CN114944492A - Preparation method of two-dimensional ultrathin nano composite material - Google Patents

Preparation method of two-dimensional ultrathin nano composite material Download PDF

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CN114944492A
CN114944492A CN202210106183.XA CN202210106183A CN114944492A CN 114944492 A CN114944492 A CN 114944492A CN 202210106183 A CN202210106183 A CN 202210106183A CN 114944492 A CN114944492 A CN 114944492A
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nico
nicopt
inorganic salt
shaped pipe
collodion
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吴丹丹
袁微
麻云磊
江国健
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Shanghai Institute of Technology
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • H01M4/88—Processes of manufacture
    • 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 invention discloses a preparation method of a two-dimensional ultrathin nano composite material, which comprises the following steps: placing a collodion liquid film in the middle of a U-shaped pipe, adding an inorganic salt mixed solution containing Ni, Co and Pt into one side of the U-shaped pipe, adding a potassium borohydride solution into the other side of the U-shaped pipe, and separating the two sides by the collodion liquid film; and after the reaction is finished, collecting a black product on the side of the tube containing the metal ions, thoroughly cleaning the black product by using distilled water and ethanol, and drying the black product in vacuum to obtain the final product, namely the two-dimensional ultrathin NiCoPt/NiCo nanocomposite. The invention prepares NiCoPt/NiCo nano structure by one-step method of artificial active collodion semipermeable membrane, and then obtains two-dimensional ultrathin NiCoPt/NiCo nano composite material by drying treatment in vacuum. The composite material is dispersed by two-dimensional ultrathin NiCo nanosheets, has high activity and long-term stability, and the preparation method disclosed by the invention is safe and simple in operation process and easy to control.

Description

Preparation method of two-dimensional ultrathin nano composite material
Technical Field
The invention relates to a preparation method of a two-dimensional ultrathin NiCoPt/NiCo nano composite material, belonging to the technical field of composite materials.
Background
In fuel cells and metal-air cells, to avoid the production of intermediate products H 2 O 2 The impact on cell structure, increasing cell efficiency, requires that the catalyst must be a four electron transfer directly to the final product. It was found that the best ORR catalyst was also a noble metal Pt based catalyst. However, the reserves of the platinum on the earth are small, the distribution is extremely uneven, the exploitation difficulty is high, the cost of the platinum catalyst is extremely high, and the large-scale application of the fuel cell is seriously hindered. Therefore, it is necessary to research an electrocatalyst with low Pt loading and excellent ORR electrical activity, which can further increase the electrochemical specific surface area of Pt-based materials and obtain higher active site exposure.
The two-dimensional nanosheet is a novel nanomaterial, particularly an ultrathin two-dimensional nanostructure, and has attracted extensive attention in the fields of catalysis, optics, electricity and the like. Because of strong coupling in and out of planes among atoms in the structure of the ultrathin two-dimensional nano material, the ultrathin two-dimensional nano material has unique electron transfer performance and shows unique catalytic activity in electrocatalysis; and also provides abundant absorption sites for reactive substances in electrocatalysis due to the ultrahigh specific surface area of the catalyst.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to improve O of two-dimensional ultrathin nano composite material 2 The activity and stability of the electrocatalyst is reduced.
In order to solve the problems, the technical scheme of the invention is as follows:
a preparation method of a two-dimensional ultrathin nano composite material comprises the following steps: placing a collodion liquid film in the middle of a U-shaped pipe, adding an inorganic salt mixed solution containing Ni, Co and Pt into one side of the U-shaped pipe, adding a potassium borohydride solution into the other side of the U-shaped pipe, and separating the two sides by the collodion liquid film; and after the reaction is finished, collecting a black product on the side of the tube containing the metal ions, thoroughly cleaning the black product by using distilled water and ethanol, and drying the black product in vacuum to obtain the final product, namely the two-dimensional ultrathin NiCoPt/NiCo nanocomposite.
Preferably, the collodion liquid film is prepared by dripping collodion liquid solution on a silicon-based spin coater, and is naturally dried for later use.
