CN115142071B - Flower-like catalyst, preparation method and application thereof - Google Patents
Flower-like catalyst, preparation method and application thereof Download PDFInfo
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- CN115142071B CN115142071B CN202210865341.XA CN202210865341A CN115142071B CN 115142071 B CN115142071 B CN 115142071B CN 202210865341 A CN202210865341 A CN 202210865341A CN 115142071 B CN115142071 B CN 115142071B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
- C25B11/061—Metal or alloy
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
- C25B11/081—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the element being a noble metal
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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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a flower-shaped catalyst, the grain diameter of which is 100-1000 nm, the spongy AlTi alloy with oxidized surface is used as a carrier, and flower-shaped platinum particles with the loading amount of 2-30% are used as active centers; the invention also discloses a preparation method of the flower-like catalyst, which is prepared by depositing flower-like platinum particles on an AlTi alloy carrier by an electrochemical deposition method and oxidizing Al on the surface of the carrier; the invention also discloses application of the flower-shaped catalyst in preparing hydrogen by electrocatalytic decomposition of water. The flower-like catalyst provided by the invention has higher stability and catalytic activity. The invention is suitable for preparing the flower-shaped catalyst, and the prepared flower-shaped catalyst is suitable for preparing hydrogen by electrocatalytic decomposition of water.
Description
Technical Field
The invention belongs to the technical field of catalysis, and relates to an electrocatalyst, in particular to a flower-shaped catalyst, a preparation method and application thereof.
Background
Today, environmental pollution and energy crisis are increasing, fossil fuel reserves are limited, and a series of researches for searching for alternative novel energy sources are initiated. Hydrogen is an environmentally friendly, resource-rich and energy-dense renewable energy source, and is one of the best alternatives to fossil fuels. The electrochemical water decomposition hydrogen production is a simple and efficient hydrogen production method and has wide development prospect. The design and development of high-performance and high-stability electrochemical water-splitting hydrogen production electrocatalyst is a key for improving the efficiency of an electrolytic water system.
As a very potential catalyst, commercial platinum carbon (Pt/C) catalysts exhibit excellent activity in electrocatalytic hydrogen evolution. However, in the acidic electrolyte condition, the acidic substance has a certain corrosion effect on the carbon carrier, which further causes the falling off and aggregation of Pt particles, reducing the stability of the catalyst. In addition, in the hydrogen evolution process of the electrolyzed water, the active center Pt has strong adsorption on intermediate products in the hydrogen evolution reaction process, so that the hydrogen evolution reaction rate is reduced to a certain extent, and the stability of the catalyst is improved by reasonably designing the catalyst structure; meanwhile, reducing the adsorption strength of the reaction intermediate product on the active site is an effective method for obtaining the high-performance hydrogen production gas electrocatalyst by decomposing water.
Disclosure of Invention
The invention aims to provide a flower-shaped catalyst which has acid corrosion resistance and simultaneously further improves the stability and catalytic activity of the catalyst;
the invention also aims to provide a preparation method of the flower-shaped catalyst, which is simple and convenient, has low cost, does not need any template agent and does not need post-treatment process;
it is also an object of the present invention to provide the use of the above flower-like catalyst.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the flower-shaped catalyst is formed by directionally assembling flower-shaped platinum particles, the particle size is 100-1000 nm, the flower-shaped catalyst is formed by directionally assembling flower-shaped platinum particles by taking spongy AlTi alloy with oxidized surfaces as a carrier and taking flower-shaped platinum particles with the loading amount of 2-30% as active centers, and the flower-shaped platinum particles are uniformly dispersed on the spongy AlTi alloy carrier with oxidized surfaces.
The invention also provides a preparation method of the flower-like catalyst, which comprises the following steps in sequence:
s1, preparation of an AlTi alloy carrier:
soaking spongy AlTi alloy in an acidic solution to obtain an AlTi alloy carrier;
preparation of Pt/AlTi intermediate
Taking an AlTi alloy carrier as a working electrode, taking Pt wires or Pt sheets as auxiliary electrodes, taking Ag-AgCl as a reference electrode, taking perchloric acid solution containing a platinum metal precursor and a directional growth agent as electrolyte, and carrying out electrochemical deposition to obtain a Pt/AlTi intermediate;
s3, preparation of flower-like catalyst
Heating the Pt/AlTi intermediate to form an AlTi alloy surface oxide layer to obtain Pt/Al 2 O 3 And (3) an AlTi catalyst, namely the flower-like catalyst.
