Mould application is restricted, therefore the electrolysis water catalysis material for finding high efficiency low cost is very important.
Lot of documents shows that researcher is concentrated mainly on the means for improving electrocatalysis characteristic: (1) improving catalysis material
The specific surface area of material makes the active site quantity of unit area increase sharply.(2) metal, nonmetal doping are to main catalytic material
It is modified to carry out surface.(3) Composite of heterogeneous material carries out interface regulation, to realize the synergistic effect between component, improves material
The intrinsic catalytic activity of material.
Compound previously mentioned heterogeneous material is a kind of a kind of means for extremely effective improving electro-catalysis hydrolysis and producing hydrogen, we
The cerium oxide nanoparticles being evenly distributed using the method for solvent heat in three nickel surface growth in situ of sheet curing.A large amount of texts
It offers and shows effectively modify ceria to the surface of the compounds such as Transition Metal Sulfur, phosphorus by method in situ, but
It is that usually used solvent thermal process technique is cumbersome and will use the virose raw material of tool in the process or generate toxic products, therefore
We need the method for finding more simple and safe green to load to cerium oxide in situ above three nickel of curing.In addition, comparing
For traditional dipping calcined materials Composite, combining between the heterojunction structure component of fabricated in situ would generally be even closer, therefore
The effective time of material can be longer, and stability can be more preferable.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, provide a kind of fabricated in situ transition metal oxide/nickel
The preparation method of base sulfide composite material.
The present invention is the technical problem solved in background technique, the technical solution adopted is that a kind of fabricated in situ transition metal
Oxide/Ni-based sulfide composite material preparation method, includes the following steps:
1) In-situ sulphiding more empty nickel foams synthesize Ni3S2-NF
(1) it handles nickel foam: being 1x3cm by area2Nickel foam (NF) respectively use acetone and each ultrasound of 3M HCl
10min is cleaned with deionized water and ethyl alcohol respectively later, is then evaporated in 60 DEG C of vacuum tank stand-by；
(2) thiourea solution of 1.45mM is prepared, nickel foam is placed in 40mL water heating kettle by treated in step (1), together
When the prepared thiourea solution of 10ml is added, sealing water heating kettle is placed in hydro-thermal case, is kept for 150 DEG C, taken out after 4-8h
Natural cooling, the nickel foam after taking out vulcanization are cleaned with deionized water and ethyl alcohol, and the sample after cleaning is placed in 60 DEG C of vacuum
It is evaporated to obtain Ni in baking oven3S2-NF；
2) fabricated in situ CeO2/Ni3S2- NF composite material
(1) taking area is 1x1.5cm2The obtained Ni of the step 1)3S2- NF material is placed on ethyl alcohol cleaning-drying
It is stand-by in the water heating kettle of 40ml；
(2) 15ml ethyl alcohol is measured, the six nitric hydrate ceriums of 0.011g, the HMT (methenamine) of 0.021g is weighed, is placed in
In the beaker of 50ml, stirring 2h obtains as clear as crystal solution；
(3) obtained solution is poured into containing Ni3S2In the water heating kettle of-NF material, juxtaposition is sealed after 30min is stirred at room temperature
In hydro-thermal case, cooled to room temperature after water heating kettle is taken out after keeping 160 DEG C of at least 6h of temperature；
(4) it is placed on vacuum drying oven drying by the washing of obtained material 3 times, finally in sheet Ni3S2Upper original position load C eO2
Nano particle obtains CeO2/Ni3S2- NF composite material.
4h is kept in hydro-thermal case in the step 1)-(2).
In order to make Transition-metal dichalcogenide Ni3S2Catalytic activity is further promoted, and the present invention is made with six nitric hydrate ceriums
For cerium source, nickel foam is as collector, by first step hydro-thermal vulcanization fabricated in situ sheet Ni on three-dimensional porous foams nickel3S2,
It is kept the temperature at relatively mild temperature by second step with ethanol as solvent, in sheet Ni3S2Load nanoscale cerium in situ
Grain, obtained CeO2/Ni3S2- NF composite material is answered compared to what more single fertile material and traditional dipping calcining obtained
Material, catalytic activity significantly improve.
