CN113231641A - Carbon black loaded highly-ordered PtCo intermetallic compound and synthesis method and application thereof - Google Patents
Carbon black loaded highly-ordered PtCo intermetallic compound and synthesis method and application thereof Download PDFInfo
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Abstract
本发明提供了一种炭黑负载高度有序的PtCo金属间化合物的合成方法，包括以下步骤：A)将钴盐、铂盐和炭黑分散于溶剂中，得到悬浊液；B)将所述悬浊液去除溶剂后依次进行高温退火和缓慢冷却，得到炭黑负载高度有序的PtCo金属间化合物，所述缓慢冷却为以1.0～1.3℃/min的降温速率将至550～650℃后，再自然冷却。本发明提供的合成方法中，进行高温退火后，再通过调控退火时降温的速率，以1～1.3℃/min的冷却速率降温至550～650℃，不仅能够有效促进颗粒内部的合金成分提高，同时在低于相转变温度的时候能够有效促进合金转变为金属间化合物，即形成有序结构。合成得到的高度有序PtCo催化剂具有优异的稳定性和催化氧化还原活性，优于商业Pt/C。The invention provides a method for synthesizing a carbon black-supported highly ordered PtCo intermetallic compound, comprising the following steps: A) dispersing cobalt salt, platinum salt and carbon black in a solvent to obtain a suspension; B) dispersing the After removing the solvent from the suspension, perform high temperature annealing and slow cooling in sequence to obtain a highly ordered PtCo intermetallic compound supported by carbon black. , and then natural cooling. In the synthesis method provided by the present invention, after high-temperature annealing is performed, the cooling rate during annealing is adjusted, and the temperature is lowered to 550-650°C at a cooling rate of 1-1.3°C/min, which can not only effectively promote the improvement of the alloy composition inside the particles, At the same time, when the temperature is lower than the phase transition temperature, the alloy can be effectively promoted to transform into an intermetallic compound, that is, an ordered structure is formed. The synthesized highly ordered PtCo catalyst exhibits excellent stability and catalytic redox activity, superior to commercial Pt/C.
Description
Technical Field
The invention belongs to the field of nanotechnology, and particularly relates to a carbon black loaded highly-ordered PtCo intermetallic compound and a synthesis method and application thereof.
Background
Proton Exchange Membrane Fuel Cells (PEMFCs) are considered as a clean energy source, and can be used in the fields of electric vehicles, consumer electronics, domestic power plants, and the like. Nano Pt catalysts dispersed on carbon black supports (Pt/C) are widely used to catalyze the Oxygen Reduction Reaction (ORR) on the cathode. However, the high cost and scarcity of Pt are major obstacles to its widespread use. In PEMFCs, Pt catalysts often suffer from insufficient activity and degradation problems under high potential and oxidizing acidic environments
At present, in order to reduce the Pt load and improve the activity of the Pt/C catalyst, many efforts are made, including platinum-based catalyst alloying, and further controlling the alloy component ratio of the platinum-based catalyst, optimizing the particle morphology and crystal face, and ordered intermetallic compound structure. The stability of the platinum-based catalyst is improved mainly by: 1. the prepared alloy is annealed at high temperature to form an intermetallic compound with an ordered structure, so that a catalyst with higher stability and higher activity is obtained; 2. and (3) segregating Pt atoms to the surface of the particles by utilizing a hydrogen reducing atmosphere to form Pt shell coated particles so as to obtain a more stable high structure.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a carbon black loaded highly ordered PtCo intermetallic compound, a synthesis method and an application thereof, wherein the synthesis method provided by the present invention can simultaneously promote the alloying and ordering of PtCo particles to obtain a commercial carbon black loaded highly ordered PtCo intermetallic compound catalyst, the method is simple and easy to implement, can be prepared in a large scale, and has an activity and a stability superior to those of commercial Pt/C.
The invention provides a synthetic method of a highly ordered PtCo intermetallic compound loaded with carbon black, which comprises the following steps:
A) dispersing cobalt salt, platinum salt and carbon black in a solvent to obtain a suspension;
B) and removing the solvent from the suspension, and then sequentially carrying out high-temperature annealing and slow cooling to obtain the carbon black loaded highly-ordered PtCo intermetallic compound, wherein the high-temperature annealing temperature is 900-1100 ℃, the slow cooling is carried out until the temperature is reduced to 550-650 ℃ at a cooling rate of 1-1.3 ℃/min, and then the mixture is naturally cooled.