In step S1, the sponge-like AlTi alloy is prepared by 3D printing, and the mass ratio of metal aluminum to metal titanium is 10:1-10;
the soaking time is 1h-24h, and stirring is carried out in the soaking process;
the acid solution is at least one of hydrochloric acid and sulfuric acid, the concentration of the hydrochloric acid is 0.5-5 mol/L, and the concentration of the sulfuric acid is 0.5-5 mol/L.
As another limitation, in step S2, the platinum metal precursor is at least one of chloroplatinic acid, platinum acetylacetonate, and ammonium chloroplatinate;
the directional growth agent is SO with anions 3 2- 、HSO 3 - Or H 2 PO 2 - At least one of the salts of (a) or ammonia;
the concentration of the platinum metal precursor in the electrolyte is 0.01-2.0 mol/L, the concentration of the directional growth agent is 0.01-0.1 mol/L, and the concentration of perchloric acid is 0.05-0.2 mol/L;
the electrochemical deposition method comprises cyclic voltammetry, potentiostatic deposition, galvanostatic deposition or pulse deposition.
As a further limitation, the cyclic voltammetry has a potential of-0.1 to 0.2V;
the potential of the constant potential deposition method is-0.1V;
the constant current deposition method has the current of 0.01-0.5 mA/cm 2 ；
The pulse deposition method was performed at 0v for 0.05s; -0.1v,0.05s;0V,0.05s; 0.1V,0.05s is one cycle, 20 cycles.
As a third limitation, in the step S3, the heating is performed in air or oxygen with a volume fraction of 10-100%, the temperature is 60-250 ℃ and the time is 0.2-12 h.
The invention also provides application of the flower-shaped catalyst, and the flower-shaped catalyst is used for preparing hydrogen by electrocatalytic decomposition of water.
By adopting the technical scheme, compared with the prior art, the invention has the following technical progress:
(1) the flower-like catalyst provided by the invention, al formed on the surface of a carrier 2 O 3 The oxidation layer has outstanding acid corrosion resistance, and can effectively inhibit the corrosion of the carrier, thereby inhibiting the falling off and agglomeration of the Pt nanocrystalline in the active center, and effectively improving the stability of the catalyst; the AlTi alloy carrier adjusts the electronic structure of the Pt active center through the electronic effect, accelerates the desorption rate of the hydrogen evolution reaction intermediate product from the surface of the catalyst in the process of preparing hydrogen by electrocatalytic decomposition of water, and further effectively improves the activity of the catalyst; in conclusion, the flower-shaped catalyst has higher chemical reaction rate and stability when catalyzing electrolysis of water to prepare hydrogen;
(2) according to the preparation method provided by the invention, the 3D printed three-dimensional titanium-aluminum alloy is used as a carrier, and the three-dimensional titanium-aluminum alloy is subjected to acid treatment and platinized, so that the transmission of reactants and products is facilitated;
(3) the preparation method provided by the invention utilizes the electrochemical deposition method to prepare the Pt/AlTi intermediate, and has the beneficial effects of controllable conditions, simple preparation method, low cost and the like;
(4) according to the preparation method provided by the invention, the perchloric acid solution containing the platinum metal precursor and the directional growth agent is used as the electrolyte, no template agent is needed to control the shape of the nanocrystalline, and post-treatment processes such as template agent removal, heat treatment and the like are not needed, so that the whole preparation process is simple and convenient to operate, low in cost and easy for mass production.
The invention is suitable for preparing the flower-shaped catalyst, and the prepared flower-shaped catalyst is suitable for preparing hydrogen by electrocatalytic decomposition of water.
Drawings
The invention will be described in more detail below with reference to the attached drawings and specific examples:
FIG. 1 shows the Pt/Al catalyst obtained in example 1 2 O 3 Field emission scanning electron microscope image of/AlTi;
FIG. 2 shows the Pt/Al catalyst obtained in example 1 2 O 3 Transmission electron microscopy of AlTi;
FIG. 3 shows the Pt/Al catalyst obtained in example 1 2 O 3 High angle annular dark field transmission electron microscopy of AlTi;
FIG. 4 shows the Pt/Al catalyst obtained in example 2 2 O 3 X-ray diffraction pattern of AlTi;
FIG. 5 shows the Pt/Al catalyst obtained in example 2 2 O 3 X-ray photoelectron spectroscopy of AlTi and commercial Pt/C;
FIG. 6 shows the Pt/Al catalyst obtained in example 1 2 O 3 Comparison of catalytic stability of AlTi and comparative sample commercial Pt/C;
FIG. 7 is a catalyst Pt/Al obtained in example 2 2 O 3 Electrocatalytic hydrogen evolution reactivity graphs of AlTi and comparative samples commercial Pt/C.