Compared with prior art, the present invention has the advantages that the composite material synthesized using method in situ, catalysis
Activity is often better than the composite material of traditional dipping calcining synthesis, in addition, safe and simple in the entire synthesis process of this experiment,
Green non-pollution.Selection cerous nitrate is cerium source, in the In-situ sulphiding conjunction on three-dimensional porous foams nickel (NF) of first step Situ Hydrothermal
Three nickel (Ni of slabbing curing3S2) on the basis of, the method for further utilizing low-temperature solvent heat with ethanol as solvent is in situ to load
Cerium oxide nanoparticles, the CeO of synthesis2/Ni3S2There is-NF composite material excellent electro-catalysis to hydrolyze Hydrogen Evolution Performance.
Specific manifestation is as follows:
1, core of the present invention is the method using low-temperature solvent heat in sheet Ni3S2Upper fabricated in situ nano Ce O2Particle.
2, CeO prepared by the present invention2/Ni3S2- NF heterojunction structure catalysis material, with single Ni3S2、CeO2And nickel foam
It compares, which there is excellent electro-catalysis to hydrolyze Hydrogen Evolution Performance.
3, process of the present invention is simple, green non-pollution, easily realizes large-scale production.
4, high reliablity of the present invention, repeatability is strong, there is good application prospect.
Detailed description of the invention
Fig. 1 is XRD diagram:
(a) Ni that hydro-thermal vulcanization 4h is obtained3S2The XRD diagram of-NF；
(b) CeO that solvent heat 6h is obtained2/Ni3S2The XRD diagram of-NF.
Fig. 2 is first step hydro-thermal SEM figure:
(a) the surface topography SEM figure of nickel foam；
(b) Ni of first step hydro-thermal In-situ sulphiding 4h synthesizing flaky in nickel foam3S2SEM figure.
Fig. 3 is second step solvent heat SEM figure:
(a) in sheet Ni3S2Upper load nanoscale CeO in situ2Particle SEM figure；
It (b) is figure (a) partial enlarged view.
Fig. 4 is Ni3S2With CeO2Interface distributions schematic diagram:
(a) the TEM figure of CeO2/Ni3S2-NF；
(b) the STEM figure of CeO2/Ni3S2-NF；
(c) Ni element uniformly distributing；
(d) S element uniformly distributing；
(e) Ce element uniformly distributing；
(f) O element uniformly distributing.
CeO prepared by Fig. 5 present invention2/Ni3S2Electrocatalytic hydrogen evolution is linear under-NF composite material alkaline condition (1M KOH)
It scans volt-ampere curve (LSV) (a)；
Corresponding Tafel slope figure (b).
Synthesis process schematic diagram Fig. 6 of the invention.
Specific embodiment
Below by specific embodiments and the drawings, the present invention is further illustrated.The embodiment of the present invention is in order to more
So that those skilled in the art is more fully understood the present invention well, any limitation is not made to the present invention.
Embodiment 1
It is 1x3cm by area2Nickel foam (NF) clean ultrasound 10min with acetone and 3M HCl respectively, use respectively later
Deionized water and ethyl alcohol clean 3 times, are then evaporated in 60 DEG C of vacuum tanks stand-by.The thiourea solution for preparing 1.45mM, processing
Nickel foam afterwards is placed in 40mL water heating kettle, while the above-mentioned thiourea solution of 10ml is added, and sealing water heating kettle is placed on hydro-thermal
In case, cooled to room temperature is taken out after 150 DEG C of holding, 4h, the nickel foam after taking out vulcanization cleans 3 with deionized water and ethyl alcohol
It is secondary, the sample after cleaning is placed in 60 DEG C of vacuum drying oven and is evaporated to obtain Ni3S2-NF.Taking area is 1x1.5cm2Ni3S2-
NF material is placed in the water heating kettle of 40ml stand-by with ethyl alcohol cleaning-drying.15ml ethyl alcohol is measured with graduated cylinder, balance weighs
The HMT (methenamine) of the six nitric hydrate ceriums of 0.011g, 0.021g, the above raw material is placed in the beaker of 50ml, stirs 2h
Obtain the as clear as crystal ethanol solution containing cerium ion, HMT.Obtained solution is transferred to above-mentioned containing Ni3S2- NF material
It in water heating kettle, is sealed and placed in hydro-thermal case after 30min is stirred at room temperature, takes out water heating kettle after keeping 160 DEG C of temperature, 6h, it is natural
It is cooled to room temperature.It is placed on vacuum drying oven drying by the washing of obtained material 3 times, finally in sheet Ni3S2Upper original position load C eO2
Nano particle obtains CeO2/Ni3S2- NF composite material.
