CN106745525B - Metal composite material, preparation method and application thereof - Google Patents
Metal composite material, preparation method and application thereof Download PDFInfo
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- CN106745525B CN106745525B CN201611088920.9A CN201611088920A CN106745525B CN 106745525 B CN106745525 B CN 106745525B CN 201611088920 A CN201611088920 A CN 201611088920A CN 106745525 B CN106745525 B CN 106745525B
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Abstract
The invention provides a metal composite material, a preparation method and application thereof, wherein the metal composite material comprises the following components: a three-dimensional support; and a metal composite oxide supported on a three-dimensional carrier; the metal composite oxide is formed from a nickel molybdenum oxide calcined at high temperature in a protective gas. Compared with the prior art, the metal composite material provided by the invention has higher catalytic activity when being used as a catalyst for water oxidation and urea oxidation.
Description
Technical Field
The invention belongs to the technical field of electrode materials, and particularly relates to a metal composite material, and a preparation method and application thereof.
Background
At present, fuel cells are no longer a new technology for developing countries, and are an important opportunity for realizing low-carbon economy globally. A fuel cell is a highly efficient clean power generation device that can convert chemical energy into electrical energy continuously by adding fuel. China relies heavily on coal-fired power plants to provide electricity, 80% of which comes from non-renewable energy coal and 19% of which comes from hydroelectric power generation, and the structure causes China to become the first major world-wide carbon dioxide emission country. Meanwhile, the Chinese population is 13 billion in the world first, and has a lot of carbon emissions in other manufacturing and household areas, so that these factors make China and even the whole world face great challenges in energy supply and safety. To solve these problems, various countries around the world have developed and implemented a renewable energy strategy, in which fuel cells are the most potential and promising option for overall marketization, and at the same time, surplus electricity can be used to produce hydrogen first and then used in fuel cell vehicles, which is a high-quality scheme for promoting low-carbon development. Therefore, the fuel cell is being commercialized in a 'point-to-face' manner in various regions, and the project of the fuel cell has been rapidly developed and recognized in power generation and grid support, transportation, cogeneration, and backup power and remote power generation, wherein korea has built the largest fuel cell power plant of the world with a power generation power as high as 11.2 MW; more than 1350 backup power fuel cells have been deployed in the united states; automobile manufacturers around the world (Benz, modern, Toyota, Honda, Ford, Nissan, and general) have begun to push the commercialization of Fuel Cell Electric Vehicles (FCEVs).
Hydrogen fuel cells are currently the focus and focus of fuel cell research due to their advantages of high mass energy density and nearly zero carbon emissions. The relatively green and environment-friendly hydrogen production method is to electrolyze water to produce hydrogen. The water electrolysis hydrogen production reaction is divided into an oxygen evolution reaction at the anode and a hydrogen evolution reaction at the cathode. Because of the existence of overpotential of anode and cathode electrolysis, theoretically, 1.23V electrolysis voltage usually needs about 2V to obtain hydrogen, and lower electric energy-hydrogen energy conversion efficiency leads to higher hydrogen production cost. The best oxygen evolution and hydrogen evolution catalysts to date are noble metal ruthenium/iridium-based and platinum-based catalysts, respectively, but their very high cost limits large scale applications. Therefore, the development of a cheap and efficient hydrogen-producing and oxygen-producing catalyst is a research with innovative significance, and is also an indispensable condition for reducing the cost of the hydrogen fuel cell and promoting the hydrogen fuel cell to be widely applied worldwide, so as to ensure that the hydrogen fuel cell can achieve great commercial success in the future.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a metal composite material, a preparation method and an application thereof, wherein the metal composite material has high activity as a catalyst for water oxidation and urea oxidation reactions.
The present invention provides a metal composite material comprising:
a three-dimensional support;
and a metal composite oxide supported on a three-dimensional carrier; the metal composite oxide is formed from a nickel molybdenum oxide calcined at high temperature in a protective gas.
Preferably, the three-dimensional carrier is one or more of foamed nickel, carbon cloth and foamed copper.
