CN114335576B - CoN/Ti with foamed nickel as substrate 3 C 2 Material preparation method and application - Google Patents
CoN/Ti with foamed nickel as substrate 3 C 2 Material preparation method and application Download PDFInfo
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- CN114335576B CN114335576B CN202111645021.5A CN202111645021A CN114335576B CN 114335576 B CN114335576 B CN 114335576B CN 202111645021 A CN202111645021 A CN 202111645021A CN 114335576 B CN114335576 B CN 114335576B
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Abstract
The invention relates to a CoN/Ti based on foamed nickel 3 C 2 A preparation method and application of the material. The method is realized by controlling the mixture ratio of three raw materials of cobalt and nitrogen, the preparation of a titanium carbide aqueous solution and the hydrothermal temperature and time; wherein the first synthesis by physical mixing contains CoN and Ti respectively 3 C 2 The two solutions are subjected to a one-step hydrothermal method to obtain cobalt and nitrogen substances and Ti 3 C 2 Loading on foamed nickel, and finally stripping the foamed nickel by ultrasonic to prepare the catalyst. The initial potential and half-wave potential of the material obtained by the method are close to those of commercial platinum carbon, the material has higher limiting current density, but the price of the material is only 20-30% of that of the commercial platinum carbon, the material has better market application prospect, and the catalytic material obtained by applying the material to ORR has good oxygen reduction catalytic activity and wide application prospect.
Description
Technical Field
The invention belongs to Ti 3 C 2 The technical field of composite materials, in particular to a foamed nickel growth substrate, more particularly to a CoN/Ti based on foamed nickel 3 C 2 A method for the preparation of the material and its use for oxygen reduction.
Background
With the coming of global energy crisis and the increasing environmental pollution and greenhouse effect caused by the combustion of fossil fuels, the development of clean energy is urgently needed. There is an increasing concern about the storage and conversion of sustainable energy, and fuel cells are of high research value as one of the most promising clean energy converters at present. In a fuel cell, fuel is oxidized at the anode, the released electrons are transferred through an external circuit to the cathode, and oxygen is reduced at the cathode. However, the kinetics are very slow due to the reduction of oxygen to a four-electron reaction, which greatly limits the energy output efficiency of the fuel cell. ORR is a very important reaction for fuel cells. It is well known that the best ORR catalyst at present is the Pt-based catalyst. Although the platinum-based catalyst has the most outstanding catalytic activity, the platinum-based catalyst has poor stability, and platinum is scarce, has a small reserve and is expensive. Therefore, it is necessary to develop a high-efficiency and high-stability catalyst of non-platinum group.
In recent years, with the intensive research on the foamed nickel, the electrocatalytic performance of the foamed nickel is increasingly prominent. The catalyst carrier for catalytic combustion has the characteristics of unique open pore structure, low-pressure feeding holes, inherent tensile strength, thermal shock resistance and the like. The foamed nickel is used as a cheap three-dimensional pore material, the higher stability of the foamed nickel is beneficial to the integral stability of the catalyst, the larger specific surface area can increase catalytic active sites, the process for preparing the catalyst is simple, the operation is convenient, and the foamed nickel has good conductivity and the like.
MXenes is a new family of two-dimensional transition metal carbides, nitrides and carbonitrides that is considered to be the next promising electrocatalytic candidate. Compared with other two-dimensional materials, MXenes has conductivity (10000S cm) -1 ) Component diversity, thin and adjustable structures, easily adjustable surfaces and hydrophilic properties are receiving increasing attention. MXenes are derived from their MAX precursor and have the general formula Mn +1XnTx (N =1, 2 or 3), where M represents a transition metal (e.g., ti, V, cr, mo, nb, etc.), X represents C or N, and T represents a functional group (e.g., -O, -OH, and-F). A large number of stable MXenes have been predicted in theory and 30 types have been synthesized from the corresponding MAX. The adjustability of MXenes composition isThe method is beneficial to regulation and control of an electronic structure, and the unique two-dimensional layered structure provides a large specific surface area and exposes active sites to the maximum extent. In addition, its excellent corrosion resistance and hydrophilicity broadens the application range as compared to carbon-based supports. The functional group greatly promotes the assembly of the MXene nanosheet, and has strong interaction with other materials, so that the aggregation of the nanomaterial can be effectively avoided, and the electronic structure of the MXene-based mixture is optimized. Under the circumstances, the application of MXenes as an oxygen reduction catalyst to fuel cells is also becoming an important issue.