Preferably, the rotating speed of the silicon-based spin coater is 1000 r/min; the preparation time of the collodion liquid film is continuous for 15 s; the thickness of the collodion liquid film is 0.2-0.5 mm.
Preferably, the inorganic salt mixed solution containing Ni, Co and Pt is an aqueous solution; the concentrations of the inorganic salt solutions of Ni, Co and Pt are all 0.005 mol/L; wherein the molar ratio of the Ni-containing inorganic salt to the Co-containing inorganic salt to the Pt-containing inorganic salt is 7:7: 6.
Preferably, the concentration of the potassium borohydride solution is 0.02mol/L, and the pH value is 12.
Preferably, the volume ratio of the inorganic salt mixed solution containing Ni, Co and Pt to the potassium borohydride solution is 1: 1.
Preferably, the reaction time is 5-8 h.
Preferably, the drying temperature is 60 ℃ and the drying time is 4-8 h.
The invention prepares NiCoPt/NiCo nano structure by one-step method of artificial active collodion semipermeable membrane, and then obtains two-dimensional ultrathin NiCoPt/NiCo nano composite material by drying treatment in vacuum. The composite material is dispersed by two-dimensional ultrathin NiCo nanosheets, has high activity and long-term stability, and the preparation method disclosed by the invention is safe and simple in operation process and easy to control.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention realizes the first synthesis of the two-dimensional ultrathin NiCoPt/NiCo nanocomposite by using common nickel chloride, cobalt chloride and chloroplatinic acid as precursors of reaction and by using an active collodion semipermeable membrane one-step method.
2. The method of the invention has high regulation and control performance on the appearance of the product.
3. The invention adopts simple inorganic salt as reactant and has strong universality.
4. The product prepared by the invention has high activity and long-term stability, and the research opens up a new way for designing a fuel cell catalyst with a two-dimensional nano alloy heterostructure with excellent activity and stability.
5. The method has the advantages of simple process, universal preparation conditions, stable product appearance, high purity and convenient and simple product treatment, and is suitable for medium-scale industrial production.
6. The method has the characteristics of mild conditions, energy conservation, high efficiency, easy control and the like.
Drawings
FIGS. 1A, 1B are TEM and SEM images, respectively, of a 60% Pt-containing NiCoPt/NiCo nanocomposite material of example 1;
FIGS. 2A, 2B, 2C, 2D are a TEM, HETEM, EDS, and XRD spectra, respectively, of a 60% Pt NiCoPt/NiCo nanocomposite in example 1;
FIG. 3A is an XPS spectrum of a NiCoPt/NiCo nanocomposite with 60% Pt content as in example 1;
FIGS. 3B, 3C, 3D are XPS spectra of Pt 4f, Co 2p, Ni 2p, respectively, for a NiCoPt/NiCo nanocomposite material of example 1 having a Pt content of 60%;
FIG. 4A is a LSV polarization curve for a NiCoPt/NiCo nanocomposite and a commercial Pt catalyst surface, curves a 'and b' representing the corresponding Pt loop current (0.7V polarization);
FIG. 4B is a Tafel slope plot of NiCoPt/NiCo nanocomposites and commercial Pt catalyst; the specific test conditions were: at O 2 Saturated 0.1M HCLO 4 In the solution, the sweeping speed is 10mV/s, and the rotating speed is 200 rpm;
FIG. 5 is a graph comparing the stability test curves of the NiCoPt/NiCo nanocomposite of example 1 and a commercial Pt catalyst under different conditions; wherein A is NiCoPt/NiCo nano composite material in N 2 Saturated 0.5M H 2 SO 4 In the electrolyte, the sweep rate is a CV curve of 100mV/s, and B is NiCoPt/NiCo nano composite material in O 2 Saturated 0.1M HCLO 4 Sweeping an LSV polarization curve with the sweep rate of 10mV/s in the electrolyte; c is commercial Pt catalyst in N 2 Saturated 0.5M H 2 SO 4 In the electrolyte, the sweep rate is 100mV/s CV curve, D is the commercial Pt catalyst in O 2 Saturated 0.1M HCLO 4 Sweeping an LSV polarization curve with the sweep rate of 10mV/s in the electrolyte;
FIGS. 6A, 6B, 6C are TEM, SEM, XRD patterns, respectively, of a 6% Pt/NiCo nanocomposite in example 2;
FIGS. 7A, 7B, 7C are TEM, SEM, XRD patterns, respectively, of a NiCoPt/NiCo nanocomposite with 90% Pt content as in example 3.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
The drugs used in the examples are shown in Table 1. Examples the equipment used are shown in table 2.