Preferably, the mass fraction of nickel in the metal composite material is 25-40%; the mass fraction of molybdenum is 45-60%; the mass fraction of oxygen is 0-30%.
Preferably, the metal composite oxide is a one-dimensional nanorod array.
Preferably, the diameter of the metal composite oxide is 40-80 nm; the length-diameter ratio of the metal composite material is (10-80): 1.
preferably, the high-temperature calcination temperature is 200-600 ℃; the high-temperature calcination time is 1-3 h.
The invention also provides a preparation method of the metal composite material, which comprises the following steps:
s1) mixing a nickel source compound, a molybdenum source compound and the three-dimensional carrier in water, and heating for reaction to obtain a nickel-molybdenum oxide-loaded three-dimensional carrier;
s2) calcining the three-dimensional carrier loaded with the nickel-molybdenum oxide in protective gas at high temperature to obtain the metal composite material.
Preferably, the heating reaction temperature in the step S1) is 120-180 ℃; the heating reaction time is 4-12 h.
The invention also provides application of the metal composite material as an anode material.
The invention also provides application of the metal composite material as an anode electrocatalyst.
The invention provides a metal composite material, a preparation method and application thereof, wherein the metal composite material comprises the following components: a three-dimensional support; and a metal composite oxide supported on a three-dimensional carrier; the metal composite oxide is formed from a nickel molybdenum oxide calcined at high temperature in a protective gas. Compared with the prior art, the metal composite material provided by the invention has higher catalytic activity when being used as a catalyst for water oxidation and urea oxidation.
Experimental results show that the metal composite material prepared by the invention is used as an oxygen precipitation reaction catalyst, and the current density can reach 100mA/cm in the urea oxidation reaction at the potential of 1.42V2(ii) a In the urea-assisted total hydrolysis reaction, the current density can reach 100mA/cm when the potential is 1.55V2。
Drawings
FIG. 1 is a scanning electron micrograph of a metal composite obtained in example 1 of the present invention;
FIG. 2 is a transmission electron micrograph of a metal composite obtained in example 1 of the present invention;
FIG. 3 is an XRD plot of the metal composite obtained in example 1 of the present invention;
FIG. 4 is a scanning electron micrograph of a metal composite obtained in example 2 of the present invention;
FIG. 5 is a scanning electron micrograph of a metal composite obtained in example 3 of the present invention;
FIG. 6 is a scanning electron micrograph of a metal composite obtained in example 4 of the present invention;
FIG. 7 is a linear sweep voltammetry measurement curve of the metal composite obtained in example 1 of the present invention as an electrocatalyst for water oxidation and urea oxidation reactions.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention provides a metal composite material comprising:
a three-dimensional support;
and a metal composite oxide supported on a three-dimensional carrier; the metal composite oxide is formed by nickel molybdenum oxide calcined at high temperature in protective gas;
the three-dimensional carrier is a three-dimensional carrier known to those skilled in the art, and is not particularly limited, and in the present invention, one or more of nickel foam, carbon cloth, and copper foam are preferable, and nickel foam is more preferable.
The three-dimensional carrier is loaded with a metal composite oxide; the metal composite oxide is formed by nickel molybdenum oxide calcined at high temperature in protective gas; the protective gas is known to those skilled in the art, and is not particularly limited, and argon is preferred in the present invention; the high-temperature calcination temperature is preferably 200-600 ℃, more preferably 300-600 ℃, still more preferably 300-500 ℃, still more preferably 350-450 ℃, and most preferably 400 ℃; the high-temperature calcination time is preferably 1-3 h, more preferably 2-3 h, and further preferably 2 h; the metal composite oxide is preferably a one-dimensional nanorod array, namely the structure of the metal composite material provided by the invention is that the three-dimensional substrate supports the one-dimensional nanorod array; the nano-rods of the one-dimensional nano-rod array are preferably provided with nano-scale pore canals; the diameter of the metal composite oxide is preferably 40-80 nm; the length-diameter ratio of the metal oxide compound is preferably (10-80): 1.
the mass fraction of nickel in the metal composite material provided by the invention is preferably 25-40%, and more preferably 25-30%; the mass fraction of molybdenum is preferably 45-60%, and more preferably 45-50%; the mass fraction of oxygen is preferably 0 to 30%.