Disclosure of Invention
The invention aims to provide a CoN/Ti based on foamed nickel aiming at the defects in the prior art 3 C 2 A method for preparing the material and application of the material as an oxygen reduction catalyst. The method is realized by controlling the mixture ratio of three raw materials of cobalt and nitrogen, the preparation of a titanium carbide aqueous solution and the hydrothermal temperature and time; wherein the first synthesis by physical mixing contains CoN and Ti respectively 3 C 2 The two solutions are subjected to a one-step hydrothermal method to obtain cobalt and nitrogen substances and Ti 3 C 2 Loading on foamed nickel, and finally stripping the foamed nickel by ultrasonic to prepare the catalyst. Most of catalysts with foam nickel as a carrier are used for hydrogen evolution reaction, and the catalyst is applied to ORR, so that the obtained catalytic material has good oxygen reduction catalytic activity and wide application prospect.
The invention provides the following specific technical scheme:
CoN/Ti with foamed nickel as substrate 3 C 2 A method of preparing a material, the method comprising the steps of:
firstly, adopting a physical mixing method to carry out foam nickel pretreatment:
sequentially adding foamed nickel into acetic acid solution, anhydrous ethanol and deionized water, and performing ultrasonic treatment for 8-12min;
a second step of preparing Ti-containing material by physical mixing 3 C 2 The solution (2):
mixing Ti 3 C 2 Adding into deionized water, and performing ultrasonic treatment at 20-25 deg.C for 15-30minTo obtain Ti 3 C 2 The solution of (1); wherein, 1-5mmol of Ti is added into every 10mL of deionized water 3 C 2 ；
Third, preparation of CoN precursor
Sequentially adding urea, cobalt nitrate hexahydrate and hexadecyl trimethyl ammonium bromide (CTAB) into the first mixed solution, and fully stirring for 15-30min at room temperature by using a magnetic stirrer to obtain a second mixed solution;
wherein the first mixed solution comprises distilled water and glycol, and the volume ratio is that the distilled water: ethylene glycol =1:1;
adding 1-3mmol CTAB into each 12ml of the first mixed solution; the mol ratio is, urea: cobalt nitrate hexahydrate: 2-4;
fourthly, adopting a one-step hydrothermal method to prepare CoN/Ti 3 C 2 Modified nickel foam:
ti obtained in the second step 3 C 2 Mixing the solution with the second mixed solution prepared in the third step, soaking the pretreated foam nickel in the mixed solution, transferring the foam nickel into a reaction kettle, and reacting at 140-180 ℃ for 8-12 hours; after the reaction is finished, washing with deionized water and absolute ethyl alcohol in sequence to obtain the foam nickel composite material;
wherein the volume ratio is Ti 3 C 2 The solution (2): second mixed solution =1:1-3;
and fifthly, stripping the foamed nickel by adopting a physical method:
performing ultrasonic treatment on the foamed nickel composite material generated in the fourth step at the temperature of between 20 and 25 ℃ for 15 to 30 minutes to ensure that the CoN/Ti 3 C 2 And stripping from the foamed nickel, and then performing suction filtration and drying to obtain the CoN/Ti3C2 material with the foamed nickel as the substrate.
The concentration of the acetic acid solution in the first step is 3-5mol/L.
The drying in the fifth step is carried out in a drying oven at the temperature of 40-80 ℃ for 10-20h.
The foam nickel is CoN/Ti with the substrate 3 C 2 The application of the material is that the composite material is loaded on the cathode of the fuel cell as a catalyst.
