CN104966841A - Method for preparing Pd / NiCu two-dimensional nanocomposite - Google Patents
Method for preparing Pd / NiCu two-dimensional nanocomposite Download PDFInfo
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Abstract
The present invention relates to a method for preparing a Pd / NiCu two-dimensional nanocomposite. The method specifically comprises two steps, 1, Ni and Cu inorganic salts are dissolved in deionized water for preparing a solution, and then are added into a conical flask-shaped collodion membrane in the molar ratio of 4: 1 to 1: 1, the conical flask-shaped collodion membrane is added with a certain amount of a surfactant, filled with inert gas argon, then sealed, and placed in a beaker, and a reducing agent is added for reducing; 2, a palladium salt is dissolved in hydrochloric acid for preparing a solution, a surfactant is added, a reducing agent is added for reducing to form a seed solution, the seed solution is mixed with the product obtained in the first step, and the final product black Pd / NiCu nanocomposite is obtained by ultrasonic treatment, washing and centrifugation. A larger specific surface area alloy nano-film is prepared by the method, and has excellent magnetic properties and catalytic activity. The method is simple and easy to operate, and easy to control.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of preparation method of Pd/NiCu two-dimensional nano composite material.
Background technology
Bimetal nano material has good optical property, thermodynamic property, dielectric property, mechanical property, catalytic performance etc.Two-dimension nano materials, because it has large specific area, have more avtive spot, have good catalytic performance as catalyst, and NiCu material price is cheaper, economy, and so much avtive spot can be good at other metals of load above.
Electrocatalytic Oxidation of Methanol agent is one of the critical material determining performance of direct methanol fuel cells, life-span and cost. people are active and reduce catalyst cost two aspects and carried out large quantifier elimination from raising anode catalyst in recent years, the strong development promoting direct methanol fuel cell. noble metal and alloy nano-material thereof are degraded at hardly degraded organic substance as catalyst, organic synthesis, fuel cell, the fields such as inorganic complex hydrolysis are widely used.The anode of DMFC can be used as containing Pd catalyst in the basic conditions, thus avoid containing Pt catalyst meeting CO poisoning, the impact of material with carbon element corrosion.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of simple, non-environmental-pollution, two-dimentional Pd/NiCu nano composite material with low cost.Solution of the present invention is: in energy savings, the Nanoalloy that specific area is large is synthesized, in order to reduce the consumption of noble metal, using the large NiCu of specific area as substrate under condition free from environmental pollution, load P d nano particle above, as the electrode material of fuel cell.
The preparation method of a kind of Pd/NiCu two-dimensional nano composite material that the present invention proposes, comprises the following steps:
(1) preparation of two-dimentional NiCu alloy
(1.1), take nickel chloride and copper chloride respectively, be respectively mixed with solution with deionized water, by Ni
2+with Cu
2+the mol ratio of 4:1 ~ 1:1 mixes, and is then placed in the pyroxylin film of conical flask pattern, then adds 1mg surfactant, is filled with argon gas, and then sealing is placed in 150ml beaker;
(1.2), taking potassium borohydride, be mixed with solution with deionized water, is 10 by NaOH solution adjust ph, then gets 10ml and 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, the black solid in pyroxylin film is collected, then centrifugal, washing, stand-by;
(2) preparation of Pd nano particle
(2.1) palladium salt is dissolved in HCl, is mixed with solution, take surfactant, be mixed with solution with deionized water, take reducing agent
,with deionized water dissolving, place in refrigerator, stand-by;
(2.2), get palladium salting liquid and surfactant respectively in 25ml vial, stir and evenly mix, then add reducing agent, after stirring and evenly mixing, stop stirring, leave standstill 3h;
(2.3), black precipitate is collected, centrifugal, washing, stand-by;
(3) preparation of Pd/NiCu alloy
(3.1), black solid that step (1) prepares and the black precipitate that step (2) prepares is got in 5ml absolute ethyl alcohol, ultrasonic 30min ~ 1h;
(3.2), centrifugal, washing, dry, obtain final black product Pd/NiCu nano composite material.
In the present invention, described nickel chloride is NiCl
26H
2o, concentration is 50mmol/L; Described copper chloride is CuCl
22H
2o, concentration is 50 ~ 20mmol/L.
In the present invention, it is obtained that pyroxylin film used is that pyroxylin solution dries.
In the present invention, the Ni described in step (1.1)
2+and Cu
2+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 use deionized water and absolute ethyl alcohol to carry out alternately washing.