The metal composite material provided by the invention has higher catalytic activity when being used as a catalyst for water oxidation and urea oxidation.
The invention also provides a preparation method of the metal composite material, which comprises the following steps: s1) mixing a nickel source compound, a molybdenum source compound and the three-dimensional carrier in water, and heating for reaction to obtain a nickel-molybdenum oxide-loaded three-dimensional carrier; s2) calcining the three-dimensional carrier loaded with the nickel-molybdenum oxide in protective gas at high temperature to obtain the metal composite material.
The present invention is not particularly limited in terms of the source of all raw materials, and may be commercially available.
The nickel source compound is not particularly limited as long as it is a soluble nickel source compound known to those skilled in the art, and nickel nitrate is preferable in the present invention; the molybdenum source compound is not particularly limited as long as it is a soluble molybdenum source compound known to those skilled in the art, and sodium molybdate is preferable in the present invention; the molar ratio of the nickel source compound to the molybdenum source compound is preferably 1: (1 to 1.2), more preferably 1: 1.
the three-dimensional carrier is a three-dimensional carrier known to those skilled in the art, and is not particularly limited, and in the present invention, one or more of nickel foam, carbon cloth, and copper foam are preferable. In the present invention, the three-dimensional support is preferably mixed with the nickel source compound and the molybdenum source compound after being pretreated, and the pretreatment method is a method well known to those skilled in the art, and is not particularly limited.
When the three-dimensional carrier is foamed nickel and foamed copper, the following steps are preferably carried out: soaking foamed nickel or foamed copper in an organic solvent to remove surface oil stains; the organic solvent is not particularly limited as long as it is well known to those skilled in the art, and acetone is preferred in the present invention; the soaking time is preferably 1-2 h; after soaking in an organic solvent, washing with water, then soaking in 1-6 mol/L hydrochloric acid for 15-30 min to remove nickel oxide or copper oxide on the surface, finally washing with deionized water and ethanol, and drying to obtain pretreated foamed nickel or copper; the drying is preferably vacuum drying; the drying temperature is preferably 50-80 ℃; the drying time is preferably 4-24 h.
When the three-dimensional carrier is carbon cloth, the pretreatment is preferably performed according to the following steps: soaking the carbon cloth in an organic solvent to remove surface oil stains; the organic solvent is not particularly limited as long as it is well known to those skilled in the art, and acetone is preferred in the present invention; the soaking time is preferably 1-2 h; after soaking in an organic solvent, cleaning with water and ethanol, and drying to obtain a pretreated carbon cloth; the drying is preferably vacuum drying; the drying temperature is preferably 50-80 ℃; the drying time is preferably 4-24 h.
Mixing a nickel source compound, a molybdenum source compound and a three-dimensional carrier in water, preferably mixing the nickel source compound and the molybdenum source compound in water, preferably uniformly stirring and mixing on a magnetic stirrer to obtain a clear mixed solution, and then immersing the three-dimensional carrier in the mixed solution; wherein the proportion of the nickel source compound, the molybdenum source compound and water is preferably (1-4) mol: (1-4) mol: 35 ml.
Then heating for reaction; the temperature of the heating reaction is preferably 120-180 ℃, more preferably 130-160 ℃, and more preferably 150 ℃; the heating reaction time is preferably 4-12 h, and more preferably 6-10 h. After the reaction was complete, a product was obtained whose surface was yellow.
After the reaction, preferably washing and drying the product to obtain the three-dimensional carrier loaded with the nickel-molybdenum oxide; the drying is preferably vacuum drying; the drying temperature is preferably 50-100 ℃, and more preferably 60-90 ℃; the drying time is preferably 12-15 h.