The invention has the substantive characteristics that:
compared with the known preparation method of other metal and nonmetal loaded foam nickel composite materials, the invention selects metal cobalt, nonmetal nitrogen and Ti 3 C 2 The three substances are precursors; ti 3 C 2 The nickel foam has low electrocatalytic activity but good conductivity, is of a three-dimensional structure, has a large specific surface area and can better adsorb oxygen; coN nano-rod and Ti are subjected to hydrothermal method 3 C 2 Nanometer block combined CoN/Ti obtained by using foamed nickel as growth substrate 3 C 2 The composite material has good morphology structure, obviously increases the electrochemical surface area, and has CoN and Ti 3 C 2 The two components are cooperated to promote the oxygen catalytic reduction reaction. The invention has the beneficial effects that:
the invention relates to CoN/Ti with foam nickel as a substrate prepared by a one-step hydrothermal method 3 C 2 The material, compared with other metal catalysts, the catalyst is added with certain nonmetal and metal; the cost is reduced, the operation is simple, and the preparation conditions are mild. Meanwhile, due to the addition of cobalt and nitrogen elements, the electron transfer rate is increased, the charge transfer resistance is reduced, and catalytic active sites are effectively increased; and under the condition that most of foamed nickel is used for oxygen evolution reduction reaction, the foamed nickel is used for oxygen reduction reaction, and the synthesized electrocatalytic composite material has good oxygen reduction catalytic activity through electrochemical performance test. The initial potential and the half-wave potential are respectively as follows: the 0.98V and 0.85V are close to 1V and 0.87V of commercial platinum carbon, and have higher limiting current density, but the price is only 20-30% of the commercial platinum carbon, the price is low, and the method has better market application prospect.
Description of the drawings:
FIG. 1 is an SEM image of the CoN precursor obtained in example 1
FIG. 2 is an SEM image of CoN precursor based on nickel foam obtained in example 1
FIG. 3 shows CoN/Ti based on foamed nickel obtained in example 1 3 C 2 SEM image of Material
FIG. 4 shows CoN and Ti obtained in example 1 3 C 2 And CoN/Ti 3 C 2 Linear voltammetric sweep in 0.1mol/L oxygen saturated KOH solution (sweep rate 10mv/s, rotation speed 1600 rpm).
FIG. 5 shows CoN/Ti obtained in example 1 3 C 2 Linear voltammetric sweep curves at different rotational speeds
FIG. 6 shows CoN/Ti obtained in example 1 3 C 2 And linear voltammetric sweep curves (sweep rate 10mv/s, rotation rate 1600 rpm) of a commercial platinum-carbon catalyst in 0.1mol/L oxygen saturated KOH solution.
Detailed Description
Following specific examples of CoN/Ti based on foamed nickel 3 C 2 The preparation of the material and its use as an oxygen reducing agent are further described.
Example 1:
1. pretreatment of foamed nickel:
cutting the foamed nickel into a square shape with the size of 1cm x 1cm for processing; diluting acetic acid in a laboratory to 3mol/L, and sequentially performing ultrasonic treatment on the foamed nickel for 10min by using the acetic acid, absolute ethyl alcohol and deionized water (the volume is all 20 ml) respectively to remove impurities on the surface of the foamed nickel.
2. Preparation of Ti-containing material by physical mixing 3 C 2 The solution (2):
adding 3mmol of Ti 3 C 2 (about 0.192 g) was added to 10ml of deionized water and sonicated at 25 ℃ for 30 minutes until mixed well.
3. Preparation of CoN precursor
12ml of distilled water was uniformly mixed with 12ml of ethylene glycol, and then 3mmol of urea (about 0.18 g), 3mmol of cobalt nitrate hexahydrate (about 0.873 g), and 3mmol of CTAB (about 1.093 g) were weighed out in this order and added to the above-prepared solution, and stirred at room temperature for 30min under the action of a magnetic stirrer.
4. Preparation of CoN/Ti by one-step hydrothermal method 3 C 2 Modified nickel foam:
pouring the two solutions and foamed nickel into a high-pressure reaction kettle, drying in an electrothermal vacuum drying oven at 160 ℃ for 12h, cooling to room temperature, and washing with deionized water and absolute ethyl alcohol during centrifugal suction filtration.
5. Stripping the foamed nickel by adopting a physical method:
subjecting the foamed nickel composite material obtained in the fourth step to ultrasonic treatment at 25 ℃ for 30 minutes to enable the CoN/Ti to be 3 C 2 The composite material was obtained in the form of a dark block by peeling off from the nickel foam, suction-filtering and keeping in a drying oven at 60 ℃ for 12 hours.
Example 2
1. Pretreatment of foamed nickel:
cutting the foamed nickel into a square shape with the size of 1cm x 1cm for processing; diluting acetic acid in a laboratory to 3mol/L, and sequentially performing ultrasonic treatment on the foamed nickel for 10min by using the acetic acid, absolute ethyl alcohol and deionized water (the volume is all 20 ml) respectively to remove impurities on the surface of the foamed nickel.