Embodiment 2
It is 1x3cm by area2Nickel foam (NF) clean ultrasound 10min with acetone and 3M HCl respectively, use respectively later
Deionized water and ethyl alcohol clean 3 times, are then evaporated in 60 DEG C of vacuum tanks stand-by.The thiourea solution for preparing 1.45mM, processing
Nickel foam afterwards is placed in 40mL water heating kettle, while the above-mentioned thiourea solution of 10ml is added, and sealing water heating kettle is placed on hydro-thermal
In case, cooled to room temperature is taken out after 150 DEG C of holding, 5h, the nickel foam after taking out vulcanization cleans 3 with deionized water and ethyl alcohol
It is secondary, the sample after cleaning is placed in 60 DEG C of vacuum drying oven and is evaporated to obtain Ni3S2-NF.Taking area is 1x1.5cm2Ni3S2-
NF material is placed in the water heating kettle of 40ml stand-by with ethyl alcohol cleaning-drying.15ml ethyl alcohol is measured with graduated cylinder, balance weighs
The HMT (methenamine) of the six nitric hydrate ceriums of 0.011g, 0.021g, the above raw material is placed in the beaker of 50ml, stirs 2h
Obtain the as clear as crystal ethanol solution containing cerium ion, HMT.Obtained solution is transferred to above-mentioned containing Ni3S2- NF material
It in water heating kettle, is sealed and placed in hydro-thermal case after 30min is stirred at room temperature, takes out water heating kettle after keeping 160 DEG C of temperature, 6h, it is natural
It is cooled to room temperature.It is placed on vacuum drying oven drying by the washing of obtained material 3 times, finally in sheet Ni3S2Upper original position load C eO2
Nano particle obtains CeO2/Ni3S2- NF composite material.
Embodiment 3
It is 1x3cm by area2Nickel foam (NF) clean ultrasound 10min with acetone and 3M HCl respectively, use respectively later
Deionized water and ethyl alcohol clean 3 times, are then evaporated in 60 DEG C of vacuum tanks stand-by.The thiourea solution for preparing 1.45mM, processing
Nickel foam afterwards is placed in 40mL water heating kettle, while the above-mentioned thiourea solution of 10ml is added, and sealing water heating kettle is placed on hydro-thermal
In case, cooled to room temperature is taken out after 150 DEG C of holding, 6h, the nickel foam after taking out vulcanization cleans 3 with deionized water and ethyl alcohol
It is secondary, the sample after cleaning is placed in 60 DEG C of vacuum drying oven and is evaporated to obtain Ni3S2-NF.Taking area is 1x1.5cm2Ni3S2-
NF material is placed in the water heating kettle of 40ml stand-by with ethyl alcohol cleaning-drying.15ml ethyl alcohol is measured with graduated cylinder, balance weighs
The HMT (methenamine) of the six nitric hydrate ceriums of 0.011g, 0.021g, the above raw material is placed in the beaker of 50ml, stirs 2h
Obtain the as clear as crystal ethanol solution containing cerium ion, HMT.Obtained solution is transferred to above-mentioned containing Ni3S2- NF material
It in water heating kettle, is sealed and placed in hydro-thermal case after 30min is stirred at room temperature, takes out water heating kettle after keeping 160 DEG C of temperature, 6h, it is natural
It is cooled to room temperature.It is placed on vacuum drying oven drying by the washing of obtained material 3 times, finally in sheet Ni3S2Upper original position load C eO2
Nano particle obtains CeO2/Ni3S2- NF composite material
Embodiment 4
It is 1x3cm by area2Nickel foam (NF) clean ultrasound 10min with acetone and 3M HCl respectively, use respectively later
Deionized water and ethyl alcohol clean 3 times, are then evaporated in 60 DEG C of vacuum tanks stand-by.The thiourea solution for preparing 1.45mM, processing
Nickel foam afterwards is placed in 40mL water heating kettle, while the above-mentioned thiourea solution of 10ml is added, and sealing water heating kettle is placed on hydro-thermal
In case, cooled to room temperature is taken out after 150 DEG C of holding, 8h, the nickel foam after taking out vulcanization cleans 3 with deionized water and ethyl alcohol
It is secondary, the sample after cleaning is placed in 60 DEG C of vacuum drying oven and is evaporated to obtain Ni3S2-NF.Taking area is 1x1.5cm2Ni3S2-
NF material is placed in the water heating kettle of 40ml stand-by with ethyl alcohol cleaning-drying.15ml ethyl alcohol is measured with graduated cylinder, balance weighs
The HMT (methenamine) of the six nitric hydrate ceriums of 0.011g, 0.021g, the above raw material is placed in the beaker of 50ml, stirs 2h
Obtain the as clear as crystal ethanol solution containing cerium ion, HMT.Obtained solution is transferred to above-mentioned containing Ni3S2- NF material
It in water heating kettle, is sealed and placed in hydro-thermal case after 30min is stirred at room temperature, takes out water heating kettle after keeping 160 DEG C of temperature, 6h, it is natural
It is cooled to room temperature.It is placed on vacuum drying oven drying by the washing of obtained material 3 times, finally in sheet Ni3S2Upper original position load C eO2
Nano particle obtains CeO2/Ni3S2- NF composite material.
