CN113258082B - Platinum-based amorphous alloy nanowire for oxygen reduction catalysis and preparation method thereof - Google Patents
Platinum-based amorphous alloy nanowire for oxygen reduction catalysis and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a platinum-based amorphous alloy nanowire for oxygen reduction catalysis and a preparation method thereof, wherein the preparation method comprises the following steps: s1, mixing platinum, nickel, copper and phosphorus according to the mass ratio of 36:1:3:2, smelting and suction casting to obtain an amorphous alloy bar; s2, cutting the amorphous alloy bar into amorphous alloy wafers; s3, overlapping the AAO template with the nano-scale holes and the amorphous alloy wafer in a mold, and carrying out hot pressing to obtain an amorphous alloy primary product; s4, cooling, taking out, and performing surface anti-oxidation treatment; s5, immersing the amorphous alloy primary product into a sodium hydroxide solution with the mass fraction of 15%, and removing the AAO template which indicates the residue to obtain the platinum-based amorphous alloy with the nanowire; and S6, placing the platinum-based amorphous alloy into an ethanol solution, performing ultrasonic treatment to separate the nanowires, and collecting the nanowires. The platinum-based amorphous alloy nanowire for oxygen reduction catalysis has the advantages of stable reduction catalysis performance, simple process requirement, short preparation time, strong repeatability, convenience in collection and suitability for large-scale production.
Description
Technical Field
The invention relates to the technical field of gas catalysis, in particular to a platinum-based amorphous alloy nanowire for oxygen reduction catalysis and a preparation method thereof.
Background
The rapid increase of global economy has rapidly increased the demand of human society for energy, and fossil energy is the most important energy, but faces the problems of shortage, pollution and the like. The strategy of sustainable development has become a consensus of human beings, and the development and utilization of clean and renewable new energy sources (such as wind energy and solar energy) is a necessary way for the development of future energy sources. At present, wind power generation and photovoltaic power generation continuously make new breakthroughs in basic research, energy conversion efficiency is continuously improved, and meanwhile cost is continuously reduced.
Among the various alternative electrochemical storage and conversion systems, metal-air batteries, in which electricity is generated by a redox reaction between metal and oxygen in the air, the open structure of which makes it possible to obtain infinite oxygen from the atmosphere, reduce the weight of the whole battery, and give them an extremely high theoretical energy density, have attracted considerable attention. Oxygen is distributed most widely in nature, accounts for 48.6% of the mass of the earth crust and is the element with the highest abundance, but oxygen is not easy to react with many substances as a gas which is not too active at normal temperature, especially the oxygen reduction reaction is difficult to be carried out at normal temperature, and the birth of the air battery generates a great demand for the catalyst for oxygen reduction.
The conventional catalytic method generally adopts various chemical methods such as electrochemical deposition, hydrothermal/solvothermal and chemical bath deposition to carry out molecular modification on the catalyst, the process is complex, multiple steps of treatment are generally required, and the process requirement of each step is high and is not easy to repeat.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a platinum-based amorphous alloy nanowire for an oxygen reduction catalyst, which is simple to operate, and the prepared platinum-based amorphous alloy nanowire.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the platinum-based amorphous alloy nanowire for oxygen reduction catalysis comprises the following steps:
s1, mixing platinum, nickel, copper and phosphorus according to the mass ratio of 36:1:3:2, smelting and suction casting to obtain an amorphous alloy bar;
s2, cutting the amorphous alloy bar into amorphous alloy wafers with preset thickness;
s3, overlapping the AAO template with the nano-scale holes and the amorphous alloy wafer in a mold, and carrying out hot pressing under the inert gas atmosphere to obtain an amorphous alloy primary product;
s4, cooling, taking the amorphous alloy primary product out of the mold, and carrying out surface anti-oxidation treatment;
s5, immersing the amorphous alloy primary product into a sodium hydroxide solution with the mass fraction of 15%, and removing the residual AAO template to obtain the platinum-based amorphous alloy with the nanowire;
s6, placing the platinum-based amorphous alloy with the nanowires in an ethanol solution, performing ultrasonic treatment to separate the nanowires, and collecting the nanowires, wherein the nanowires are the platinum-based amorphous alloy nanowires.
Preferably, the pore diameter of the nano-scale pores on the AAO template is 100nm-300 nm.
