CN105214685B - A kind of platinum cobalt alloy structured catalysis material and preparation method thereof for electrolysis water - Google Patents
A kind of platinum cobalt alloy structured catalysis material and preparation method thereof for electrolysis water Download PDFInfo
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- CN105214685B CN105214685B CN201510579195.4A CN201510579195A CN105214685B CN 105214685 B CN105214685 B CN 105214685B CN 201510579195 A CN201510579195 A CN 201510579195A CN 105214685 B CN105214685 B CN 105214685B
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Abstract
本发明公开了一种用于电解水的铂钴合金结构催化材料，所述电解水催化材料是由催化活性物和载体组成，所述催化活性物为铂钴合金结构，所述载体为超细碳纤维，所述载体上催化活性物的负载量为2‑20 wt%。本发明为一种铂钴合金结构/超细碳纤维杂化材料，该杂化材料采用原位法制备铂钴合金。本发明为了在降低铂催化剂含量的同时提高其催化活性，所述载体选择了超细碳纤维。本发明的催化材料具有高比表面积和孔隙率，有利于电解液的扩散和气体脱附，铂钴合金的特性使得该材料具有较高的析氢活性，同时无需负载到电极上，可直接用做工作电极进行电催化制氢。The invention discloses a platinum-cobalt alloy structural catalytic material for water electrolysis. The electrolytic water catalytic material is composed of a catalytic active substance and a carrier, the catalytic active substance is a platinum-cobalt alloy structure, and the carrier is an ultra-fine Carbon fibers, the loading of catalytic actives on the carrier is 2-20 wt%. The invention is a platinum-cobalt alloy structure/ultrafine carbon fiber hybrid material, and the hybrid material adopts an in-situ method to prepare a platinum-cobalt alloy. In the present invention, in order to reduce the content of platinum catalyst and at the same time improve its catalytic activity, the carrier selects ultrafine carbon fiber. The catalytic material of the invention has high specific surface area and porosity, which is beneficial to the diffusion of electrolyte and gas desorption, and the characteristics of platinum-cobalt alloy make the material have high hydrogen evolution activity, and at the same time, it does not need to be loaded on the electrode, and can be directly used as The working electrode performs electrocatalytic hydrogen production.
Description
Technical field
The present invention relates to a kind of electrolysis water catalysis material, in particular to a kind of platinum cobalt alloy structured catalysis for electrolysis water
Material and preparation method thereof.
Background technique
Currently, Hydrogen Energy cleanliness without any pollution, and it is efficient, renewable, it is acknowledged as the following most potential energy carrier.Electricity
Solution water hydrogen manufacturing is one of a kind of efficient, cleaning and most promising method for preparing hydrogen.For water electrolysis hydrogen production, how to improve
The activity of electrode catalytic materials reduces overpotential of hydrogen evolution, and the stability and durability of raising electrode material are electro-catalysis necks
The emphasis and key of domain research.In recent years, the bimetallic catalyst of alloy structure is more next for the correlative study of water electrolysis hydrogen production
It is more, the utilization rate of metal can not only be improved, catalyst cost, and the electronic effect due to having between two kinds of metals are reduced
With synergistic effect catalytic performance is improved.It is well known that Pt and 3d transition metal (Ni, Fe, Co etc.) are prepared into alloy knot
Structure, this nanometer electrical catalyst show good catalytic activity and stability in electrocatalytic reaction.
Carbon nano-fiber (CNF) is the fibrous nano carbon material as made of the curling of Multi-layer graphite piece, since its is good
Characteristics, the potential applications such as mechanical property, light and high electric conductivity are compound in hydrogen storage material, high-capacity electrode material, high-performance
The fields such as material, fuel cell.As novel carbon material, CNF is due to acid-alkali-corrosive-resisting, large specific surface area, unique
The series of advantages such as surface texture have a wide range of applications in catalytic field.
So far, there are still more problems for electro-catalysis hydrogen preparation field for platinum cobalt alloy structure, one is 3d transition metal exists
Poor stability in acid solution, reduces the catalytic efficiency of catalyst；The second is the stability and recyclability problem of electrode.
