CN104966841B - A kind of preparation method of Pd/NiCu two-dimensional nano composite - Google Patents
A kind of preparation method of Pd/NiCu two-dimensional nano composite Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The present invention relates to a kind of preparation method of Pd/NiCu two-dimensional nano composite.It is specially：It is carried out in two steps, Ni, the inorganic salt of Cu are dissolved in deionized water and are configured to solution by the first step, then in molar ratio 4:1~1:1 is added in the pyroxylin film of conical flask pattern, adds a certain amount of surfactant, is filled with noble gases argon, then sealed, be placed in beaker, add reducing agent to be reduced, palladium salt is dissolved in wiring solution-forming in hydrochloric acid by second step, adds surfactant, is reduced with reducing agent, form seed solution, then it is mixed with the product that the first step obtains, ultrasonic, wash sample, centrifugation, obtains the Pd/NiCu nano composite material that final product is black.Prepare the big alloy nano thin film of specific surface area using the inventive method, there is excellent magnetic and catalysis activity.The inventive method is simple to operation, easy to control.
Description
Technical field
The invention belongs to technical field of nano material, specifically related to a kind of preparation of Pd/NiCu two-dimensional nano composite
Method.
Background technology
Bimetal nano material has good optical property, thermodynamic property, dielectric properties, mechanical property, catalytic performance
Deng.Two-dimension nano materials, because it has big specific surface area, have more avtive spots, have good catalytic as catalyst
Can, and NiCu material price ratio is less expensive, economy, and so much avtive spot can be good at loading other above
Metal.
Electrocatalytic Oxidation of Methanol agent is to determine one of critical material of performance of direct methanol fuel cells, life-span and cost.
People have carried out substantial amounts of research from raising anode catalyst activity and reduction by two aspects of catalyst cost in recent years,
Effectively promoting the development of DMFC. noble metal and its alloy nano-material are organic in difficult degradation as catalyst
Thing is degraded, organic synthesiss, fuel cell, and the field such as inorganic complex hydrolysis is widely used.Catalyst containing Pd can be in alkalescence
Under the conditions of as DMFC anode, thus avoid catalyst containing Pt can CO poisoning, material with carbon element corrosion impact.
Content of the invention
It is an object of the invention to provide a kind of simple, non-environmental-pollution, two-dimentional Pd/NiCu with low cost are nano combined
The preparation method of material.The solution of the present invention is：In energy saving, free from environmental pollution under conditions of synthesize specific surface area
Big Nanoalloy, in order to reduce the consumption of noble metal, using the big NiCu of specific surface area as substrate, above load P d nanometer
Particle, the electrode material as fuel cell.
A kind of preparation method of Pd/NiCu two-dimensional nano composite proposed by the present invention, comprises the following steps：
(1）The preparation of two-dimentional NiCu alloy
(1.1), Nickel dichloride. and copper chloride are weighed respectively, deionized water is respectively configured to solution, by Ni2+With Cu2+4:1~
1:1 mol ratio is mixed, and is subsequently placed in the pyroxylin film of conical flask pattern, adds 1mg surfactant, is filled with
Argon, then sealing is placed in 150ml beaker；
(1.2), weigh potassium borohydride, deionized water is configured to solution, adjusting pH value with NaOH solution is 10, Ran Houqu
10ml is incorporated in the beaker of step (1.1) gained mixed liquor, with sealed membrane, beaker envelope is got up；
(1.3), after reaction 3 ~ 12h time, collect the black solid in pyroxylin film, be then centrifuged for, washing, stand-by；
(2）The preparation of Pd nanoparticle
(2.1) palladium salt is dissolved in HCl, is configured to solution, weigh surfactant, deionized water is configured to molten
Liquid, weighs reducing agent,Deionized water dissolves, and places in refrigerator, stand-by；
(2.2) palladium salt solution and surfactant, are taken respectively in 25ml vial, stirring and evenly mixing, it is subsequently adding
Reducing agent, after stirring and evenly mixing, stops stirring, stands 3h；
(2.3), collect black precipitate, centrifugation, wash, stand-by；
(3）The preparation of Pd/NiCu alloy
(3.1) black solid that step (1) prepares and the black precipitate that step (2) prepares, are taken in 5ml no
In water-ethanol, ultrasonic 30min ~ 1h；
(3.2), it is centrifuged, washing, be dried, obtain final black product Pd/NiCu nano composite material.