Preferably, the cobalt salt is selected from Co (NO)3)2·6H2O or CoCl2·6H2O, the platinum salt is selected from H2PtCl4·6H2O。
Preferably, said Co (NO)3)2·6H2O and H2PtCl4·6H2The molar ratio of O is 1.1-1.3: 1.
preferably, the mass ratio of the total mass of the cobalt salt and the platinum salt to the carbon black is (0.14-0.15): 1.
Preferably, the solvent is selected from absolute ethanol or ultrapure water.
Preferably, the solvent removal method is rotary evaporation.
Preferably, the high-temperature annealing and slow cooling method comprises the following steps:
under the protective atmosphere of hydrogen and argon with the volume ratio of 5:95, raising the temperature of the powder precursor to 1000 ℃ at the speed of 5 ℃/min, and keeping the temperature for 2 hours; then the temperature is reduced to 600 ℃ at a slow cooling speed of 1.1 ℃/min, and then the mixture is naturally cooled to the room temperature.
The invention also provides the carbon black loaded highly-ordered PtCo intermetallic compound prepared by the synthesis method, and the total metal loading of the PtCo intermetallic compound is 9-13 wt%.
Preferably, the degree of order of the PtCo intermetallic compound is 70% to 90%.
The invention also provides application of the carbon black loaded highly-ordered PtCo intermetallic compound prepared by the synthesis method as a catalyst in an oxygen reduction reaction.
Compared with the prior art, the invention provides a synthesis method of a carbon black loaded highly-ordered PtCo intermetallic compound, which comprises the following steps: A) dispersing cobalt salt, platinum salt and carbon black in a solvent to obtain a suspension; B) and removing the solvent from the suspension, sequentially carrying out high-temperature annealing and slow cooling to obtain the carbon black loaded highly-ordered PtCo intermetallic compound, wherein the slow cooling is carried out after the temperature is reduced to 550-650 ℃ at the temperature reduction rate of 1.0-1.3 ℃/min, and then naturally cooling. According to the synthesis method provided by the invention, after high-temperature annealing is carried out, the temperature is reduced to 550-650 ℃ at a cooling rate of 1.0-1.3 ℃/min by adjusting and controlling the temperature reduction rate during annealing, so that not only can the improvement of alloy components in particles be effectively promoted, but also the alloy can be effectively promoted to be converted into intermetallic compounds when the temperature is lower than the phase transition temperature, namely, an ordered structure is formed. The synthesized highly ordered PtCo catalyst has excellent stability and catalytic oxidation-reduction activity, and is superior to commercial Pt/C. The transmission electron microscope shows that the platinum nanoparticles are uniformly dispersed on the carrier; x-ray diffraction showed that the sample had a highly ordered structure.
Drawings
Fig. 1 is a transmission electron micrograph of a PtCo intermetallic compound prepared according to example 1 of the present invention;
fig. 2 is a scanning tunneling electron micrograph of the PtCo intermetallic compound prepared in example 1 of the present invention;
fig. 3 is a scanning electron microscope photograph of spherical aberration correction of PtCo intermetallic compound prepared in example 1 of the present invention;
FIG. 4 shows an X-ray diffraction pattern of a PtCo intermetallic compound produced in example 1 of the present invention;
FIG. 5 is a Cyclic Voltammogram (CV) for initial and post-30000-cycle stability of PtCo intermetallic compounds prepared in example 1 of the present invention;
FIG. 6 is a linear polarization curve of the initial and post-30000-cycle stability of PtCo intermetallic compounds prepared in example 1 of the present invention;
FIG. 7 is a scanning tunneling electron micrograph of comparative example 1 according to the present invention;
FIG. 8 is an X-ray diffraction pattern of comparative example 1 of the present invention;
FIG. 9 is a scanning tunneling electron micrograph of comparative example 2 according to the present invention;
FIG. 10 is an X-ray diffraction pattern of comparative example 2 of the present invention;
FIG. 11 is an LSV of example 1 and comparative examples 2 and 3 of the present invention and commercial Pt/C.