Control sample
It is 1x3cm by area2Nickel foam (NF) clean ultrasound 10min with acetone and 3M HCl respectively, use respectively later
Deionized water and ethyl alcohol clean 3 times, are then evaporated in 60 DEG C of vacuum tanks stand-by.The thiourea solution for preparing 1.45mM, processing
Nickel foam afterwards is placed in 40mL water heating kettle, while the above-mentioned thiourea solution of 10ml is added, and sealing water heating kettle is placed on hydro-thermal
In case, cooled to room temperature is taken out after 150 DEG C of holding, 8h, the nickel foam after taking out vulcanization cleans 3 with deionized water and ethyl alcohol
It is secondary, the sample after cleaning is placed in 60 DEG C of vacuum drying oven and is evaporated to obtain Ni3S2-NF.Taking area is 1x1.5cm2Ni3S2-
NF material, is cleaned and dried with ethyl alcohol.15ml DMF (N-N dimethylformamide) is measured with graduated cylinder, balance weighs the six of 0.011g
The above raw material is placed in the beaker of 20ml by nitric hydrate cerium, and stirring 2h obtains uniform solution, by 1x1.5cm2Ni3S2-
NF material impregnates for 24 hours in the solution, later drying at room temperature, and calcines 2h under 500 DEG C of argon atmospheres, obtains CeO2/
Ni3S2- NF composite material.
What (a) was indicated in Fig. 1 is by first step hydro-thermal 6h, and original flavor generates Ni on nickel foam3S2The XRD diagram of object phase, can be with
It determines other than the diffraction maximum of simple substance nickel substrate, there are Ni3S2Object phase shows the fabricated in situ Ni in nickel foam3S2Substance；
(b) it indicates after second step solvent thermal reaction, has ceria generation, i.e., successfully load to cerium oxide nanoparticles in situ
In Ni3S2 nanometer sheet.
(a) indicates that foam nickel skeleton low power SEM figure and (b) are that nickel foam office is further amplified after 6h hydro-thermal in Fig. 2
The SEM of portion's skeleton schemes, and can determine after hydro-thermal reaction there is the Ni of sheet on nickel skeleton3S2It generates, and distribution is very fine and close,
Further partial enlargement b figure (i.e. illustration), it can be seen that Ni3S2Surface is smooth and thickness is lower than 50nm.
What Fig. 3 (a) and (b) were indicated is the relative coarseness that nickel foam becomes after second step solvent thermal reaction, partial enlargement
It is further seen that there is cerium dioxide nano can be with uniform load in Ni3S2 nanometer sheet.
It is Ni shown in Fig. 4 (a)3S2With CeO2Interface, show the boundary for successfully having constructed transition metal oxide and sulfide
Face；(b) scheme for STEM；It (c-f) is corresponding Elemental redistribution, it can be seen that tetra- kinds of elements of Ni, S, Ce, O are uniformly distributed.
(a) and (b) is respectively the LSV curve and Tafel slope of material prepared and contrast material in Fig. 5, it can be deduced that
By the material of growth in situ ceria, required overpotential is calcined required for material obtained more than tradition dipping
It is small, Tafel slope further confirms, by its dynamics significant increase of the material of fabricated in situ.Fig. 6 is that material preparation is shown
It is intended to.