Preferably, the diameter of the amorphous alloy wafer is 5mm, and the thickness of the amorphous alloy wafer is 75mm-80 mm; the diameter of the AAO template is 5mm +/-2 mm.
Preferably, in step S3, the temperature of the hot pressing is 200 ℃ to 205 ℃, and the pressure of the hot pressing is 15kN to 20 kN.
Preferably, the amorphous alloy primary product comprises an amorphous alloy bottom plate and a nanowire formed on the amorphous alloy bottom plate; the nano-wire is formed by the way that amorphous alloy enters the nano-scale hole of the AAO template through hot melting.
Preferably, in step S4, the surface oxidation preventing treatment is performed as follows: and putting the amorphous alloy primary product into an absolute ethyl alcohol solution with the mass fraction of 0.3%.
Preferably, in step S5, the amorphous alloy primary product is immersed in the sodium hydroxide solution for 30 minutes to 50 minutes.
Preferably, in step S6, the platinum-based amorphous alloy with the nanowires is subjected to ultrasonic treatment for 45 minutes to 60 minutes in an ethanol solution by using an ultrasonic cleaning apparatus; and after the ultrasonic treatment is finished, removing the ethanol solution by adopting a rotary evaporator at the low pressure of 200-1000 Pa, and collecting the nanowires separated from the platinum-based amorphous alloy.
Preferably, the composition of the platinum-based amorphous alloy is Pt57.5Cu14.7Ni5.3P22.5。
The invention also provides a platinum-based amorphous alloy nanowire for oxygen reduction catalysis, which is prepared by adopting any one of the preparation methods.
The invention has the beneficial effects that: the nanowires are formed on the platinum-based amorphous alloy by matching with an AAO template in a hot-pressing mode, are separated and collected in an ultrasonic mode, and are used for oxygen reduction catalysis, the surface area can be increased by the nanowires to achieve more active sites to improve the reaction efficiency, the reduction catalysis performance is stable, the process requirement is simple, the preparation time is short, the repeatability is strong, the collection is convenient, and the preparation method is suitable for large-scale production.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is a process diagram of the preparation method of the platinum-based amorphous alloy nanowires of the present invention;
FIG. 2 is SEM images of platinum-based amorphous alloy nanowires prepared by the method of the invention under different resolutions;
FIG. 3 is SEM images of separated platinum-based amorphous alloy nanowires prepared by the present invention at different resolutions;
FIG. 4 is a TEM image of isolated platinum-based amorphous alloy nanowires prepared by the present invention;
FIG. 5 is an X-ray diffraction pattern of platinum-based amorphous alloy nanowires prepared according to the present invention;
FIG. 6 is a cyclic voltammetry scanning diagram of platinum-based amorphous alloy nanowires prepared by the invention under 0.1mol KOH solution, nitrogen atmosphere and saturated oxygen atmosphere;
FIG. 7 is a linear sweep voltammetry scan (compared with platinum carbon catalyst) of the platinum-based amorphous alloy nanowires prepared by the invention in a 0.1mol KOH solution under a saturated oxygen atmosphere;
FIG. 8 is a Tafel plot of platinum-based amorphous alloy nanowires prepared according to the present invention in a 0.1mol KOH solution under a saturated oxygen atmosphere (compare with a platinum-carbon catalyst);
FIG. 9 is a graph of current density versus time (j-t) for electrocatalytic oxygen reduction of platinum-based amorphous alloy nanowires prepared according to the present invention in a 0.1mol KOH solution under a saturated oxygen atmosphere.
Detailed Description
Referring to fig. 1, the preparation method of the platinum-based amorphous alloy nanowires for oxygen reduction catalysis of the present invention comprises the following steps:
s1, mixing platinum (Pt), nickel (Ni), copper (Cu) and phosphorus (P) according to the mass ratio of 36:1:3:2, smelting and suction casting to obtain the amorphous alloy bar.