TABLE 1
Name of reagent Chemical formula (II) Specification of Manufacturer of the product
Nickel chloride hexahydrate NiCl 2 ·6H 2 O 98％ Group of traditional Chinese medicines
Cobalt chloride hexahydrate CoCl 2 ·6H 2 O 99％ Group of traditional Chinese medicines
Chloroplatinic acid hexahydrate H 2 PtCl 6 ·6H 2 O 99％ Group of traditional Chinese medicines
Sodium hydroxide NaOH 96％ Group of traditional Chinese medicines
Potassium borohydride KBH 4 95％ Group of national herbs
Anhydrous ethanol C 2 H 5 OH AR Group of traditional Chinese medicines
TABLE 2
Name of instrument and equipment Manufacturer of life Model number Origin of birth
Vacuum drying oven Hengscientific instruments Co Ltd DZF-6020 China
Electronic analytical balance Mettler-Tollido Shanghai Instrument Equipment Co Ltd AB-104～N China
High-speed centrifugal machine Shanghai Pigeon instruments Co Ltd TDL-60B China
Electric heating constant temperature blast air drying box Fine Equipment Ltd DHG-9076A China
Example 1
The first step is as follows: 100mL of 5mM H was prepared 2 PtCl 6 ·6H 2 O aqueous solution, 100mL of 5mM CoCl 2 ·6H 2 O aqueous solution, 100mL of 5mM NiCl 2 ·6H 2 O aqueous solution and 100mL of 20mM KBH 4 Preparing collodion liquid film by adopting a silicon-based spin coater, and naturally drying for later use.
The second step is that: and (2) according to a molar ratio of 7:7:6 sequence NiCl was added to one side of the U-tube 2 ·6H 2 O、CoCl 2 ·6H 2 O and H 2 PtCl 6 ·6H 2 10mL of O mixed solution, and KBH of pH 12 added to the other side 4 And after the reaction is finished, centrifuging the side of the tube containing the metal ions to collect a black product, thoroughly cleaning the black product by using distilled water and ethanol, re-dispersing the final product in the ethanol for storage, and directly separating out the NiCoPt/NiCo nano structure from the ethanol solution.
The third step: and drying the obtained product at 60 ℃ in vacuum for 4 hours, cooling to room temperature, taking out, sealing and storing for subsequent experiments.
FIGS. 1A, 1B are TEM and SEM images, respectively, of a 60% Pt-containing NiCoPt/NiCo nanocomposite material of example 1.
FIGS. 2A, 2B, 2C, 2D are a TEM, HETEM, EDS, and XRD spectra, respectively, of a NiCoPt/NiCo nanocomposite with 60% Pt content in example 1. It can be clearly observed from the electron microscope photograph that the NiCoPt nanoparticles are uniformly dispersed on the two-dimensional NiCo nanosheets to form a NiCoPt/NiCo nano structure. The existence of Ni, Co, Pt and O elements can be clearly seen from an EDS map, and the in-situ EDX spectra at the areas (a) and (b) are basically consistent with the component contents of the NiCo carrier and the NiCoPt particles, and further shows that the NiCoPt nanoparticles are uniformly dispersed on the surface of the NiCo nanosheets. Meanwhile, in an XRD pattern, two obvious diffraction peaks are positioned at 40.5 degrees (111) and 47.0 degrees (200) and are positioned between standard peaks of Pt (JCPDF 04-0802) and Ni (JCPDF 04-0850) & Co (JCPDF 15-0806), which indicates the existence of NiCoPt alloy. The HEMEM image in FIG. 2B also further confirms the formation of a NiCoPt alloy, and particles with a lattice spacing of about 0.23nm are clearly observed, which corresponds to the (111) plane spacing of the NiCoPtPt crystal.