The stability and cyclicity of electro catalytic electrode prepared by current various methods are often poor, therefore good conductive substrates load
Catalyst is vital for electro-catalysis.Therefore, how to design and prepare with high catalytic activity and good steady
Qualitative water electrolysis hydrogen production catalysis material is current urgent problem to be solved.
Summary of the invention
It is an object of the invention to solve disadvantages mentioned above of the existing technology, a kind of platinum cobalt conjunction for electrolysis water is provided
Golden structured catalysis material.
The present invention also provides the preparation methods of the platinum cobalt alloy structured catalysis material.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of platinum cobalt alloy structured catalysis material for electrolysis water, the electrolysis water catalysis material is by catalytic activity object
It is formed with carrier, the catalytic activity object is platinum cobalt alloy structure, and the carrier is ultrafine carbon fiber, is catalyzed and lives on the carrier
Property object load capacity be 2-20 wt%.The present invention is a kind of platinum cobalt alloy structure/ultrafine carbon fiber hybrid material, the hybrid material
Platinum cobalt alloy is prepared using in-situ method.Ultrafine carbon fiber presoma is configured to spinning solution first, then by the presoma of platinum and cobalt
It is dissolved in spinning solution.Spinning solution is prepared into ultrafine carbon fiber using electrostatic spinning technique, then using tube furnace to ultra-fine
Carbon fiber is carbonized, and platinum cobalt alloy structure/ultrafine carbon fiber hybrid material is formed in carbonisation.
For the present invention in order to improve its catalytic activity while reducing platinum catalyst content, the carrier has selected ultra-fine carbon
Fiber.Catalysis material of the invention has high-specific surface area and porosity, is conducive to diffusion and the desorbing gas of electrolyte, platinum cobalt
The characteristic of alloy makes material hydrogen evolution activity with higher, while without loading on electrode, can be directly with electricity of working
Pole carries out electro-catalysis hydrogen manufacturing.
Preferably, the platinum cobalt alloy structure is platinum cobalt alloy nanoparticles, particle size is 5-20 nm.It is described
Platinum cobalt alloy structure is coated by thin carbon layer, and carbon thin layer herein is not carrier, is a small amount of carbon packet in the preparation process of alloy
The thin layer that the surface of alloy is formed is overlayed on, as shown in the carbon layer in Fig. 2 f upper right illustration.
Preferably, the fineness of the ultrafine carbon fiber is 50-1000 nm.
A kind of preparation method of the platinum cobalt alloy structured catalysis material for electrolysis water, this method include following step
It is rapid: 1) ultrafine carbon fiber presoma to be made into the spinning solution that mass concentration is 5-15 % with n,N-Dimethylformamide, by platinum cobalt
The presoma of alloy is dissolved in spinning solution, and spinning solution is then prepared into ultrafine carbon fiber using method of electrostatic spinning；2) ultra-fine
Heat preservation pre-oxidation 3 hours after carbon fiber is warming up to 200-300 DEG C at room temperature, then under inert gas shielding and vacuum state
Continue to heat up, 800-1200 DEG C is warming up in 2 hours, heat preservation carbonization 5-12 hours is finally cooled under inert gas protection
Room temperature is to get platinum cobalt alloy structured catalysis material.The inert gas can choose common protective gas, such as argon gas.
Preferably, in step 1), control spinning voltage is 8-20 kV, reception device to spinning syringe needle when electrostatic spinning
Distance be 10-20 cm, solution flow velocity be 0.2 mL/h.
Preferably, the ultrafine carbon fiber presoma is polyacrylonitrile, polyethyleneimine, polyvinyl alcohol in step 1)
One or more of.
Preferably, the presoma of platinum is one of chloroplatinic acid, acetylacetone,2,4-pentanedione platinum or two in platinum cobalt alloy in step 1)
Kind.