The method comprises the following specific operations: according to the principle of high melting point and low melting point, firstly, platinum, nickel and copper are stacked in a copper cavity of a WK series vacuum electric arc furnace, the electric arc furnace is pumped to low vacuum of 5Pa or below by a mechanical pump, and then a molecular pump of the electric arc furnace is switched on to pump high vacuum to 3 x 10-3And Pa, introducing argon protective gas, striking an arc gun, and burning a titanium ingot by using 120A current to absorb oxygen so as to ensure that no oxygen exists in the reaction furnace. The current is aligned to the copper cavity, and the arc current is adjusted to 70-120A, so that the raw materials are uniformly fused together to form the master alloy. And then, filling the smelted master alloy and the phosphorus weighed according to the proportion into a test tube, sealing the test tube by using a PyCoPyPrein station tube sealing machine, placing the test tube on the tube sealing machine at an inclination angle of 15 degrees to rotate at 10 r/min, pumping the test tube to 5Pa in vacuum by using a mechanical pump, and sealing the opening of the test tube by using a CopIcPrein water fuel oxyhydrogen machine at the flow rate of 200 plus 300L/H. The test tube is mounted on a vacuum rapid quenching spray casting machine, a mechanical pump is used for pumping the test tube to a low vacuum of 5Pa or below, and a molecular pump of the spray casting machine is started to pump the test tube to a high vacuum of 3 multiplied by 10-3Pa, then introducing argon protective gas, opening electromagnetic induction melting, stepping on a pedal to adjust the current by 20A until the raw materials in the tube are completely melted. Adding boron trioxide for purification, placing the test tube on a vacuum rapid quenching injection molding machine, pumping to low vacuum of 5Pa or below by using a mechanical pump, and opening a molecular pump of the injection molding machine to pump high vacuum to 3 DEG×10-3Pa, then introducing argon protective gas, opening electromagnetic induction melting, stepping on a pedal to adjust the current by 20A until the raw materials in the tube are completely melted. Finally, the master alloy melted with phosphorus is stacked in a copper cavity of a WK series vacuum arc furnace, the arc furnace is pumped to low vacuum of 5Pa or below by a mechanical pump, and a molecular pump of the arc furnace is switched on to pump high vacuum to 3 multiplied by 10-3And Pa, introducing argon protective gas, striking an arc gun, and burning a titanium ingot by using 120A current to absorb oxygen so as to ensure that no oxygen exists in the reaction furnace. The current is aligned to the copper cavity, the arc current is adjusted to 70-120A, the raw materials are uniformly fused together, and then the suction casting button is pressed, so that the amorphous alloy bar is obtained by suction casting.
The diameter, length, etc. of the amorphous alloy bar may be determined corresponding to the forming die, such as 5mm in diameter, etc.
S2, cutting the amorphous alloy bar into amorphous alloy discs 10 with a predetermined thickness by using a wire cutter and a diamond cutter in a radial direction, as shown in fig. 1 (a).
The thickness of the amorphous alloy disk 10 may be, but is not limited to, 75mm to 80 mm. According to the selection of the whole length and the preset thickness of the amorphous alloy bar, the amorphous alloy bar can be cut into a plurality of amorphous alloy wafers 10, and 600-2000 sand paper is used for grinding and polishing after cutting.
S3, overlapping the AAO template (alumina template) 20 with the nanometer-scale holes and the polished amorphous alloy wafer 10 in a mould 30, and carrying out hot pressing under an inert gas atmosphere and keeping the pressing for 15-30 seconds to obtain the amorphous alloy primary product 40.
Under the hot pressing, the amorphous alloy wafer 10 enters the nano-scale holes of the AAO template 20 under melting, and the nano-lines are formed corresponding to the nano-scale holes.
Wherein the hot pressing temperature is 200-205 ℃, and the hot pressing pressure is 15-20 kN.
The inert gas is preferably argon. Specifically, before argon gas is filled, vacuum pumping is firstly carried out to form low vacuum of 5Pa-10Pa, and then argon gas is filled.
The aperture of the nano-scale hole on the AAO template 20 is 100nm-300 nm. The diameter of the AAO template 20 superposed with the amorphous alloy wafer 10 is set corresponding to the diameter of the amorphous alloy wafer 10; for example, for an amorphous alloy wafer 10 having a diameter of 5mm, the AAO template 20 has a diameter of 5mm 2 mm.
When the outer diameter of the AAO template 20 is much larger than the diameter of the amorphous alloy wafer 10, the AAO template may be cut first and then placed in the cavity of the mold 30 in an up-down overlapping manner with the amorphous alloy wafer 10.