Calcining the three-dimensional carrier loaded with the nickel-molybdenum oxide in protective gas at high temperature to obtain a metal composite material; the protective gas is a protective gas known to those skilled in the art and is not particularly limited, and in the present invention, argon is preferred; the high-temperature calcination temperature is preferably 300-600 ℃, more preferably 300-500 ℃, further preferably 350-450 ℃, and most preferably 400 ℃; the high-temperature calcination time is preferably 1-3 h, more preferably 2-3 h, and still more preferably 2 h.
The preparation method is simple, has low cost and is suitable for large-scale industrial popularization.
The invention also provides an application of the metal composite material as an anode material.
The invention also provides an application of the metal composite material as an anode electrocatalyst, preferably an oxygen evolution catalyst, and more preferably a water oxidation and urea oxidation reaction catalyst.
In order to further illustrate the present invention, the following detailed description of a metal composite material, a preparation method and applications thereof are provided in connection with examples.
The reagents used in the following examples are all commercially available.
Example 1
1.1 pretreatment of foam nickel: immersing commercial nickel foam in acetone for 2 hours, washing with deionized water to remove the acetone, immersing the obtained nickel foam in 3mol/L hydrochloric acid for 20 minutes, taking out the nickel foam, repeatedly washing with deionized water for more than ten times, washing with ethanol for 1-3 times, and drying the obtained nickel foam in a vacuum drying oven at 60 ℃ for 12 hours.
1.2 hydrothermal growth method for growing NiMoO on foam nickel skeleton4And (3) nanorod array: 2mmol of Ni (NO)3)2·6H2O and 2mmol Na2MoO4·2H2Dissolving O in 17.5ml deionized water respectively, stirring to dissolve completely, and adding the above Na2MoO4Solution addition to Ni (NO)3)2Stirring the solution for 10 minutes to form a uniform solution; transferring the mixed solution into a 50ml reaction kettle, and adding the mixed solution into the cut 1.1 to obtain the productNickel foam (about 2X 4 cm)2) Pouring the mixture into a container and completely immersing the mixture by the solution, and putting the mixture into an oven at 150 ℃ for reaction for 6 hours; and (3) taking out the foamed nickel substrate, repeatedly washing with deionized water and ethanol, and removing powder attached to the surface to obtain the foamed nickel loaded with the nickel-molybdenum oxide.
And 1.3, calcining the foamed nickel loaded with the nickel-molybdenum oxide obtained in the step 1.2 in argon at a high temperature to obtain the metal composite material, wherein the calcining temperature is 400 ℃, and the calcining time is 2 hours.
The metal composite material obtained in example 1 was analyzed by a scanning electron microscope, and a scanning electron micrograph thereof is shown in fig. 1. As can be seen from FIG. 1, the metal composite material maintains the one-dimensional structure of the nickel-molybdenum oxide nanorods grown on the surface of the three-dimensional foam nickel.
The metal composite material obtained in example 1 was analyzed by a transmission electron microscope, and a transmission electron micrograph thereof is shown in fig. 2. As can be seen from FIG. 2, dehydrated NiMoO4The surface of the nano rod is relatively uniform, and no particles appear.
The metal composite material obtained in example 1 was analyzed by X-ray diffraction, and the XRD profile thereof was obtained as shown in fig. 3. From FIG. 3, it can be seen that the prepared metal composite material phase and pure NiMoO4The JCPDS card of (a).
Example 2
Example 1 was repeated with the following differences: and (3) changing the high-temperature calcination temperature in the step 1.3 to 200 ℃ to obtain the metal composite material.
The metal composite material obtained in example 2 was analyzed by a scanning electron microscope, and a scanning electron micrograph thereof is shown in fig. 4. As can be seen from FIG. 4, the metal composite material maintains the one-dimensional structure of the nickel-molybdenum oxide nanorod grown on the surface of the three-dimensional foam nickel, and the morphology is relatively uniform.