In the present invention, described Nickel dichloride. is NiCl2·6H2O, concentration is 50mmol/L;Described copper chloride is
CuCl2·2H2O, concentration is 50 ~ 20mmol/L.
In the present invention, it is prepared that pyroxylin film used is that pyroxylin solution dries.
Ni in the present invention, described in step (1.1)2+And Cu2+Cumulative volume be 10ml.
In the present invention, the surfactant described in step (1.1) is PVP.
In the present invention, described washing is all alternately to be washed using deionized water and dehydrated alcohol.
In the present invention, described stir as ultrasonic vibration or magnetic agitation, the time is 30～60 minutes.
In the present invention, described centrifugation rotating speed is 6000 revs/min, and the time is 5 minutes.
In the present invention, described drying is 4h to be dried at 60 DEG C of vacuum drying oven.
In the present invention, described palladium salt is Palladous chloride., and the concentration of its wiring solution-forming is 0.01mol/L.
In the present invention, the surfactant described in step (2.1) is CTAC, and its concentration is 0.1mol/L.
In the present invention, step (2.1), the reducing agent described in (2.2) is sodium borohydride, and its concentration is 0.01mol/L.
In the present invention, the reducing agent in step (1.1) is potassium borohydride, and its concentration is 30 ~ 50mmol/L.
The structure of the inventive method products therefrom, pattern, composition are characterized, scanning electron microscopy can be selected respectively
Mirror (SEM), high resolution transmission electron microscopy (TEM), energy chromatograph (EDS) etc. is characterized, and SEM, TEM characterize nanometer material
The microstructure of material, EDS shows the constituent of product.
In the present invention, the present invention is respectively adopted simple chlorate as reactant, has very strong versatility.
The product of present invention preparation has good chemical property, has more wide in the electrode material of fuel cell
Development prospect and application space.
Brief description
Fig. 1,2 be embodiment 1 in 1）The SEM figure of step products therefrom.
Fig. 3,4 be embodiment 2 in 1）The SEM figure of step products therefrom.
Fig. 5,6 be embodiment 1,2,3 in 2）The TEM figure of step products therefrom.
Fig. 7 is 3 in embodiment 1）The TEM figure of step products therefrom.
Fig. 8 is 3 in embodiment 2）The TEM figure of step products therefrom.
Fig. 9 is 3 in embodiment 1）The EDS figure of step products therefrom.
Figure 10 is 3 in embodiment 2）The EDS figure of step products therefrom.
Figure 11 is 1 in embodiment 3）The SEM figure of step products therefrom.
Figure 12 is 3 in embodiment 3）The SEM figure of step products therefrom.
Specific embodiment
The present invention is further illustrated with reference to embodiments.
Embodiment 1:
1）The preparation of two-dimentional NiCu alloy
The first step, accurately weighs 0.1185gNiCl2·6H2O, deionized water is configured to 100ml solution, and concentration is
50mmol/L, accurately weighs 0.0340gCuCl2·2H2O, deionized water is configured to 100ml solution, and concentration is 20mmol/L,
Ni2+：Cu2+According to 1:1 mol ratio is mixed, and cumulative volume is 10ml, is subsequently placed in the pyroxylin film of conical flask pattern, then
Add 1mg PVP in pyroxylin film, be filled with argon, then sealing is placed in 150ml beaker.