Preferably, the presoma of cobalt is cobalt nitrate, in cobalt chloride, cobaltous sulfate, cobalt carbonate in platinum cobalt alloy in step 1)
One or more.
Preferably, the heating rate is 5 DEG C/min in step 2.
A kind of application of the platinum cobalt alloy structured catalysis material for electrolysis water, specifically: the platinum cobalt alloy
Catalyst of the structured catalysis material as the cathode catalysis liberation of hydrogen of electrolysis water.Electrolysis water catalysis material prepared by the present invention have compared with
High catalytic hydrogen evolution effect.
The beneficial effects of the present invention are:
(1) using the electronic effect and synergistic effect that have between two kinds of metals of alloy structure catalytic performance is improved,
Catalyst cost can be reduced simultaneously；
(2) electrolysis water catalysis material prepared by has high-specific surface area and porosity, be conducive to electrolyte diffusion and
Desorbing gas；
(3) it is acted on using the confinement of graphite linings in one-dimensional carbon material and induced growth, regulates and controls nano-interface structure, Ke Yijin
One step improves electro catalytic activity；
(4) ultrafine carbon fiber it is good can to assign hybrid material with effective protection platinum cobalt alloy from the erosion of electrolyte
Stability and durability；
(5) electrolysis water catalysis material can directly be used as electrode and carry out electro-catalysis hydrogen manufacturing without loading on electrode.
Detailed description of the invention
Fig. 1 is platinum cobalt alloy of the present invention/ultrafine carbon fiber (PtCo/CNFs) hybrid material microscopic appearance.(a-c):
The field emission scanning electron microscope photo of PtCo/CNFs, Pt/CNFs and Co/CNFs；(d, e) PtCo/CNFs transmission electron microscope photo is inserted
Figure is respectively the high score of the corresponding particle diameter distribution of platinum cobalt alloy nanoparticles and the platinum cobalt alloy being coated on inside ultrafine carbon fiber
Distinguish transmission electron microscope photo；(f): the energy spectrum diagram of PtCo/CNFs；
The electro catalytic activity of Fig. 2 electrolysis water catalysis material of the present invention.(a, b): CNFs, Co/CNFs, Pt/CNFs, quotient
Industry Pt/C (20 wt%) and PtCo/CNFs are in 0.5 M H2SO4In polarization curve and corresponding Tafel slope (catalyst
Load capacity is 212 μ g cm-2, sweep speed is 2 mV/s), and illustration is the PtCo/ overlayed on glass-carbon electrode (GCE) in a
CNFs catalyst generates the photo of hydrogen gas bubbles when 50mV is operated on its surface；(c): Co/CNFs, Pt/CNFs and PtCo/
The energy Qwest curve that CNFs is tested under open-circuit voltage；(d) PtCo/CNFs and business Pt/C (20 wt%) are followed at 1000 times
Polarization curve before and after ring test, illustration are the Cyclic voltamogram curve of PtCo/CNFs before and after loop test；(e)PtCo/
(catalyst loadings are 1 mg/cm to CNFs film2) time current response curve (j-t) in constant voltage -0.3V, illustration is
PtCo/CNFs catalyst generates the picture of hydrogen gas bubbles when test proceeds to 6 hours, and enlarged drawing refers to place shown in circle of dotted line；(f)
Corresponding high-resolution-ration transmission electric-lens photo in transmission electron microscope photo and illustration after PtCo/CNFs stability test.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention will be further explained in detail.In the present invention, if not
It refers in particular to, used raw material and equipment etc. are commercially available or commonly used in the art.Method in following embodiments, such as
It is the conventional method of this field without special instruction.
Embodiment 1:
0.15 g chloroplatinic acid and 0.1 g cobalt chloride is taken to be added to the N,N-dimethylformamide containing 3 g polyacrylonitrile
In solution (wherein the mass concentration of polyacrylonitrile is 12 %), spinning, control are then carried out to the spinning solution using method of electrostatic spinning
Spinning voltage processed is 15 kV, and the distance of reception device to spinning syringe needle is that receive distance be 15 cm to 15 cm(), solution flow velocity
For 0.2 mL/h to get arrive ultrafine carbon fiber.