In the present invention, described stirring is ultrasonic vibration or magnetic agitation, and 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 dry 4h at vacuum drying chamber 60 DEG C.
In the present invention, described palladium salt is palladium bichloride, 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 (SEM), high resolution transmission electron microscopy (TEM) can be selected respectively, energy chromatograph (EDS) etc. characterizes, SEM, TEM characterize the microstructure of nano material, and EDS shows the constituent of product.
In the present invention, the present invention adopts simple chlorate as reactant respectively, has very strong versatility.
Product prepared by the present invention has good electrical chemical property, has comparatively vast potential for future development and application space in the electrode material of fuel cell.
Accompanying drawing explanation
Fig. 1,2 is in embodiment 1 1) the SEM figure of step products therefrom.
Fig. 3,4 is in embodiment 2 1) the SEM figure of step products therefrom.
Fig. 5,6 is in embodiment 1,2,3 2) the TEM figure of step products therefrom.
Fig. 7 is in embodiment 1 3) the TEM figure of step products therefrom.
Fig. 8 is in embodiment 2 3) the TEM figure of step products therefrom.
Fig. 9 is in embodiment 1 3) the EDS figure of step products therefrom.
Figure 10 is in embodiment 2 3) the EDS figure of step products therefrom.
Figure 11 is in embodiment 3 1) the SEM figure of step products therefrom.
Figure 12 is in embodiment 3 3) the SEM figure of step products therefrom.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1:
1) preparation of two-dimentional NiCu alloy
The first step, accurately takes 0.1185gNiCl
26H
2o, is mixed with 100ml solution with deionized water, and concentration is 50mmol/L, accurately takes 0.0340gCuCl
22H
2o, is mixed with 100ml solution with deionized water, and concentration is 20mmol/L, Ni
2+: Cu
2+mix according to 1:1 mol ratio, cumulative volume is 10ml, is then placed in the pyroxylin film of conical flask pattern, then adds 1mg PVP in pyroxylin film, is filled with argon gas, and then sealing is placed in 150ml beaker.
Second step, accurately takes the potassium borohydride of 0.162g, is mixed with 100ml solution with deionized water, and concentration is 30mmol/L, uses 0.2molL
-1naOH regulate PH ~ 10, then get 10ml in the beaker of the first step, with sealed membrane beaker envelope get up.
3rd step, after the reaction 5h time, collects the black solid in pyroxylin film, and then centrifugal, washing is once, stand-by.
2) preparation of Pd nano particle
The first step, accurately takes 44.5mgPdCl
2be dissolved in the HCl of 25ml 0.02M, be mixed with the H of 0.01M
2pdCl
4solution.Accurately take 0.80g CTAC, be mixed with solution with deionized water, with 25ml volumetric flask constant volume.Accurately take the NaBH of 0.0038g
4,with deionized water dissolving, with 10ml volumetric flask constant volume, place refrigerator and cooled and hide, stand-by.
Second step, gets 0.01M 0.25ml H respectively
2pdCl
4solution and 0.1M 9.75ml CTAC, in 25ml vial, stir and evenly mix, and then add 0.01M 0.60ml NaBH
4, after stirring and evenly mixing, stop after 10s stirring, then leave standstill 3h.
3rd step, collects black precipitate, centrifugal, and washing is stand-by.
3) preparation of Pd/NiCu nano composite material
The first step, gets 1) in black solid and 2) in black precipitate in 5ml absolute ethyl alcohol, ultrasonic 30min.
Second step, centrifugal, washing, dry, obtain final black product Pd/NiCu nano composite material.
Fig. 1,2 is in embodiment 1 1) the SEM figure of step products therefrom different amplification.Fig. 5,6 is in embodiment 1 2) the TEM figure of step products therefrom.Fig. 7 is in embodiment 1 3) the TEM figure of step products therefrom.As can be seen from picture, the pattern of two-dimentional NiCu can be seen clearly, and the dispersion of Pd nano particle is very even, and do not have agglomeration, in the TEM of the Pd/NiCu nano composite material of formation, the good load of Pd particle is on NiCu alloy, and does not reunite.Fig. 9 is in embodiment 1 3) the EDS figure of step products therefrom.