Second step, accurately weighs the potassium borohydride of 0.162g, and deionized water is configured to 100ml solution, and concentration is
30mmol/L, uses 0.2mol L-1NaOH adjust PH ~ 10, then take 10ml in the beaker of the first step, with sealed membrane burn
Cup envelope is got up.
3rd step, after the reaction 5h time, collects the black solid in pyroxylin film, is then centrifuged for, washed once, stand-by.
2）The preparation of Pd nanoparticle
The first step, accurately weighs 44.5mgPdCl2It is dissolved in the HCl of 25ml 0.02M, be configured to 0.01M's
H2PdCl4Solution.Accurately weigh 0.80g CTAC, deionized water is configured to solution, use 25ml volumetric flask constant volume.Accurately claim
Take the NaBH of 0.0038g4,Deionized water dissolves, and uses 10ml volumetric flask constant volume, places cold preservation in refrigerator, stand-by.
Second step, takes 0.01M 0.25ml H respectively2PdCl4Solution and 0.1M 9.75ml CTAC are in 25ml vial
In, stirring and evenly mixing, it is subsequently adding 0.01M 0.60ml NaBH4, after stirring and evenly mixing, after 10s, stop stirring, then stand 3h.
3rd step, collects black precipitate, centrifugation, washs, stand-by.
3）The preparation of Pd/NiCu nano composite material
The first step, takes 1）Middle black solid and 2）Middle black precipitate in 5ml dehydrated alcohol, ultrasonic 30min.
Second step, centrifugation, washing, it is dried, obtain final black product Pd/NiCu nano composite material.
Fig. 1,2 is 1 in embodiment 1）The SEM figure of step products therefrom different amplification.Fig. 5,6 be embodiment 1 in 2）
The TEM figure of step products therefrom.Fig. 7 is 3 in embodiment 1）The TEM figure of step products therefrom.By picture as can be seen that two dimension
The pattern of NiCu can be clearly visible that, and the dispersion of Pd nanoparticle is very uniform, does not have agglomeration, the Pd/NiCu of formation
In the TEM of nano composite material, Pd particle is supported on NiCu alloy well, and does not reunite.Fig. 9 is 3 in embodiment 1）
The EDS figure of step products therefrom.
Embodiment 2：
1）The preparation of two-dimentional NiCu alloy
The first step, accurately weighs 0.1185gNiCl2·6H2O, deionized water is configured to 100ml solution, and concentration is
50mmol/L, accurately weighs 0.0850gCuCl2·2H2O, deionized water is configured to 100ml solution, and concentration is 50mmol/L,
Ni2+：Cu2+According to 4:1 mol ratio is mixed, and cumulative volume is 10ml, is subsequently placed in the pyroxylin film of conical flask pattern, then
Add 1mg PVP in pyroxylin film, be filled with argon, then sealing is placed in 150ml beaker.
Second step, accurately weighs the potassium borohydride of 0.27g, and deionized water is configured to 100ml solution, and concentration is 50mmo/
L, uses 0.2mol L-1NaOH adjust PH be 10, then take 10ml in the beaker of the first step, with sealed membrane, beaker sealed
Come.
3rd step, after the reaction 5h time, collects the black solid in pyroxylin film, is then centrifuged for, washed once, stand-by.
2）The preparation of Pd nanoparticle
The first step, accurately weighs 44.5mgPdCl2It is dissolved in the HCl of 25ml 0.02M, be configured to 0.01M's
H2PdCl4Solution.Accurately weigh 0.80g CTAC, deionized water is configured to solution, use 25ml volumetric flask constant volume.Accurately claim
Take the NaBH of 0.0038g4,Deionized water dissolves, and uses 10ml volumetric flask constant volume, places cold preservation in refrigerator, stand-by.
Second step, takes 0.01M 0.25ml H respectively2PdCl4Solution and 0.1M 9.75ml CTAC are in 25ml vial
In, stirring and evenly mixing, then
Add 0.01M 0.60ml NaBH4, after stirring and evenly mixing, after 10s, stop stirring, then stand 3h.
