CN114361472A - Preparation method of high-activity/anti-reversal-pole catalyst for proton exchange membrane fuel cell - Google Patents
Preparation method of high-activity/anti-reversal-pole catalyst for proton exchange membrane fuel cell Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-activity/anti-reversal-pole catalyst for a proton exchange membrane fuel cell, which comprises the following steps: adding MXene into a solvent A, and performing ultrasonic dispersion to obtain MXene dispersion liquid; ultrasonically dispersing a precursor of the catalytic active material in a solvent B uniformly for later use; mixing and stirring the dispersion liquid and the precursor solution of the catalytic active material; adding metal salt into the mixed solution, stirring, and pouring the mixed solution into a crucible for drying; placing the crucible containing the solid mixture obtained after drying in a box furnace for sintering for 0.1-20 hours; and adding a solvent C into the sintered solid, performing ultrasonic dispersion, then performing centrifugal washing to neutrality, and drying to obtain the high-activity/anti-reversal catalyst for the proton exchange membrane fuel cell. The catalyst prepared by the invention not only has good conductivity and specific surface area, but also has good electrolytic selectivity and anti-reversal capability.
Description
Technical Field
The invention relates to the field of electrocatalysis materials, in particular to a preparation method of a high-activity/anti-reversal catalyst for a proton exchange membrane fuel cell.
Background
In recent years, our country has paid high attention to the development of hydrogen energy, especially in the field of hydrogen fuel cell vehicles. Proton exchange membrane fuel cells used in hydrogen fuel cell vehicles have many advantages of high efficiency, direct conversion of internal fuel, convenient refueling, zero emission and the like, but the durability of proton exchange membrane fuel cells is a problem to be solved. The phenomenon of reversal is that when the fuel cell stack is under the working conditions of rapid load change, start and stop, and the like, or when the catalytic layer is flooded, and the like, hydrogen fuel supply is insufficient locally at the anode, the anode potential is increased, the voltage of a single cell is reduced and even becomes a negative value, namely, the phenomenon of reversal occurs, and permanent damage can be caused to the performance of the cell. The traditional antipole catalyst is noble metal oxide such as ruthenium, iridium and the like, the HOR catalytic performance and the electrical conductivity of the oxide are poor, the antipole time is short, the effect is not ideal, and the price is high. Therefore, the design and development of the novel anode anti-reversal catalyst for the proton exchange membrane fuel cell not only can obviously improve the performance and anti-reversal characteristics of the cell, but also can reduce the material cost and promote the commercialization process of the hydrogen fuel cell.
Disclosure of Invention
The invention aims to provide a preparation method of a high-activity/anti-reversal catalyst for a proton exchange membrane fuel cell, the prepared catalyst has good catalytic performances of Hydrogen Oxidation (HOR) and electrolytic water Oxygen Evolution (OER), has good conductivity and specific surface area, and also has good electrolytic selectivity, namely, the anode preferentially generates oxidation reaction of water under the condition of hydrogen deficiency so as to reduce corrosion of a carbon carrier, and has good anti-reversal capability.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a high-activity/anti-reversal-pole catalyst for a proton exchange membrane fuel cell comprises the following steps:
step 1: adding MXene into a solvent A, and uniformly dispersing by ultrasonic to obtain MXene dispersion liquid;
step 2: calculating the amount of a precursor of the required catalytic active material according to the proportion that the mass of the catalytic active material is 1-60% of the total mass of the catalyst, and ultrasonically dispersing the precursor of the catalytic active material in a solvent B uniformly for later use;
and step 3: mixing the dispersion liquid and the solution obtained in the step 1 and the step 2, and magnetically stirring for 0.1-20 hours;
and 4, step 4: weighing a certain amount of metal salt, adding the metal salt into the mixed solution obtained in the step (3), and magnetically stirring for 0.1-20 hours;
and 5: pouring the mixed solution obtained in the step (4) into a crucible, placing the crucible into an oven for drying treatment, and drying for 1-40 hours at the temperature of 20-120 ℃;
step 6: placing the crucible containing the solid mixture obtained after drying in the step 5 into a box furnace for sintering for 0.1-20 hours at the sintering temperature of 100-600 ℃;
and 7: adding a certain amount of solvent C into the sintered solid obtained in the step 6, and performing ultrasonic dispersion for 0.1-20 hours;
and 8: and (4) centrifugally washing the mixed solution obtained in the step (7) to be neutral, and drying to obtain the high-activity/anti-reversal catalyst for the proton exchange membrane fuel cell.
Preferably, the raw materials comprise the following components in parts by weight: 0.1-20 parts of MXene, 0.1-100 parts of a precursor of a catalytic active material, 1-200 parts of a metal salt, 1-400 parts of a solvent A, 1-400 parts of a solvent B, and 1-400 parts of a solvent C.