Detailed Description
In order to make the present application solution better understood by those skilled in the art, the following description will be made in detail and with reference to the accompanying drawings in the embodiments of the present application, it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, shall fall within the scope of the present application.
Example 1 preparation of a flower-shaped catalyst
The embodiment comprises the following steps sequentially carried out:
preparation of S1.AlTi alloy Carrier
2g of spongy 3D printed AlTi alloy (the mass ratio of metal aluminum to metal titanium is 10:1) is taken and soaked in 200ml of sulfuric acid solution with the concentration of 2mol/L for 5 hours under stirring, so that partial oxide layers formed on the surface of the AlTi alloy are removed, and an AlTi alloy carrier is obtained;
preparation of Pt/AlTi intermediate
S21. Weighing 2.7g of ammonium chloroplatinate and 1.76g of NaH 2 PO 2 Dissolving in 200ml perchloric acid water solution with concentration of 0.1M to obtain chloroplatinic acid (with concentration of 0.03 mol/L) containing platinum metal precursor and oriented growth agent NaH 2 PO 2 (concentration of 0.1 mol/L), namely an electrolyte;
s22, immersing all the AlTi alloy carrier serving as a working electrode into the electrolyte, taking Ag-AgCl as a reference electrode, taking Pt wires as a counter electrode (auxiliary electrode), reacting for 30min by a constant potential electrochemical deposition method under the potential of-0.1V (relative to a standard hydrogen electrode), and quantitatively depositing 0.12g of Pt (with the loading amount of 6%) on the carrier to obtain a Pt/AlTi intermediate;
s3, putting the Pt/AlTi intermediate into a drying box, and drying for 2 hours at 80 ℃ to enable the AlTi alloy to form a surface oxide layer to obtain the Pt/Al 2 O 3 AlTi catalyst, namely flower-like catalyst α1.
The field emission scanning electron microscope image of the flower-like catalyst alpha 1 is shown in FIG. 1, and the flower-like catalyst alpha 1 is formed by Pt/Al in FIG. 1 2 O 3 The scanning electron microscope picture of the AlTi catalyst shows that the Pt nanocrystalline is flower-shaped, the size is about 500nm, and the Pt nanocrystalline is uniformly distributed on the carrier;
the transmission electron microscope image of the flower-shaped catalyst alpha 1 is shown in fig. 2, and the high-angle annular dark field transmission electron microscope image of the flower-shaped catalyst alpha 1 is shown in fig. 3; as can be seen from fig. 2 and 3, the Pt nanocrystals in the flower-like catalyst α1 prepared in this example were flower-like and had a size of about 500 nm.
Examples 2 to 6 preparation of flower-like catalysts
Examples 2 to 6 are each a preparation method of a flower-like catalyst, which is basically the same as example 1, except that the raw material amounts and the process parameters are different, and specifically, see table 1:
table 1 list of process parameters in examples 2 to 6
Examples 2 to 6 were prepared as flower-like catalysts α2 to α6, respectively, wherein the X-ray diffraction pattern of the flower-like catalyst α2 is shown in fig. 4; as can be seen from FIG. 4, al 2 O 3 The AlTi carrier is amorphous, and Pt is in a polycrystalline structure;
x-ray photoelectron spectra of the flower-like catalyst alpha 2 and the commercial Pt/C are shown in FIG. 5; as can be seen from fig. 5, the binding energy of Pt in the flower-like catalyst α2 shifts to a lower binding energy than Pt/C.
Example 7 Performance test of flower-like catalyst
This example is a performance test of the flower-like catalysts prepared in examples 1 to 6, and specifically includes the following:
(1) Catalytic stability test
The commercial Pt/C catalyst (Pt loading 20 wt%) and the flower-like catalyst α1 prepared in example 1 were respectively taken for catalytic stability test by: ag/AgCl is used as a reference electrode, pt wire is used as a counter electrode, a flower-shaped catalyst is used as a working electrode, and 0.1M HClO is used 4 Recording the decay of current with time by adopting a potentiostatic method (-0.1V vs RHE) as electrolyte;
as shown in fig. 6, the stability of the flower-like catalyst α1 was significantly improved as compared with the commercial Pt/C catalyst (Pt loading of 20 wt%) as shown in fig. 6.