2. Preparation of Ti-containing material by physical mixing 3 C 2 The solution (2):
2mmol of Ti 3 C 2 (about 0.128 g) was added to 10ml of deionized water and sonicated at 25 ℃ for 30 minutes until the mixed solution was sonicated until well mixed.
3. Preparation of CoN precursor
12ml of distilled water was uniformly mixed with 12ml of ethylene glycol, and then 3mmol of urea (about 0.18 g), 3mmol of cobalt nitrate hexahydrate (about 0.873 g), and 3mmol of CTAB (about 1.093 g) were weighed in this order and added to the above-prepared solution in sequence, and stirred at room temperature for 30min under the action of a magnetic stirrer.
4. Preparation of CoN/Ti by one-step hydrothermal method 3 C 2 Modified nickel foam:
pouring the two solutions and foamed nickel into a high-pressure reaction kettle, drying in an electrothermal vacuum drying oven at 160 ℃ for 12h, cooling to room temperature, and washing with deionized water and absolute ethyl alcohol during centrifugal suction filtration.
5. Stripping the foamed nickel by adopting a physical method:
ultrasonically treating the foamed nickel composite material generated in the fourth step at 25 ℃ for 30 minutes to ensure that the CoN/Ti 3 C 2 The composite material was obtained in the form of a dark block by peeling off from the nickel foam, suction-filtering and keeping in a drying oven at 60 ℃ for 12 hours.
Example 3
1. Pretreatment of foamed nickel:
cutting the foamed nickel into a square shape with the size of 1cm x 1cm for processing; diluting acetic acid in a laboratory to 3mol/L, and respectively carrying out ultrasonic treatment on the foamed nickel for 10min by using the acetic acid, absolute ethyl alcohol and deionized water (the volume is all 20 ml) in sequence to remove impurities on the surface of the foamed nickel.
2. Preparation of Ti-containing material by physical mixing 3 C 2 The solution (2):
2mmol of Ti 3 C 2 (about 0.128 g) was added to 10ml of deionized water and sonicated at 25 ℃ for 30 minutes until the mixed solution was sonicated until well mixed.
3. Preparation of CoN precursor
12ml of distilled water was uniformly mixed with 12ml of ethylene glycol, and then 3mmol of urea (about 0.18 g), 3mmol of cobalt nitrate hexahydrate (about 0.873 g), and 2mmol of CTAB (about 0.7289 g) were weighed in this order into the above-prepared solution, and stirred at room temperature for 30min under the action of a magnetic stirrer.
4. Preparation of CoN/Ti by one-step hydrothermal method 3 C 2 Modified nickel foam:
pouring the two solutions and foamed nickel into a high-pressure reaction kettle, drying in an electrothermal vacuum drying oven at 160 ℃ for 12h, cooling to room temperature, and washing with deionized water and absolute ethyl alcohol during centrifugal suction filtration.
5. Stripping the foamed nickel by adopting a physical method:
ultrasonically treating the foamed nickel composite material generated in the fourth step at 25 ℃ for 30 minutes to ensure that the CoN/Ti 3 C 2 The composite material was obtained in the form of a dark block by peeling off from the nickel foam, suction-filtering and keeping in a drying oven at 60 ℃ for 12 hours.
Application examples
Foam nickel based CoN/Ti 3 C 2 The material being an oxygen reduction catalyst in the ORRThe application is tested.
Electrocatalytic performance testing was performed using an electrochemical workstation and an RDE rotating disk electrode, with a three-electrode system (auxiliary electrode was a platinum electrode; reference electrode was a platinum electrode) in 0.1MKOH solution saturated with oxygen at 1600rpm for LSV testing (as catalyst, the catalyzed reaction was O) 2 +2H 2 O+4e - →4OH - (i.e., oxygen reduction reaction)). The potentials of the invention are all converted into standard hydrogen electrodes, oxygen is introduced for 20 minutes before the test to saturate the electrolyte, the electrode material is activated by 20 circles of volt-ampere circulation at 1600rpm and the sweep speed of 50mv/s, and then the linear volt-ampere test is carried out at the sweep speed of 10mv/s and the range of 1-0.2V. Each experiment was repeated 3 times to ensure the reliability of the experimental data.
Fig. 1 is an SEM image of the CoN precursor, from which we can see that agglomeration occurs.
Fig. 2 is an SEM image of a nickel foam-based CoN precursor, from which we can see a significant reduction in agglomeration, relative dispersion, as compared to the CoN precursor of fig. 1.