By 500 mg ultrafine carbon fibers cut it is regular be placed in corundum boat, be then transferred to the heating part in tube furnace
Position is warming up to 230 DEG C in air first with 5 DEG C/min and maintains 3 hours.After opening argon gas 30 minutes, by temperature with 5
DEG C/min continue to heat up；After 2 hours, tubular type furnace temperature rises to 1000 DEG C, keeps the temperature 8 hours, finally cools down under protection of argon gas
To room temperature, platinum cobalt alloy/ultrafine carbon fiber hybrid material is obtained, which is the platinum cobalt alloy knot that the present invention is used for electrolysis water
Structure catalysis material, microscopic appearance are shown in Fig. 1.By the material directly as electrode, its electro-catalysis is tested in 0.5 M sulfuric acid solution
Hydrogen evolution activity, obtained data are as shown in Figure 2.
The electrolysis water catalysis material with platinum cobalt alloy structure obtained by this method, between two kinds of metals of alloy structure
Electronic effect and synergistic effect catalytic performance is improved, and ultrafine carbon fiber can with effective protection platinum cobalt alloy from electrolysis
The erosion of liquid assigns the good stability of hybrid material and durability.
Embodiment 2:
0.15 g acetylacetone,2,4-pentanedione platinum and 0.1 g cobalt carbonate is taken to be added to the N containing 1 g polyethyleneimine, N- dimethyl methyl
In amide solution (wherein the mass concentration of polyethyleneimine is 8 %), then the spinning solution is spun using method of electrostatic spinning
Silk, control spinning voltage are 8 kV, and the distance of reception device to spinning syringe needle is that receive distance be 10 cm to 10 cm(), solution
Flow velocity be 0.2 mL/h to get arrive ultrafine carbon fiber.
By 500 mg ultrafine carbon fibers cut it is regular be placed in corundum boat, be then transferred to the heating part in tube furnace
Position is warming up to 200 DEG C in air first with 5 DEG C/min and maintains 3 hours.After opening argon gas 30 minutes, by temperature with 5
DEG C/min continue to heat up；After 2 hours, tubular type furnace temperature rises to 800 DEG C, keeps the temperature 12 hours, finally cools down under protection of argon gas
To room temperature, platinum cobalt alloy/ultrafine carbon fiber hybrid material is obtained, which is the platinum cobalt alloy knot that the present invention is used for electrolysis water
Structure catalysis material.
Embodiment 3:
0.3 g chloroplatinic acid and 0.2 g cobalt carbonate is taken to be added to the N,N-dimethylformamide containing 5 g polyvinyl alcohol molten
In liquid (wherein the mass concentration of polyvinyl alcohol is 12 %), spinning, control are then carried out to the spinning solution using method of electrostatic spinning
Spinning voltage is 20 kV, and the distance of reception device to spinning syringe needle is that receive distance be 20 cm to 20 cm(), solution flow velocity is
0.2 mL/h to get arrive ultrafine carbon fiber.
By 500 mg ultrafine carbon fibers cut it is regular be placed in corundum boat, be then transferred to the heating part in tube furnace
Position is warming up to 300 DEG C in air first with 5 DEG C/min and maintains 3 hours.After opening argon gas 30 minutes, by temperature with 5
DEG C/min continue to heat up；After 2 hours, tubular type furnace temperature rises to 1200 DEG C, keeps the temperature 5 hours, finally cools down under protection of argon gas
To room temperature, platinum cobalt alloy/ultrafine carbon fiber hybrid material is obtained, which is the platinum cobalt alloy knot that the present invention is used for electrolysis water
Structure catalysis material.
Referring to the method for specific embodiment, the present invention according to the adjustable raw material of the scope of the claims, technological parameter etc.,
Prepare multiple material.Above-mentioned embodiment is only a preferred solution of the present invention, any shape not is made to the present invention
Limitation in formula, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (5)
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