Preferably, the MXene is Ti3C2、Ti2C、Nb3C2、Nb2C、TiNbC、Cr2TiC、Ti3CN、Ti4N3、Ta4C3、V2C、Mo2C or MoTiC2。
Preferably, the catalytically active material precursor is RuCl3·xH2O、RuCl3、H2PtCl6·6H2O、H2IrCl6·6H2O、PdCl2、PtCl4、AuCl、Na2PdCl4、K2PdCl6One or more of them.
Preferably, the metal salt is NaNO3、KNO3、Ca(NO3)2、Mg(NO3)2、MgCl2、NaCl、KCl、Na2SO4、K2SO4、MgSO4、CaSO4One or more of them.
Preferably, the solvent A, the solvent B and the solvent C are respectively one or more of deionized water, ethanol, ethylene glycol, isopropanol and n-butanol.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention takes MXene as a carrier, carries metal active particles, and improves the catalytic activity and the anti-reversal property of the material by utilizing the interaction of metal and the carrier. The prepared catalyst has good catalytic performances of Hydrogen Oxidation (HOR) and electrolytic water Oxygen Evolution (OER), has good conductivity and specific surface area, and also has good electrolytic selectivity, namely the anode preferentially generates oxidation reaction of water under the condition of hydrogen deficiency to reduce corrosion of a carbon carrier, and has good anti-polarity capability.
(2) MXene as a two-dimensional material has large specific surface area and surface defects, so that the active area can be greatly increased, an anchoring site can be effectively provided for metal particles, and the catalytic reaction and the material stability are facilitated.
(3) According to the invention, some metal salts with good thermal stability and solubility are used as sintering media, and the agglomeration of materials is effectively inhibited in the sintering process, so that the appearance of a sintered sample is kept good.
(4) The invention adopts lower sintering temperature, so that the precursor is only partially oxidized. The oxidized fraction has good OER catalytic properties and it is reduced to metal active particles by hydrogen in the fuel cell anode, thus having good HOR properties and electrical conductivity. The addition of the bifunctional catalyst not only improves the performance of the fuel cell, but also greatly improves the anti-reversal capability of the fuel cell.
Drawings
FIG. 1 shows RuO in example 1 of the present invention2@Ti3C2TxThe concentration of the antipole catalyst is 0.1mol L-1HOR performance test chart in perchloric acid aqueous solution;
FIG. 2 shows RuO in example 1 of the present invention2@Ti3C2TxThe concentration of the antipole catalyst is 0.1mol L-1The OER performance test chart in the perchloric acid aqueous solution;
FIG. 3 shows RuO in example 1 of the present invention2@Ti3C2TxAnti-reversal catalyst used as fuel cell anode catalyst in combination with commercial Pt/C and pure commercial Pt/C (RT stands for RuO in the legend)2@Ti3C2Tx) Cell performance plots under hydrogen air and hydrogen oxygen conditions, respectively.
FIG. 4 shows RuO in example 1 of the present invention2@Ti3C2TxThe addition of the catalyst increased the cell anti-reversal time by a factor of 38 when used in conjunction with commercial Pt/C as the fuel cell anode catalyst and pure commercial Pt/C as the fuel cell anode catalyst in the hydrogen-free condition for the anti-reversal test.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
Example 1
In this embodiment, a high activity/anti-reverse catalyst for a proton exchange membrane fuel cell is prepared from the following raw materials: ti3C2Tx50mg、RuCl3·xH2O 217mg、NaNO32g, ethanol 25ml and deionized water 75 ml.
A preparation method of a high-activity/anti-reversal-pole catalyst for a proton exchange membrane fuel cell comprises the following steps:
step 1: 50mg of Ti3C2TxPlacing the mixture in 25ml of ethanol, and ultrasonically dispersing for 2 hours;
step 2: 217mgRuCl3·xH2O is put in 25ml for separationCarrying out ultrasonic treatment for 2 hours in the child water;
and step 3: mixing the two solutions, and stirring for 2 hours;
and 4, step 4: 2g of NaNO3Adding the mixture into the mixed solution, and stirring for 2 hours;
and 5: pouring the mixed solution into a crucible, and drying for 12 hours in an oven at 60 ℃;
step 6: placing the dried crucible containing the solid mixture in a box furnace, sintering for 0.1-20 hours, heating to 350 ℃, preserving heat for 1 hour, and cooling along with the furnace;
and 7: taking out the crucible, adding 50ml of deionized water, placing the crucible in an ultrasonic machine for dispersing for 2 hours, and then centrifugally cleaning the crucible to be neutral by using the deionized water and ethanol;
and 8: vacuum filtering and drying at 60 ℃ for 12 hours to obtain powdered RuO2@Ti3C2TxThe anode was resistant to reverse catalyst and then tested for electrochemical half and full cells.