(2) Electrocatalytic hydrogen evolution reactivity test
The commercial Pt/C catalyst (Pt carrying amount is 20 wt%) and the flower-shaped catalyst alpha 2 prepared in example 2 are respectively taken for the electrocatalytic hydrogen evolution reaction activity test, and the test method is as follows: takes Ag/AgCl as a reference electrode, pt wire as a counter electrode and flower-shaped catalysisThe agent is a working electrode, and 0.1M HClO is used as a catalyst 4 Recording the change condition of current along with potential (-0.2-0.1V vs RHE) by using a polarization curve as electrolyte;
as shown in fig. 7, it is clear from fig. 7 that the activity of the flower-like catalyst α2 was superior to that of the commercial Pt/C catalyst in the case where the platinum loading was lower than that of the commercial Pt/C catalyst (Pt loading of 20 wt%).
As can be seen from fig. 6 and 7, compared with the conventional Pt/C catalyst, the hydrogen evolution activity and stability of the flower-shaped catalyst prepared by the method are both obviously improved, which indicates that the carrier can effectively optimize the electronic structure of Pt and improve the hydrogen evolution reaction rate of the catalyst; al formed on the surface of the support 2 O 3 The oxide layer has outstanding acid corrosion resistance, so that the stability of the catalyst is improved.
Claims (7)
1. The flower-shaped catalyst is characterized in that the particle size of the catalyst is 100-1000 nm, spongy AlTi alloy with oxidized surface is used as a carrier, and flower-shaped platinum particles with the mass loading of 2-30% are used as active centers.
2. The method for preparing a flower-like catalyst according to claim 1, comprising the following steps, which are sequentially performed:
s1, preparation of an AlTi alloy carrier:
soaking spongy AlTi alloy in an acidic solution to obtain an AlTi alloy carrier;
preparation of Pt/AlTi intermediate
Taking an AlTi alloy carrier as a working electrode, taking Pt wires or Pt sheets as auxiliary electrodes, taking Ag-AgCl as a reference electrode, taking perchloric acid solution containing a platinum metal precursor and a directional growth agent as electrolyte, and carrying out electrochemical deposition to obtain a Pt/AlTi intermediate;
s3, preparation of flower-like catalyst
Heating the Pt/AlTi intermediate to form an AlTi alloy surface oxide layer to obtain Pt/Al 2 O 3 And (3) an AlTi catalyst, namely the flower-like catalyst.
3. The method for preparing the flower-like catalyst according to claim 2, wherein in the step S1, the sponge-like AlTi alloy is prepared by a 3D printing method, and the mass ratio of the metal aluminum to the metal titanium is 10:1-10;
the soaking time is 1h-24h, and stirring is carried out in the soaking process;
the acid solution is at least one of hydrochloric acid and sulfuric acid, the concentration of the hydrochloric acid is 0.5-5 mol/L, and the concentration of the sulfuric acid is 0.5-5 mol/L.
4. The method for preparing a flower-like catalyst according to claim 2, wherein in step S2, the platinum metal precursor is at least one of chloroplatinic acid, platinum acetylacetonate, and ammonium chloroplatinate;
the directional growth agent is SO with anions 3 2- 、 HSO 3 - Or H 2 PO 2 - At least one of the salts of (a) or ammonia;
the concentration of the platinum metal precursor in the electrolyte is 0.01-2.0 mol/L, the concentration of the directional growth agent is 0.01-0.1 mol/L, and the concentration of perchloric acid is 0.05-0.2 mol/L;
the electrochemical deposition method comprises cyclic voltammetry, potentiostatic deposition, galvanostatic deposition or pulse deposition.
5. The method for preparing a flower-like catalyst according to claim 4, wherein the cyclic voltammetry has a potential of-0.1 to 0.2V;
the potential of the constant potential deposition method is-0.1V;
the constant current deposition method has a current of 0.01-0.5 mA/cm 2 ；
The pulse deposition method was performed at 0v for 0.05s; 0.1V,0.05s is one cycle, 20 cycles.
6. The method of preparing a flower-like catalyst according to any one of claims 2 to 5, wherein in step S3, the heating is performed in air or 10 to 100% by volume of oxygen at a temperature of 60 to 250 ℃ for a time of 0.2 to 12 hours.
7. The use of a flower-like catalyst according to claim 1, wherein the flower-like catalyst is used for electrocatalytic decomposition of water to hydrogen.
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| CN110575830A (en) * | 2019-09-12 | 2019-12-17 | 中国原子能科学研究院 | platinum-containing catalyst and preparation method and application thereof |
| CN111411386A (en) * | 2020-05-15 | 2020-07-14 | 北京工业大学 | Method for preparing platinum/titanium dioxide nanotube composite electrode by atomic layer deposition method |
| CN113373475B (en) * | 2021-05-31 | 2023-03-10 | 中国人民解放军空军勤务学院 | Platinum monatomic hydrogen oxidation reaction electrocatalyst based on reactant enrichment and preparation method thereof |
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