3rd step, collects black precipitate, centrifugation, washs, stand-by.
3）The preparation of Pd/NiCu nano composite material
The first step, takes 1）Middle black solid and 2）Middle black precipitate in 5ml dehydrated alcohol, ultrasonic 30min.
Second step, centrifugation, washing, it is dried, obtain final black product Pd/NiCu nano composite material.
Fig. 3,4 be embodiment 2 in 1）The SEM figure of step products therefrom different amplification.Fig. 5,6 be embodiment 2 in 2）
The TEM figure of step products therefrom.Fig. 8 is 3 in embodiment 2）The TEM figure of step products therefrom.By picture as can be seen that two dimension
The pattern of NiCu also can be clearly visible that, it is fine that film tiles, and illustrates that the increase of Ni content is conducive to the formation of film, Pd nanoparticle
The dispersion of son is very uniform, does not have agglomeration, the load of Pd uniform particle in the TEM of Pd/NiCu nano composite material of formation
On NiCu alloy, and do not reunite.Simply the amount of the Pd particle of load is a lot, and Figure 10 is 3 in embodiment 1）Step gained
The EDS of product schemes it can be seen that the ratio of Pd is very big, illustrates a lot in Pd load.
Embodiment 3：
1）The preparation of two-dimentional NiCu alloy
The first step, accurately weighs 0.1185gNiCl2·6H2O, deionized water is configured to 100ml solution, and concentration is
50mmol/L, accurately weighs 0.0340gCuCl2·2H2O, deionized water is configured to 100ml solution, and concentration is 20mmol/L,
Ni2+：Cu2+According to 7:2 mol ratios are mixed, and cumulative volume is 10ml, is subsequently placed in the pyroxylin film of conical flask pattern, then
Add 1mg PVP in pyroxylin film, be filled with argon, then sealing is placed in 150ml beaker.
Second step, accurately weighs the potassium borohydride of 0.162g, and deionized water is configured to 100ml solution, and concentration is
30mmol/L, uses 0.2mol L-1NaOH adjust PH ~ 10, then take 10ml in the beaker of the first step, with sealed membrane burn
Cup envelope is got up.
3rd step, after the reaction 5h time, collects the black solid in pyroxylin film, is then centrifuged for, washed once, stand-by.
2）The preparation of Pd nanoparticle
The first step, accurately weighs 44.5mgPdCl2It is dissolved in the HCl of 25ml 0.02M, be configured to 0.01M's
H2PdCl4Solution.Accurately weigh 0.80g CTAC, deionized water is configured to solution, use 25ml volumetric flask constant volume.Accurately claim
Take the NaBH of 0.0038g4,Deionized water dissolves, and uses 10ml volumetric flask constant volume, places cold preservation in refrigerator, stand-by.
Second step, takes 0.01M 0.25ml H respectively2PdCl4Solution and 0.1M 9.75ml CTAC are in 25ml vial
In, stirring and evenly mixing, then
Add 0.01M 0.60ml NaBH4, after stirring and evenly mixing, after 10s, stop stirring, then stand 3h.
3rd step, collects black precipitate, centrifugation, washs, stand-by.
3）The preparation of Pd/NiCu nano composite material
The first step, takes 1）Middle black solid and 2）Middle black precipitate in 5ml dehydrated alcohol, ultrasonic 30min.
Second step, centrifugation, washing, it is dried, obtain final black product Pd/NiCu nano composite material.
Figure 11 is 1 in embodiment 3）The SEM figure of step products therefrom.Figure 12 is 3 in embodiment 3）Step products therefrom
SEM schemes.From Figure 12 it will be clear that on NiCu alloy film, load has Pd particle.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and apply this
Bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiment without through performing creative labour.Therefore, the invention is not restricted to enforcement here
Example, in the modification made without departing from the scope of the invention all within protection scope of the present invention.