FIG. 3 shows a nickel foam based CoN/Ti 3 C 2 From the SEM image of the material, we can see that the dispersion degree of the CoN nano rod is much higher compared with the CoN precursor and the CoN precursor taking foam nickel as the substrate.
FIG. 4 shows CoN and Ti 3 C 2 And CoN/Ti 3 C 2 The performance test results of (1). From the figure we can see CoN/Ti 3 C 2 The initial potential and half-wave potential of the electrode are respectively 0.98 and 0.85 which are obviously higher than those of CoN and Ti 3 C 2 The starting potential and the half-wave potential of (c). Indicating that our catalyst possesses catalytic activity far exceeding that of a single raw material.
FIG. 5 is a linear voltammogram of CoN/Ti3C2 at different rotational speeds. From the figure we can see that the electrode rotation speed is proportional to the current density, indicating a primary oxygen reduction reaction.
Fig. 6 is a performance test chart. From the figure we can see CoN/Ti 3 C 2 The performance of the electrode is similar to that of a platinum carbon electrode. While the price of the current 1g platinum-carbon catalyst is 191.2 yuanWhile the present invention only takes about 40 yuan to prepare 1g of CoN/Ti3C2 catalyst. Therefore, under the condition of similar performance, the CoN/Ti3C2 catalyst has low price and better market application prospect.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and that, while the invention has been described in detail with reference to the above-mentioned embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention as defined by the appended claims.
The invention is not the best known technology.
Claims (4)
1. CoN/Ti with foamed nickel as substrate 3 C 2 A method for preparing a material, characterized in that the method comprises the steps of:
firstly, adopting a physical mixing method to carry out foam nickel pretreatment:
sequentially adding foamed nickel into acetic acid solution, anhydrous ethanol and deionized water, and performing ultrasonic treatment for 8-12min;
secondly, preparing Ti-containing material by adopting a physical mixing method 3 C 2 The solution (2):
mixing Ti 3 C 2 Adding into deionized water, and performing ultrasonic treatment at 20-25 deg.C for 15-30min to obtain Ti 3 C 2 The solution of (1); wherein, 1-5mmol of Ti is added into every 10mL of deionized water 3 C 2 ；
Third, preparation of CoN precursor
Sequentially adding urea, cobalt nitrate hexahydrate and Cetyl Trimethyl Ammonium Bromide (CTAB) into the first mixed solution, and fully stirring for 15-30min at room temperature by using a magnetic stirrer to obtain a second mixed solution;
wherein the first mixed solution comprises distilled water and glycol, and the volume ratio is that the distilled water: ethylene glycol =1:1;
adding 1-3mmol CTAB into each 12ml of the first mixed solution; the molar ratio is as follows: cobalt nitrate hexahydrate: CTAB = 2-4;
fourthly, preparing CoN/Ti by adopting a one-step hydrothermal method 3 C 2 Modified nickel foam:
ti obtained in the second step 3 C 2 Mixing the solution with the second mixed solution prepared in the third step, soaking the pretreated foam nickel in the mixed solution, transferring the foam nickel into a reaction kettle, and reacting at 140-180 ℃ for 8-12 hours; after the reaction is finished, washing with deionized water and absolute ethyl alcohol in sequence to obtain the foam nickel composite material;
wherein the volume ratio is, ti 3 C 2 The solution (2): the second mixed solution =1 to 3;
and fifthly, stripping the foamed nickel by adopting a physical method:
performing ultrasonic treatment on the foamed nickel composite material generated in the fourth step at the temperature of between 20 and 25 ℃ for 15 to 30 minutes to ensure that the CoN/Ti 3 C 2 Stripping off the nickel foam, then carrying out suction filtration and drying to obtain the foamed nickel-based CoN/Ti 3 C 2 A material.
2. The nickel foam-based CoN/Ti of claim 1 3 C 2 The material preparation method is characterized in that the concentration of the acetic acid solution in the first step is 3-5mol/L.
3. The nickel foam-based CoN/Ti of claim 1 3 C 2 The material preparation method is characterized in that the drying in the fifth step is kept for 10-20 hours in a drying oven at the temperature of 40-80 ℃.
4. The nickel foam-based CoN/Ti produced by the method of claim 1 3 C 2 The application of the material is characterized in that the composite material is loaded on a cathode of a fuel cell as a catalyst.
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