Embodiment 2:
1) preparation of two-dimentional NiCu alloy
The first step, accurately takes 0.1185gNiCl
26H
2o, is mixed with 100ml solution with deionized water, and concentration is 50mmol/L, accurately takes 0.0850gCuCl
22H
2o, is mixed with 100ml solution with deionized water, and concentration is 50mmol/L, Ni
2+: Cu
2+mix according to 4:1 mol ratio, cumulative volume is 10ml, is then placed in the pyroxylin film of conical flask pattern, then adds 1mg PVP in pyroxylin film, is filled with argon gas, and then sealing is placed in 150ml beaker.
Second step, accurately takes the potassium borohydride of 0.27g, is mixed with 100ml solution with deionized water, and concentration is 50mmo/L, uses 0.2molL
-1naOH regulate PH be 10, then get 10ml in the beaker of the first step, with sealed membrane beaker envelope get up.
3rd step, after the reaction 5h time, collects the black solid in pyroxylin film, and then centrifugal, washing is once, stand-by.
2) preparation of Pd nano particle
The first step, accurately takes 44.5mgPdCl
2be dissolved in the HCl of 25ml 0.02M, be mixed with the H of 0.01M
2pdCl
4solution.Accurately take 0.80g CTAC, be mixed with solution with deionized water, with 25ml volumetric flask constant volume.Accurately take the NaBH of 0.0038g
4,with deionized water dissolving, with 10ml volumetric flask constant volume, place refrigerator and cooled and hide, stand-by.
Second step, gets 0.01M 0.25ml H respectively
2pdCl
4solution and 0.1M 9.75ml CTAC, in 25ml vial, stir and evenly mix, then
Add 0.01M 0.60ml NaBH
4, after stirring and evenly mixing, stop after 10s stirring, then leave standstill 3h.
3rd step, collects black precipitate, centrifugal, and washing is stand-by.
3) preparation of Pd/NiCu nano composite material
The first step, gets 1) in black solid and 2) in black precipitate in 5ml absolute ethyl alcohol, ultrasonic 30min.
Second step, centrifugal, washing, dry, obtain final black product Pd/NiCu nano composite material.
Fig. 3,4 is in embodiment 2 1) the SEM figure of step products therefrom different amplification.Fig. 5,6 is in embodiment 2 2) the TEM figure of step products therefrom.Fig. 8 is in embodiment 2 3) the TEM figure of step products therefrom.As can be seen from picture, the pattern of two dimension NiCu also can be seen clearly, it is fine that film tiles, illustrate that the increase of Ni content is conducive to the formation of film, the dispersion of Pd nano particle is very even, do not have agglomeration, in the TEM of the Pd/NiCu nano composite material of formation, the load of Pd uniform particle is on NiCu alloy, and does not reunite.Just the amount of the Pd particle of load is a lot, and Figure 10 is in embodiment 1 3) the EDS figure of step products therefrom, can find out that the ratio of Pd is very large, illustrate in Pd load a lot.
Embodiment 3:
1) preparation of two-dimentional NiCu alloy
The first step, accurately takes 0.1185gNiCl
26H
2o, is mixed with 100ml solution with deionized water, and concentration is 50mmol/L, accurately takes 0.0340gCuCl
22H
2o, is mixed with 100ml solution with deionized water, and concentration is 20mmol/L, Ni
2+: Cu
2+mix according to 7:2 mol ratio, cumulative volume is 10ml, is then placed in the pyroxylin film of conical flask pattern, then adds 1mg PVP in pyroxylin film, is filled with argon gas, and then sealing is placed in 150ml beaker.
Second step, accurately takes the potassium borohydride of 0.162g, is mixed with 100ml solution with deionized water, and concentration is 30mmol/L, uses 0.2molL
-1naOH regulate PH ~ 10, then get 10ml in the beaker of the first step, with sealed membrane beaker envelope get up.
3rd step, after the reaction 5h time, collects the black solid in pyroxylin film, and then centrifugal, washing is once, stand-by.
2) preparation of Pd nano particle
The first step, accurately takes 44.5mgPdCl
2be dissolved in the HCl of 25ml 0.02M, be mixed with the H of 0.01M
2pdCl
4solution.Accurately take 0.80g CTAC, be mixed with solution with deionized water, with 25ml volumetric flask constant volume.Accurately take the NaBH of 0.0038g
4,with deionized water dissolving, with 10ml volumetric flask constant volume, place refrigerator and cooled and hide, stand-by.