Detailed Description
The invention provides a synthetic method of a highly ordered PtCo intermetallic compound loaded with carbon black, which comprises the following steps:
A) dispersing cobalt salt, platinum salt and carbon black in a solvent to obtain a suspension;
B) and removing the solvent from the suspension, and then sequentially carrying out high-temperature annealing and slow cooling to obtain the carbon black loaded highly-ordered PtCo intermetallic compound, wherein the high-temperature annealing temperature is 900-1100 ℃, the slow cooling is carried out until the temperature is reduced to 550-650 ℃ at a cooling rate of 1.1-1.3 ℃/min, and then the mixture is naturally cooled.
Firstly, cobalt salt, platinum salt and carbon black are dispersed in a solvent to obtain a suspension. Wherein the cobalt salt is selected from Co (NO)3)2·6H2O or CoCl2·6H2O, the platinum salt is selected from H2PtCl4·6H2O。
The Co (NO)3)2·6H2O or CoCl2·6H2O and H2PtCl4·6H2The molar ratio of O is 1.1-1.3: 1. preferably 1.2:1, 1.3:1, or 1.2 to 1.3: any value between 1.
The mass ratio of the total mass of the cobalt salt and the platinum salt to the carbon black is (0.14-0.15): 1, preferably any value between 0.14:1, 0.142:1, 0.145:1, 0.147:1, 0.15:1, or (0.14-0.15): 1.
In the present invention, the carbon black is a commercial carbon black.
The solvent is not particularly limited in the present invention, and may be an organic solvent known to those skilled in the art, and the solvent is preferably absolute ethanol.
And then, removing the solvent from the suspension to obtain a powder precursor.
In the present invention, the method for removing the solvent is not particularly limited, and a method for removing the solvent, which is well known to those skilled in the art, is preferably rotary evaporation.
The above method can mix the raw materials thoroughly to obtain a uniform mixture.
And after a powder precursor is obtained, sequentially carrying out high-temperature annealing and slow cooling on the precursor to obtain the carbon black loaded highly-ordered PtCo intermetallic compound.
The method for high-temperature annealing and slow cooling comprises the following steps:
under the protective atmosphere of hydrogen and argon with the volume ratio of 5:95, raising the temperature of the powder precursor to 900-1100 ℃ at the speed of 5 ℃/min, and keeping the temperature for 2 hours; then the temperature is reduced to 550-650 ℃ at a slow cooling speed of 1-1.3 ℃/min, and then the mixture is naturally cooled to the room temperature.
In some embodiments of the invention, the high temperature annealing and slow cooling method comprises: under the protective atmosphere of hydrogen and argon with the volume ratio of 5:95, raising the temperature of the powder precursor to 1000 ℃ at the speed of 5 ℃/min, and keeping the temperature for 2 hours; then the temperature is reduced to 600 ℃ at a slow cooling speed of 1.1 ℃/min, and then the mixture is naturally cooled to the room temperature.
The powder precursor in this step promotes the formation of particles as the pyrolysis temperature rises, and the alloy composition inside the particles gradually reaches the required stoichiometric ratio of 1: 1, then slowly cooling from 900-1100 ℃ to 550-650 ℃ at a cooling rate of 1-1.3 ℃/min, and promoting the ordered arrangement inside the particles to generate the PtCo intermetallic compound when the temperature is lower than the phase transition temperature of the PtCo.
The invention also provides the carbon black loaded highly ordered PtCo intermetallic compound prepared by the synthesis method.
Wherein the total metal loading of the PtCo intermetallic compound is 9-13 wt%, and the degree of order of the PtCo intermetallic compound is 70-90%.
The invention also provides application of the carbon black loaded highly-ordered PtCo intermetallic compound prepared by the synthesis method as a catalyst in an oxygen reduction reaction.
The application provides a method for preparing a highly ordered PtCo intermetallic compound loaded with commercial carbon black through slow cooling, and the synthesis method provided by the application has the advantages of wide raw material source, simplicity in preparation and capability of realizing large-scale synthesis, so that the method has universality.
According to the synthesis method provided by the invention, after high-temperature annealing is carried out, the temperature is reduced to 600 ℃ at the cooling rate of 1.1 ℃/min by adjusting and controlling the cooling rate during annealing, so that not only can the improvement of alloy components in particles be effectively promoted, but also the alloy can be effectively promoted to be converted into intermetallic compounds when the temperature is lower than the phase transition temperature, namely, an ordered structure is formed. The synthesized highly ordered PtCo catalyst has excellent stability and catalytic oxidation-reduction activity, and is superior to commercial Pt/C. The transmission electron microscope shows that the platinum nanoparticles are uniformly dispersed on the carrier; x-ray diffraction showed that the sample had a highly ordered structure.