FIG. 3A is an XPS spectrum of a NiCoPt/NiCo nanocomposite with 60% Pt content as in example 1; FIGS. 3B, 3C, 3D are XPS spectra of Pt 4f, Co 2p, Ni 2p, respectively, for a NiCoPt/NiCo nanocomposite material having a Pt content of 60% in example 1. The spectrum of Pt is shown in FIG. 3B, 4f 7/2 And 4f 5/2 The spin-orbit bimodal split results in two peaks at 72.1 and 74.8eV, with peak positions shifted to higher binding energies than previously reported values for metallic Pt. This is mainly due to the fact that after NiCoPt alloy is formed, Pt and Co&Electron transfer between Ni transfers the binding energy. FIG. 3C shows two spikes at 851.8eV and 870.7eV, which are attributed to the amplified spin-orbit splitting of Ni 2p by 2p 3/2 And 2p 1/2 . In FIG. 3D, two distinct peaks are observed at 778.6 and 794.0eV, respectively, due to the 2p of Co (0) 3/2 And 2p 1/2 Multiple state splitting of. Therefore, we can conclude that not only Pt but also Ni and Co are completely reduced in NiCoPt/NiCo nanostructures, all of which are in the metallic state.
FIG. 4A is a LSV polarization curve for a NiCoPt/NiCo nanocomposite and a commercial Pt catalyst surface, curves a 'and b' representing the corresponding Pt loop current (0.7V polarization); FIG. 4B is a Tafel slope plot for NiCoPt/NiCo nanocomposites and commercial Pt catalysts. From FIG. 4A, it can be seen that the NiCoPt/NiCo catalyst has a higher positive potential and a stronger activity than the Pt reference catalyst. It is evident from FIG. 4B that the NiCoPt/NiCo nanocomposites have a lower Tafel slope.
FIG. 5 is a graph comparing the stability test curves of the NiCoPt/NiCo nanocomposites of example 1 with commercial Pt catalysts under different conditions. As can be seen from the figure, compared with the Pt reference catalyst, the specific surface area of the electrochemical activity of the NiCoPt/NiCo catalyst is hardly changed after 30000 CV cycles, and the half-wave potential is only slightly attenuated, which indicates the good cycle stability of the NiCoPt/NiCo nano composite material.
Example 2
The first step is as follows: 100mL of 5mM H was prepared 2 PtCl 6 ·6H 2 O aqueous solution, 100mL of 5mM CoCl 2 ·6H 2 O aqueous solution, 100mL of 5mM NiCl 2 ·6H 2 O aqueous solution and 100mL of 20mM KBH 4 Preparing collodion liquid film by adopting a silicon-based spin coater, and naturally drying for later use.
The second step is that: according to the molar ratio of 25: 25: 1 sequence NiCl is added to one side of the U-tube 2 ·6H 2 O、CoCl 2 ·6H 2 O and H 2 PtCl 6 ·6H 2 10mL of O mixed solution, and KBH of pH 12 added to the other side 4 And after the reaction is finished, centrifuging the side of the tube containing the metal ions to collect a black product, thoroughly cleaning the black product by using distilled water and ethanol, re-dispersing the final product in the ethanol for storage, and directly separating out the NiCoPt/NiCo nano structure from the ethanol solution.
The third step: and drying the obtained product at 60 ℃ in vacuum for 4 hours, cooling to room temperature, taking out, sealing and storing for subsequent experiments.
FIGS. 6A, 6B, 6C are TEM, SEM, XRD patterns, respectively, of a NiCoPt/NiCo nanocomposite with 6% Pt content as in example 2. As can be seen from the figure, there are fewer NiCoPt nanoparticles dispersed in the NiCoPt/NiCo nanostructure. Meanwhile, the diffraction peaks of the crystalline NiCoPt (111) at 40.5 ° and (200)47 ° in the XRD pattern are not sufficiently pronounced.