Second step, gets 0.01M 0.25ml H respectively
2pdCl
4solution and 0.1M 9.75ml CTAC, in 25ml vial, stir and evenly mix, then
Add 0.01M 0.60ml NaBH
4, after stirring and evenly mixing, stop after 10s stirring, then leave standstill 3h.
3rd step, collects black precipitate, centrifugal, and washing is stand-by.
3) preparation of Pd/NiCu nano composite material
The first step, gets 1) in black solid and 2) in black precipitate in 5ml absolute ethyl alcohol, ultrasonic 30min.
Second step, centrifugal, washing, dry, obtain final black product Pd/NiCu nano composite material.
Figure 11 is in embodiment 3 1) the SEM figure of step products therefrom.Figure 12 is in embodiment 3 3) the SEM figure of step products therefrom.What can be clear that load on NiCu alloy film from Figure 12 has Pd particle.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, the amendment made when not departing from category of the present invention is all within protection scope of the present invention.
Claims (13)
1. a preparation method for Pd/NiCu two-dimensional nano composite material, is characterized in that: concrete steps are as follows:
(1) preparation of two-dimentional NiCu alloy
(1.1), take nickel chloride and copper chloride respectively, be respectively mixed with solution with deionized water, by Ni
2+with Cu
2+the mol ratio of 4:1 ~ 1:1 mixes, and is then placed in the pyroxylin film of conical flask pattern, then adds 1mg surfactant, is filled with argon gas, and then sealing is placed in 150ml beaker;
(1.2), taking reducing agent, be mixed with solution with deionized water, is 10 by NaOH solution adjust ph, then gets 10ml and 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, the black solid in pyroxylin film is collected, then centrifugal, washing, stand-by;
(2) preparation of Pd nano particle
(2.1) palladium salt is dissolved in HCl, is mixed with palladium salting liquid, takes surfactant, be mixed with surfactant solution with deionized water, take reducing agent
,with deionized water dissolving, obtain reductant solution, place in refrigerator, stand-by;
(2.2), get palladium salting liquid and surfactant solution respectively in 25ml vial, stir and evenly mix, then add reductant solution, after stirring and evenly mixing, stop stirring, leave standstill 3h;
(2.3), black precipitate is collected, centrifugal, washing, stand-by;
(3) preparation of Pd/NiCu alloy
(3.1), black solid that step (1) prepares and the black precipitate that step (2) prepares is got in 5ml absolute ethyl alcohol, ultrasonic 30min ~ 1h;
(3.2), centrifugal, washing, dry, obtain final black product Pd/NiCu nano composite material.
2. preparation method according to claim 1, is characterized in that described nickel chloride is NiCl
26H
2o, concentration is 50mmol/L, and described copper chloride is CuCl
22H
2o, concentration is 50 ~ 20mmol/L.
3. preparation method according to claim 1, is characterized in that pyroxylin film used is that pyroxylin solution dries obtained.
4. preparation method according to claim 1, is characterized in that Ni in step (1.1)
2+and Cu
2+cumulative volume be 10ml.
5. preparation method according to claim 1, is characterized in that the surfactant in step (1.1) is PVP.
6. preparation method according to claim 1, is characterized in that step (1.3), (2.3) and the washing described in (3.2) are all use deionized water and absolute ethyl alcohol to carry out alternately washing.
7. preparation method according to claim 1, it is characterized in that stirring described in step (2.2) as ultrasonic vibration or magnetic agitation, the time is 30 ~ 60 minutes.
8. preparation method according to claim 1, it is characterized in that in step (3.2), centrifugation rotating speed is 6000 revs/min, the time is 5 minutes.
9. preparation method according to claim 1, is characterized in that in step (3.2), drying is dry 4h at vacuum drying chamber 60 DEG C.
10. preparation method according to claim 1, it is characterized in that the palladium salt in step (2.1) is palladium bichloride, the concentration of its wiring solution-forming is 0.01mol/L.
11. preparation methods according to claim 1, it is characterized in that the surfactant in step (2.1) is CTAC, its concentration is 0.1mol/L.
12. preparation methods according to claim 1, is characterized in that step (2.1), and the reducing agent in (2.2) is sodium borohydride, and its concentration is 0.01mol/L.
13. preparation methods according to claim 1, is characterized in that step (1.1), and the reducing agent in (1.2) is potassium borohydride, and its concentration is 30 ~ 50mmol/L.
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| CN114944492A (en) * | 2022-01-28 | 2022-08-26 | 上海应用技术大学 | Preparation method of two-dimensional ultrathin nano composite material |
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