In order to further understand the present invention, the following description is made with reference to the following examples to illustrate the carbon black loaded highly ordered PtCo intermetallic compound and the synthesis method and application thereof, and the scope of the present invention is not limited by the following examples.
Example 1
a. 50g of commercial carbon black BP2000, 14.7mg of H2PtCl4·6H2O and 10.8mg Co (NO)3)2·6H2Mixing O with 50mL of absolute ethyl alcohol, soaking, stirring, filtering, and removing the solvent through a rotary evaporator to obtain precursor powder which is uniformly mixed;
b. transferring the precursor powder to a quartz crucible after drying in a transfer oven, putting the quartz crucible into a tube furnace, heating the powder precursor to 1000 ℃ at a speed of 5 ℃/min under the protective atmosphere of 5% hydrogen and 95% argon, and keeping for 2 h; then the temperature is reduced to 600 ℃ at a slow cooling speed of 1.1 ℃/min, and then the PtCo intermetallic compound with high order is obtained after natural cooling to the room temperature.
The PtCo intermetallic compound obtained as described above is characterized, and the results are shown in fig. 1 to 4, and fig. 1 is a transmission electron microscope picture of a common transmission electron microscope photograph of the PtCo intermetallic compound prepared in example 1 of the present invention, which shows that the PtCo intermetallic compound is uniformly dispersed on the commercial carbon black; fig. 2 is a scanning tunneling electron micrograph of the PtCo intermetallic compound prepared in example 1 of the present invention, showing that the average particle size of the PtCo intermetallic compound dispersed on the commercial carbon black is approximately 5 nm; fig. 3 is a scanning electron microscope photograph of spherical aberration correction of the PtCo intermetallic compound prepared in example 1 of the present invention, which shows the atomic distribution of a single particle of the PtCo intermetallic compound, and it can be seen that the brighter atom is Pt, and the darker is Co atom, and it can be seen that the arrangement of Pt and Co atoms alternate between light and dark, which means that an ordered PtCo intermetallic compound is synthesized; fig. 4 is an X-ray diffraction pattern of the PtCo intermetallic compound prepared in example 1 of the present invention, showing a superlattice peak of the PtCo ordered structure, indicating that the highly ordered PtCo intermetallic compound is synthesized.
Performing electrochemical test on the obtained PtCo intermetallic compound, specifically, the ORR electrochemical test process of the catalyst is as follows:
1. 4mg of the catalyst was dispersed in 1.96ml of isopropanol, 40. mu.L of a 5% Nafion solution and sonicated for 2h to give ink of the catalyst.
2. Dropping 10 μ link onto a glassy carbon electrode with diameter of 5mm, and naturally drying.
CV testing at N2Saturated 0.1MHClO4The CV is in the range of 0.05V to 1.05V (vs RHE) and the sweep rate is 50mV s-1。
LSV test 0.1MHClO saturated at O24The CV is in the range of 0.05V to 1.05V (vs RHE) and the sweep rate is 10mV s-1。
5. Stability test 0.1M HClO saturated at O24The CV range is 0.6V to 0.95V (vs RHE), and the sweep rate is 100mV s-1The number of scanning turns is 30000 turns.
The test results are shown in fig. 5 and fig. 6, fig. 5 is a cyclic voltammetry Curve (CV) of the PtCo intermetallic compound prepared in example 1 of the present invention with initial and stability after 30000 cycles, and the CV results show that the CV change before and after the stability test is not large, and only a slight decrease appears in the Hupd region of 0.05V-0.4V (vs RHE), which indicates that the electrochemical active area of platinum only slightly decreases, indicating that the highly ordered PtCo intermetallic compound catalyst has better stability.
Fig. 6 is a linear polarization curve of the PtCo intermetallic compound prepared in example 1 of the present invention after initial and 30000 cycles of stability, and the LSV results show that the half-wave potential on the LSV decreased by only 9mV before and after the stability test, indicating that the PtCo intermetallic compound catalyst has excellent stability and excellent activity.