RuO in half cell HOR test, as shown in FIG. 12@Ti3C2TxThe antipole catalyst showed 1mA cm-2The limiting current of (a) indicates that certain HOR catalytic performance is achieved; as shown in FIG. 2, in the half-cell OER test, the current density was 10mA cm-2RuO (r) 22@Ti3C2TxThe anti-bipolar catalyst showed 263mV overpotential, indicating good OER catalytic performance.
In full cell testing, a commercial 60% platinum-carbon catalyst, RuO, was incorporated2@Ti3C2TxAdding into the anode by means of additive, wherein the loading of platinum and ruthenium are both 0.1mg cm-2(ii) a The loading capacity of the cathode platinum is 0.3mg cm-2And the back pressure of 0.1MPa is additionally applied to both the cathode and the anode. As shown in FIG. 3, the cell exhibited 1.04W cm under hydrogen air conditions with both the cathode and anode being commercial 60% platinum carbon catalyst-2Peak power density of (d); in contrast, anti-antipole catalyst RuO2@Ti3C2TxSo that the peak power density of the battery is increased to 1.13W cm-2Improve appointment9 percent. As shown in FIG. 4, the peak power density of the former is 1.92W cm under hydrogen-oxygen condition-2The peak power density of the latter cell is 2.28W cm-2The improvement is about 18%. In the anode anti-reversal test, the conventional commercial 60% platinum-carbon catalyst anti-reversal time is about 5 min; in contrast, anode adds RuO2@Ti3C2TxAfter the catalyst is used for resisting the reverse polarity, the reverse polarity resisting time is 189min which is 38 times of that of the catalyst. This indicates that RuO2@Ti3C2TxThe addition of the anti-reversal catalyst not only improves the performance of the battery, but also greatly improves the anti-reversal capability of the battery.
Example 2
In this embodiment, a high activity/anti-reverse catalyst for a proton exchange membrane fuel cell is prepared from the following raw materials: ti3C2Tx 100mg、RuCl3·xH2O 217mg、KNO33g, n-butanol 50ml and deionized water 75 ml.
A preparation method of a high-activity/anti-reversal-pole catalyst for a proton exchange membrane fuel cell comprises the following steps:
step 1: mixing 100mg of Ti3C2TxPlacing the mixture in 50ml of deionized water, and carrying out ultrasonic dispersion for 3 hours;
step 2: 217mgRuCl3·xH2Placing O in 25ml of deionized water, and carrying out ultrasonic treatment for 3 hours;
and step 3: mixing the two solutions, and stirring for 3 hours;
and 4, step 4: mixing 3g KNO3Adding the mixture into the mixed solution, and stirring for 3 hours;
and 5: pouring the mixed solution into a crucible, and drying for 12 hours in an oven at 60 ℃;
step 6: placing the dried crucible containing the solid mixture in a box furnace, sintering for 0.1-20 hours at a temperature rising speed of 10 ℃ for min-1Heating to 300 ℃, preserving heat for 2 hours, and cooling along with the furnace;
and 7: taking out the crucible, adding 50ml of deionized water, placing the crucible in an ultrasonic machine for dispersing for 2 hours, and then centrifugally cleaning the crucible to be neutral by using the deionized water and ethanol;
and 8: vacuum filtering and drying at 60 ℃ for 12 hours to obtain powdered RuO2@Ti3C2TxThe anode was resistant to reverse catalyst and then tested for electrochemical half and full cells.
RuO in half-cell HOR test2@Ti3C2TxThe antipole catalyst showed 0.7mA cm-2The limiting current of (a) indicates that certain HOR catalytic performance is achieved; RuO in half-cell OER test2@Ti3C2TxThe anti-bipolar catalyst showed an overpotential of 304mV, indicating good OER catalytic performance. In full cell testing, a commercial 60% platinum-carbon catalyst, RuO, was incorporated2@Ti3C2TxAdding into the anode by means of additive, wherein the loading of platinum and ruthenium are both 0.1mg cm-2(ii) a The loading capacity of the cathode platinum is 0.3mg cm-2And the back pressure of 0.1MPa is additionally applied to both the cathode and the anode. Under the condition of hydrogen air, the addition of the catalyst improves the battery performance by 2 percent and improves the anti-reversal time to 20 times of the original time. This shows that the addition of the anti-reversal catalyst not only improves the battery performance, but also improves the anti-reversal capability of the battery.
Example 3
In this embodiment, a high activity/anti-reverse catalyst for a proton exchange membrane fuel cell is prepared from the following raw materials: MoTiC2 100mg、H2IrCl6·6H2O250 mg, KCl 3g, isopropanol 50ml and deionized water 75 ml.