Claims (13)
1. a kind of preparation method of Pd/NiCu two-dimensional nano composite it is characterised in that：Comprise the following steps that：
(1）The preparation of two-dimentional NiCu alloy
(1.1), Nickel dichloride. and copper chloride are weighed respectively, deionized water is respectively configured to solution, by Ni2+With Cu2+4:1~1:1
Mol ratio is mixed, and is subsequently placed in the pyroxylin film of conical flask pattern, adds 1mg surfactant, is filled with argon,
Then sealing is placed in 150ml beaker；
(1.2), weigh reducing agent, deionized water is configured to solution, adjusting pH value with NaOH solution is 10, then takes 10ml to add
Enter in the beaker of step (1.1) gained mixed liquor, with sealed membrane, beaker envelope is got up；
(1.3), after reaction 3 ~ 12h time, collect the black solid in pyroxylin film, be then centrifuged for, washing, stand-by；
(2）The preparation of Pd nanoparticle
(2.1) palladium salt is dissolved in HCl, is configured to palladium salt solution, weigh surfactant, deionized water is configured to surface
Activator solution, weighs reducing agent,Deionized water dissolves, and obtains reductant solution, places in refrigerator, stand-by；
(2.2) palladium salt solution and surfactant solution, are taken respectively in 25ml vial, stirring and evenly mixing, it is subsequently adding reduction
Agent solution, after stirring and evenly mixing, stops stirring, stands 3h；
(2.3), collect black precipitate, centrifugation, wash, stand-by；
(3）The preparation of Pd/NiCu alloy
(3.1) black solid that step (1) prepares and the black precipitate that step (2) prepares, are taken in the anhydrous second of 5ml
In alcohol, ultrasonic 30min ~ 1h；
(3.2), it is centrifuged, washing, be dried, obtain final black product Pd/NiCu nano composite material.
2. preparation method according to claim 1 is it is characterised in that described Nickel dichloride. is NiCl2·6H2O, concentration is
50mmol/L, described copper chloride is CuCl2·2H2O, concentration is 50 ~ 20mmol/L.
3. preparation method according to claim 1 dries system it is characterised in that pyroxylin film used is pyroxylin solution
?.
4. preparation method according to claim 1 is it is characterised in that Ni in step (1.1)2+And Cu2+The cumulative volume of solution is
10ml.
5. preparation method according to claim 1 is it is characterised in that the surfactant in step (1.1) is PVP.
6. preparation method according to claim 1 is it is characterised in that washing described in step (1.3), (2.3) and (3.2)
Wash is all alternately to be washed using deionized water and dehydrated alcohol.
7. preparation method according to claim 1 is it is characterised in that step (2.2）Described in stir as ultrasonic vibration or magnetic
Power stirs, and the time is 30～60 minutes.
8. preparation method according to claim 1 it is characterised in that in step (3.2) centrifugation rotating speed be 6000 turns/
Minute, the time is 5 minutes.
9. preparation method according to claim 1 it is characterised in that in step (3.2) drying be in 60 DEG C of vacuum drying oven
Under 4h is dried.
10. it is characterised in that the palladium salt in step (2.1) is Palladous chloride., it is made into preparation method according to claim 1
The concentration of solution is 0.01mol/L.
11. preparation methoies according to claim 1 it is characterised in that surfactant in step (2.1) is CTAC, its
Concentration is 0.1mol/L.
It is characterised in that step (2.1), the reducing agent in (2.2) is boron hydrogen to 12. preparation methoies according to claim 1
Change sodium, its concentration is 0.01mol/L.
13. preparation methoies according to claim 1 it is characterised in that reducing agent in step (1.2) is potassium borohydride, its
Concentration is 30 ~ 50mmol/L.
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| CN109261156B (en) * | 2018-10-26 | 2021-08-10 | 同济大学 | Nickel film and zinc oxide nanorod composite material as well as preparation method and application thereof |
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