Claims (2)
1. a kind of fabricated in situ transition metal oxide/Ni-based sulfide composite material preparation method, which is characterized in that including
Following steps:
1) In-situ sulphiding more empty nickel foams synthesize Ni3S2-NF
(1) it handles nickel foam: being 1x3cm by area2Nickel foam use acetone and each ultrasound 10min of 3M HCl respectively, distinguish later
It is cleaned, is then evaporated in 60 DEG C of vacuum tank stand-by with deionized water and ethyl alcohol；
(2) thiourea solution of 1.45mM is prepared, nickel foam is placed in 40mL water heating kettle by treated in step (1), is added simultaneously
Entering the thiourea solution of 10ml, sealing water heating kettle is placed in hydro-thermal case, natural cooling is taken out after 150 DEG C of holding, 4-8h,
Nickel foam after taking out vulcanization is cleaned with deionized water and ethyl alcohol, the sample after cleaning is placed in 60 DEG C of vacuum drying oven and is evaporated
Obtain Ni3S2-NF；
2) fabricated in situ CeO2/Ni3S2- NF composite material
(1) taking area is 1x1.5cm2The obtained Ni of the step 1)3S2- NF material is placed on 40ml with ethyl alcohol cleaning-drying
Water heating kettle in it is stand-by；
(2) 15ml ethyl alcohol is measured, the six nitric hydrate ceriums of 0.011g, the methenamine of 0.021g is weighed, is placed in the beaker of 50ml
In, stirring 2h obtains as clear as crystal solution；
(3) obtained solution is poured into containing Ni3S2In the water heating kettle of-NF material, water is sealed and placed in after 30min is stirred at room temperature
In hot tank, cooled to room temperature after water heating kettle is taken out after keeping 160 DEG C of at least 6h of temperature；
(4) it is placed on vacuum drying oven drying by the washing of obtained material 3 times, finally in sheet Ni3S2Upper original position load C eO2Nanometer
Particle obtains CeO2/Ni3S2- NF composite material.
2. a kind of preparation of fabricated in situ transition metal oxide/Ni-based sulfide composite material according to claim 1
Method, which is characterized in that keep 4h in hydro-thermal case in the step 1)-(2).
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| 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 |
| CN113416976A (en) * | 2021-05-31 | 2021-09-21 | 江苏大学 | Cu5FeS4/Ni3S2Preparation method of @ NF composite material and application of @ NF composite material in photoelectric hydrolysis |
| CN113416980A (en) * | 2021-06-09 | 2021-09-21 | 江西理工大学 | Efficient full-hydrolysis water catalyst MoO2-CeOx/NF and preparation method thereof |
| CN113957468A (en) * | 2021-07-28 | 2022-01-21 | 上海应用技术大学 | Ni3S2@ CoO-NF composite material and synthesis method and application thereof |
| CN114045503A (en) * | 2021-11-10 | 2022-02-15 | 鄂尔多斯应用技术学院 | Efficient non-noble metal electrolytic water catalytic material and preparation method and application thereof |
| CN114774958A (en) * | 2022-04-20 | 2022-07-22 | 天津大学 | Corrosion-resistant nickel-iron electrode and preparation method and application thereof |
| CN114797889A (en) * | 2022-04-12 | 2022-07-29 | 上海工程技术大学 | Fe 3 O 4 @MnO 2 -CeO 2 Nano material and preparation method and application thereof |
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Cited By (10)
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| 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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| CN113416980A (en) * | 2021-06-09 | 2021-09-21 | 江西理工大学 | Efficient full-hydrolysis water catalyst MoO2-CeOx/NF and preparation method thereof |
| CN113957468A (en) * | 2021-07-28 | 2022-01-21 | 上海应用技术大学 | Ni3S2@ CoO-NF composite material and synthesis method and application thereof |
| CN113957468B (en) * | 2021-07-28 | 2023-11-24 | 上海应用技术大学 | Ni (nickel) 3 S 2 @CoO-NF composite material and synthetic method and application thereof |
| CN114045503A (en) * | 2021-11-10 | 2022-02-15 | 鄂尔多斯应用技术学院 | Efficient non-noble metal electrolytic water catalytic material and preparation method and application thereof |
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