Within the cavity of mold 30, AAO template 20 is preferably positioned below and amorphous alloy wafer 10 is stacked above AAO template 20.
And S4, cooling to room temperature, taking the amorphous alloy primary product 40 out of the die 30, and performing surface anti-oxidation treatment.
Preferably, the surface oxidation preventing treatment of the amorphous alloy preform 40 is performed as follows: and putting the amorphous alloy primary product 40 into an absolute ethyl alcohol solution with the mass fraction of 0.3%.
As shown in fig. 1 (c), the amorphous alloy primary product 40 includes an amorphous alloy base sheet 41 and nanowires 42 formed on the amorphous alloy base sheet 41; the nanowires 42 are formed by hot melting an amorphous alloy into the nanoscale pores of the AAO template 20.
S5, immersing the amorphous alloy primary product 40 in a sodium hydroxide solution with a mass fraction of 15% for 30-50 minutes to completely dissolve the residual AAO template indicated by the amorphous alloy primary product 40 in the sodium hydroxide solution, removing the residual AAO template on the surface of the amorphous alloy primary product 40 to obtain the platinum-based amorphous alloy 50 with nanowires, and cleaning the surface of the amorphous alloy with ethanol, as shown in fig. 1 (c) to (d).
Before step S5, a sodium hydroxide solution is prepared: solid sodium hydroxide with the purity of 97 percent is adopted for preparation.
The component of the platinum-based amorphous alloy 50 is Pt57.5Cu14.7Ni5.3P22.5The structure of the nanowire is the same as that of the amorphous alloy primary product 40, and the nanowire comprises a bottom plate 51 and a nanowire 52 positioned on the bottom plate 51, wherein the nanowire 52 on the bottom plate 51 is formed by the nanowire 42 on the amorphous alloy primary product 40 and is also a platinum-based amorphous alloy nanowire 52.
S6, as shown in fig. 1 (e), placing the platinum-based amorphous alloy 50 in an ethanol solution, placing in an ultrasonic cleaner, performing ultrasonic treatment at room temperature for 45-60 minutes to peel the platinum-based amorphous alloy nanowires 52 from the substrate 51, then removing the ethanol solution at room temperature and low pressure by using a rotary evaporator, and collecting the platinum-based amorphous alloy nanowires 52 to obtain the platinum-based amorphous alloy nanowires 52 as a catalyst for oxygen reduction catalysis. Among the above, the low pressure is preferably 200Pa to 1000Pa, and more preferably 200 Pa.
SEM images of the platinum-based amorphous alloy nanowires prepared by the invention are respectively shown in FIGS. 2 (10 μm and 2 μm) and 3 (100 μm and 5 μm), and it can be seen from the figure that the platinum-based amorphous alloy nanowires have a three-dimensional structure and an increased active area for reaction. A TEM (transmission electron microscope) image of the platinum-based amorphous alloy nanowire is shown in fig. 4, and it is understood from the drawing that atoms are disordered and in an amorphous phase. The X-ray diffraction pattern of the platinum-based amorphous alloy nanowires is shown in FIG. 5.
The oxidation-reduction catalytic effect of the platinum-based amorphous alloy nanowire prepared by the method is detected as follows: 6.0mg of the platinum-based amorphous alloy nanowire is placed in a mixed solution formed by mixing 20uL of 5% perfluorosulfonate (Nafion), 700uL of water and 280uL of ethanol, and the mixture is subjected to ultrasonic treatment for 30 minutes and then is uniformly dispersed to form slurry. And then 20uL of the uniformly dispersed slurry is taken to be dripped on a glassy carbon electrode with the diameter of 5mm, and the glassy carbon electrode is used as a working electrode with the platinum-based amorphous alloy nanowire after being dried. A standard three-electrode system is used, a silver-silver chloride electrode is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, a glassy carbon electrode coated with platinum-based amorphous alloy nanowires is used as a working electrode, an electrolyte is 0.1M potassium hydroxide solution, and the catalytic performance of an oxygen reduction reaction is tested and tested by a circulating voltammetry method and a linear scanning voltammetry method in a saturated oxygen atmosphere by using a Chenghua CHI660 electrochemical workstation. The scanning speed in the cyclic voltammetry test is 20 mv/s, the scanning speed in the linear voltammetry test is 2 mv/s, the cyclic voltammetry scanning graph is shown in figure 6, and the oxygen reduction current in the electrolyte filled with oxygen is obviously higher than that in the electrolyte filled with nitrogen, so that the oxygen reduction effect is obvious.