Example 3
The first step is as follows: 100mL of 5mM H was prepared 2 PtCl 6 ·6H 2 O aqueous solution, 100mL of 5mM CoCl 2 ·6H 2 O aqueous solution, 100mL of 5mM NiCl 2 ·6H 2 O aqueous solution and 100mL of 20mM KBH 4 Preparing collodion liquid film by adopting a silicon-based spin coater, and naturally drying for later use.
The second step is that: and (3) according to molar ratio: 3: 14 sequence NiCl was added to one side of the U-tube 2 ·6H 2 O、CoCl 2 ·6H 2 O and H 2 PtCl 6 ·6H 2 10mL of O mixed solution, and KBH of pH 12 added to the other side 4 And after the reaction is finished, centrifuging the side of the tube containing the metal ions to collect a black product, thoroughly cleaning the black product by using distilled water and ethanol, re-dispersing the final product in the ethanol for storage, and directly separating out the NiCoPt/NiCo nano structure from the ethanol solution.
The third step: and drying the obtained product at 60 ℃ in vacuum for 4 hours, cooling to room temperature, taking out, sealing and storing for subsequent experiments.
FIGS. 7A, 7B, 7C are TEM, SEM, XRD patterns, respectively, of a NiCoPt/NiCo nanocomposite with 90% Pt content as in example 3. As can be seen from the figure, a large amount of NiCoPt nanoparticles are loaded on the NiCo nanosheets, and serious agglomeration phenomenon exists. Meanwhile, two sharp diffraction peaks corresponding to the crystalline NiCoPt (111) and (200) crystal planes can be clearly observed at 40.5 ° and 47 ° in the XRD pattern.

Claims (8)

1. A preparation method of two-dimensional ultrathin nanometer composite material is characterized in that collodion liquid films are placed in the middle of a U-shaped pipe, inorganic salt mixed solution containing Ni, Co and Pt is added into one side of the U-shaped pipe, potassium borohydride solution is added into the other side of the U-shaped pipe, and the middle parts of the U-shaped pipe and the U-shaped pipe are separated by the collodion liquid films; and after the reaction is finished, collecting a black product on the side of the tube containing the metal ions, thoroughly cleaning the black product by using distilled water and ethanol, and drying the black product in vacuum to obtain the final product, namely the two-dimensional ultrathin NiCoPt/NiCo nanocomposite.
2. The method of claim 1, wherein the collodion liquid film is prepared by dropping collodion liquid solution on a silicon-based spin coater, and drying naturally for use.
3. The method of claim 1, wherein the spin coater on silicon is rotated at 1000 r/min; the preparation time of the collodion liquid film is continuous 15 s; the thickness of the collodion liquid film is 0.2-0.5 mm.
4. The method of preparing a two-dimensional ultra-thin nanocomposite material according to claim 1, wherein the inorganic salt mixed solution containing Ni, Co, Pt is an aqueous solution; the concentrations of the inorganic salt solutions of Ni, Co and Pt are all 0.005 mol/L; wherein the molar ratio of the Ni-containing inorganic salt to the Co-containing inorganic salt to the Pt-containing inorganic salt is 7:7: 6.
5. The method of claim 1, wherein the potassium borohydride solution has a concentration of 0.02mol/L and a pH of 12.
6. The method for preparing a two-dimensional ultra-thin nanocomposite material according to claim 1, wherein the volume ratio of the inorganic salt mixed solution containing Ni, Co and Pt to the potassium borohydride solution is 1: 1.
7. The method for preparing a two-dimensional ultra-thin nanocomposite material according to claim 1, wherein the reaction time is 5 to 8 hours.
8. The method for preparing a two-dimensional ultra-thin nanocomposite material according to claim 1, wherein the drying temperature is 60 ℃ and the drying time is 4-8 hours.
CN202210106183.XA 2022-01-28 2022-01-28 Preparation method of two-dimensional ultrathin nano composite material Pending CN114944492A (en)

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