Comparative example 1
a. 50g of commercial carbon black BP2000, 14.7mg of H2PtCl4·6H2O and 10.8mg Co (NO)3)2·6H2Mixing O with 50mL of absolute ethanol, soaking, stirring, removing by rotary evaporatorSolvent to obtain precursor powder which is uniformly mixed;
b. transferring the precursor powder to a quartz crucible after drying in a transfer oven, putting the quartz crucible into a tube furnace, heating the powder precursor to 1000 ℃ at a speed of 5 ℃/min under the protective atmosphere of 5% hydrogen and 95% argon, and keeping for 2 h; naturally cooling to room temperature to obtain the PtCo intermetallic compound with low degree of order.
FIG. 7 is a scanning tunneling electron micrograph of comparative example 1, which shows an average particle size of about 2 nm. FIG. 8 is an X-ray diffraction pattern of comparative example 1, which shows that a PtCo intermetallic compound having a low degree of order is obtained.
Comparative example 2
a. 50g of commercial carbon black BP2000, 14.7mg of H2PtCl4·6H2O and 10.8mg Co (NO)3)2·6H2Mixing O with 50mL of absolute ethyl alcohol, soaking, stirring, filtering, and removing the solvent through a rotary evaporator to obtain precursor powder which is uniformly mixed;
b. transferring the precursor powder to a quartz crucible after drying in a transfer oven, putting the quartz crucible into a tube furnace, heating the powder precursor to 800 ℃ at a speed of 5 ℃/min under the protective atmosphere of 5% hydrogen and 95% argon, and keeping the temperature for 2 hours; and naturally cooling to room temperature to obtain the disordered PtCo alloy.
FIG. 9 is a scanning tunneling electron micrograph of comparative example 2, which shows that the average particle size is about 4 nm.
FIG. 10 shows the X-ray diffraction pattern of comparative example 2 of the present invention, which shows that a disordered PtCo intermetallic compound is obtained.
FIG. 11 is an LSV of example 1 and comparative examples 2 and 3 of the present invention and commercial Pt/C showing a highly ordered PtCo intermetallic compound initial mass activity as high as 2.49A/mg, far superior to the comparative example and commercial catalyst.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A synthetic method of a carbon black loaded highly ordered PtCo intermetallic compound is characterized by comprising the following steps:
A) dispersing cobalt salt, platinum salt and carbon black in a solvent to obtain a suspension;
B) and removing the solvent from the suspension, and then sequentially carrying out high-temperature annealing and slow cooling to obtain the carbon black loaded highly-ordered PtCo intermetallic compound, wherein the high-temperature annealing temperature is 900-1100 ℃, the slow cooling is carried out until the temperature is reduced to 550-650 ℃ at a cooling rate of 1-1.3 ℃/min, and then the mixture is naturally cooled.
2. The synthesis method according to claim 1, characterized in that the cobalt salt is selected from Co (NO)3)2·6H2O or CoCl2·6H2O, the platinum salt is selected from H2PtCl4·6H2O。
3. The method of synthesis according to claim 2, wherein the Co (NO) is3)2·6H2O and H2PtCl4·6H2The molar ratio of O is 1.1-1.3: 1.
4. the synthesis method according to claim 1, wherein the mass ratio of the total mass of the cobalt salt and the platinum salt to the carbon black is (0.14-0.15): 1.
5. The method of synthesis according to claim 1, wherein the solvent is selected from absolute ethanol or ultrapure water.
6. The method of synthesis according to claim 1, wherein the solvent removal is by rotary evaporation.
7. The synthesis method according to claim 1, wherein the high-temperature annealing and slow cooling method comprises the following steps:
under the protective atmosphere of hydrogen and argon with the volume ratio of 5:95, raising the temperature of the powder precursor to 900-1100 ℃ at the speed of 5 ℃/min, and keeping the temperature for 2 hours; then the temperature is reduced to 550-650 ℃ at a slow cooling speed of 1-1.3 ℃/min, and then the mixture is naturally cooled to the room temperature.
8. The carbon black loaded highly ordered PtCo intermetallic compound prepared by the synthesis method according to any one of claims 1 to 7, wherein the total metal loading of the PtCo intermetallic compound is 9-13 wt%.
9. The PtCo intermetallic compound according to claim 8, wherein the degree of order of the PtCo intermetallic compound is 70 to 90%.
10. An application of the carbon black loaded highly ordered PtCo intermetallic compound prepared by the synthesis method according to any one of claims 1 to 7 as a catalyst in an oxygen reduction reaction.
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| CN121042070A (en) * | 2025-11-03 | 2025-12-02 | 东华大学 | Transition metal carbide platinum-based intermetallic compounds, their preparation methods and applications |
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