The catalytic effect of the oxidation-reduction reaction of the platinum-based amorphous alloy nanowire obtained by the detection is as follows: the oxygen reduction half-peak potential of the reversible hydrogen electrode was 830mV compared to 850mV for a commercial platinum-carbon catalyst, and the linear sweep voltammetry scan pair of the two was as shown in FIG. 7. As shown in FIG. 8, the Tafel slope of the platinum-based amorphous alloy nanowires reached 62 mV/dec, which is close to 60 mV/dec of the platinum-carbon catalyst.
The j-t graph of the platinum-based amorphous alloy nanowire in the presence of 0.1mol of KOH solution and saturated oxygen is shown in FIG. 9, and the curve in the graph shows that the platinum-based amorphous alloy nanowire is long in circulation and stable in time in the aspect of oxidation-reduction catalysis.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (7)
1. A preparation method of a platinum-based amorphous alloy nanowire for oxygen reduction catalysis is characterized by comprising the following steps:
s1, mixing platinum, nickel, copper and phosphorus according to the mass ratio of 36:1:3:2, smelting and suction casting to obtain an amorphous alloy bar;
s2, cutting the amorphous alloy bar into amorphous alloy wafers with preset thickness;
the predetermined thickness is 75mm-80 mm;
s3, overlapping the AAO template with the nano-scale holes and the amorphous alloy wafer in a mold, and carrying out hot pressing in an inert gas atmosphere to obtain an amorphous alloy primary product;
the aperture of the nano-scale hole on the AAO template is 100nm-300 nm; the temperature of the hot pressing is 200-205 ℃;
the amorphous alloy primary product comprises an amorphous alloy bottom plate and a nanowire formed on the amorphous alloy bottom plate; the nano-wires are formed by the amorphous alloy entering the nano-scale holes of the AAO template through hot melting;
s4, cooling, taking the amorphous alloy primary product out of the mold, and carrying out surface anti-oxidation treatment;
the surface anti-oxidation treatment operation is as follows: putting the amorphous alloy primary product into an absolute ethyl alcohol solution with the mass fraction of 0.3%;
s5, immersing the amorphous alloy primary product with the surface subjected to anti-oxidation treatment into a sodium hydroxide solution with the mass fraction of 15%, and removing the residual AAO template on the surface to obtain the platinum-based amorphous alloy with the nanowires;
s6, placing the platinum-based amorphous alloy with the nanowires in an ethanol solution, performing ultrasonic treatment to separate the nanowires, and collecting the nanowires, wherein the nanowires are the platinum-based amorphous alloy nanowires.
2. The method for preparing platinum-based amorphous alloy nanowires for oxygen reduction catalysis as claimed in claim 1, wherein the diameter of the amorphous alloy wafer is 5 mm; the diameter of the AAO template is 5mm +/-2 mm.
3. The method of preparing platinum-based amorphous alloy nanowires for oxygen reduction catalysis as claimed in claim 1, wherein the pressure of the hot pressing in step S3 is 15kN-20 kN.
4. The method of claim 1, wherein in step S5, the surface-treated primary amorphous alloy is immersed in the sodium hydroxide solution for 30 to 50 minutes.
5. The method of claim 1, wherein in step S6, the platinum-based amorphous alloy nanowires are placed in an ethanol solution and ultrasonically treated with an ultrasonic cleaner for 45 to 60 minutes; and after the ultrasonic treatment is finished, removing the ethanol solution by adopting a rotary evaporator at the low pressure of 200-1000 Pa, and collecting the nanowires separated from the platinum-based amorphous alloy.
6. Root of herbaceous plantThe method for preparing platinum-based amorphous alloy nanowires for oxygen reduction catalysis according to any one of claims 1 to 5, wherein the platinum-based amorphous alloy comprises Pt as a component57.5Cu14.7Ni5.3P22.5。
7. A platinum-based amorphous alloy nanowire for oxygen reduction catalysis, which is characterized by being prepared by the preparation method of any one of claims 1 to 6.
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