Example 3
Example 1 was repeated with the following differences: and (3) changing the high-temperature calcination temperature in the step 1.3 to 300 ℃ to obtain the metal composite material.
The metal composite material obtained in example 3 was analyzed by a scanning electron microscope, and a scanning electron micrograph thereof is shown in fig. 5. As can be seen from FIG. 5, the metal composite material maintains the one-dimensional structure of the nickel molybdenum oxide nanorods grown on the surface of the three-dimensional foam nickel.
Example 4
Example 1 was repeated with the following differences: and (3) changing the high-temperature calcination temperature in the step 1.3 to 500 ℃ to obtain the metal composite material.
The metal composite material obtained in example 4 was analyzed by a scanning electron microscope, and a scanning electron micrograph thereof is shown in fig. 6. As can be seen from FIG. 6, the metal composite material maintains the one-dimensional structure of the nickel-molybdenum oxide nanorods grown on the surface of the three-dimensional foam nickel, and the one-dimensional morphology of the nanorods is not damaged by high temperature.
The electrocatalytic performance of the metal composite obtained by example 1 as an electrocatalyst in the water oxidation and urea oxidation reactions was measured, and the results were shown in the linear sweep voltammetry measurement curves shown in fig. 7. As can be seen from FIG. 7, the metal composite obtained in example 1 has better water oxidation and urea oxidation properties, wherein 1.52V, 1.62V and 1.68V are required to reach 10mA/cm in the water oxidation reaction2、100mA/cm2、250mA/cm2Current density of (d); in the urea oxidation reaction, the voltage of only 1.37V, 1.42V and 1.50V is needed to reach 10mA/cm2、100mA/cm2、250mA/cm2The current density of (1).
Claims (2)
1. A metal composite as a catalyst for an oxygen evolution reaction, comprising:
a three-dimensional support;
and a metal composite oxide supported on a three-dimensional carrier; the metal composite oxide is formed by nickel molybdenum oxide calcined at high temperature in protective gas;
the three-dimensional carrier is one or more of foamed nickel, carbon cloth and foamed copper;
the mass fraction of nickel in the metal composite material is 25-30%; the mass fraction of molybdenum is 45-50%; the mass fraction of oxygen is 0-30%;
the metal composite oxide is a one-dimensional nanorod array; the nano rods of the one-dimensional nano rod array are provided with nano-scale pore canals;
the diameter of the metal composite oxide is 40-80 nm; the length-diameter ratio of the metal composite material is (10-80): 1;
the high-temperature calcination temperature is 200-600 ℃; the high-temperature calcination time is 1-3 h.
2. A method for preparing a metal composite material as a catalyst for an oxygen evolution reaction, comprising:
s1) mixing a nickel source compound, a molybdenum source compound and the three-dimensional carrier in water, and heating for reaction to obtain a nickel-molybdenum oxide-loaded three-dimensional carrier; the molar ratio of the nickel source compound to the molybdenum source compound is 1: (1-1.2); the proportion of the nickel source compound, the molybdenum source compound and water is preferably (1-4) mol: (1-4) mol: 35ml of the solution; the temperature of the heating reaction is 120-180 ℃; the heating reaction time is 4-12 h;
s2) calcining the three-dimensional carrier loaded with the nickel-molybdenum oxide at high temperature in protective gas to obtain a metal composite material;
the high-temperature calcination temperature is 200-600 ℃; the high-temperature calcination time is 1-3 h.
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| CN107611453A (en) * | 2017-08-22 | 2018-01-19 | 哈尔滨工程大学 | Foamed nickel supported NiMoO for direct urea fuel cell4The preparation method of@C micron bar anode-array |
| CN108033518B (en) * | 2017-11-27 | 2024-04-12 | 山西大学 | Method and device for degrading urea in chlorine-containing swimming pool water |
| CN110783574A (en) * | 2019-11-05 | 2020-02-11 | 江苏大学 | Direct alcohol fuel cell gas diffusion electrode and preparation method thereof and direct alcohol fuel cell |
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