A preparation method of a high-activity/anti-reversal-pole catalyst for a proton exchange membrane fuel cell comprises the following steps:
step 1: mixing 100mgMoTiC2Placing the mixture in 50ml of deionized water, and carrying out ultrasonic dispersion for 3 hours;
step 2: mixing 250mgH2IrCl6·6H2Placing O in 25ml of deionized water, and carrying out ultrasonic treatment for 3 hours;
and step 3: mixing the two solutions, and stirring for 3 hours;
and 4, step 4: adding 3g of KCl into the mixed solution, and stirring for 3 hours;
and 5: pouring the mixed solution into a crucible, and drying for 12 hours in an oven at 60 ℃;
step 6: placing the dried crucible containing the solid mixture in a box furnace, sintering for 0.1-20 hours at a temperature rising speed of 10 ℃ for min-1Heating to 300 ℃, preserving heat for 2 hours, and cooling along with the furnace;
and 7: taking out the crucible, adding 50ml of deionized water, placing the crucible in an ultrasonic machine for dispersing for 2 hours, and then centrifugally cleaning the crucible to be neutral by using the deionized water and ethanol;
and 8: vacuum filtering, and drying at 60 deg.C for 12 hr to obtain powdered IrO2@MoTiC2The anode was resistant to reverse catalyst and then tested for electrochemical half and full cells.
In the half-cell OER test, IrO2@MoTiC2The anti-bipolar catalyst showed an overpotential of 320mV, indicating good OER catalytic performance. In the full cell test, a commercial 60% platinum-carbon catalyst, IrO, was used in combination2@MoTiC2Added into the anode in an additive mode, wherein the loading amount of platinum and iridium is 0.1mg cm-2And 0.05mg cm-2(ii) a The loading capacity of the cathode platinum is 0.3mg cm-2And the back pressure of 0.1MPa is additionally applied to both the cathode and the anode. Under the condition of hydrogen air, the addition of the catalyst improves the battery performance by 1 percent and improves the anti-reversal time to 50 times of the original time. This shows that the addition of the anti-reversal catalyst not only improves the battery performance, but also improves the anti-reversal capability of the battery.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.
Claims (6)
1. A preparation method of a high-activity/anti-reversal catalyst for a proton exchange membrane fuel cell is characterized by comprising the following steps:
step 1: adding MXene into a solvent A, and uniformly dispersing by ultrasonic to obtain MXene dispersion liquid;
step 2: calculating the amount of a precursor of the required catalytic active material according to the proportion that the mass of the catalytic active material is 1-60% of the total mass of the catalyst, and ultrasonically dispersing the precursor of the catalytic active material in a solvent B uniformly for later use;
and step 3: mixing the dispersion liquid and the solution obtained in the step 1 and the step 2, and magnetically stirring for 0.1-20 hours;
and 4, step 4: weighing a certain amount of metal salt, adding the metal salt into the mixed solution obtained in the step (3), and magnetically stirring for 0.1-20 hours;
and 5: pouring the mixed solution obtained in the step (4) into a crucible, placing the crucible into an oven for drying treatment, and drying for 1-40 hours at the temperature of 20-120 ℃;
step 6: placing the crucible containing the solid mixture obtained after drying in the step 5 into a box furnace for sintering for 0.1-20 hours at the sintering temperature of 100-600 ℃;
and 7: adding a certain amount of solvent C into the sintered solid obtained in the step 6, and performing ultrasonic dispersion for 0.1-20 hours;
and 8: and (4) centrifugally washing the mixed solution obtained in the step (7) to be neutral, and drying to obtain the high-activity/anti-reversal catalyst for the proton exchange membrane fuel cell.
2. The preparation method of the high-activity/anti-reversal catalyst for the proton exchange membrane fuel cell according to claim 1, which is characterized in that the raw materials comprise the following components in parts by mass: 0.1-20 parts of MXene, 0.1-100 parts of a precursor of a catalytic active material, 1-200 parts of a metal salt, 1-400 parts of a solvent A, 1-400 parts of a solvent B, and 1-400 parts of a solvent C.
3. The method of claim 1, wherein the method comprises the steps of: the MXene is Ti3C2、Ti2C、Nb3C2、Nb2C、TiNbC、Cr2TiC、Ti3CN、Ti4N3、Ta4C3、V2C、Mo2C or MoTiC2。
4. The method of claim 1, wherein the method comprises the steps of: the precursor of the catalytic active material is RuCl3·xH2O、RuCl3、H2PtCl6·6H2O、H2IrCl6·6H2O、PdCl2、PtCl4、AuCl、Na2PdCl4、K2PdCl6One or more of them.
5. The method of claim 1, wherein the method comprises the steps of: the metal salt is NaNO3、KNO3、Ca(NO3)2、Mg(NO3)2、MgCl2、NaCl、KCl、Na2SO4、K2SO4、MgSO4、CaSO4One or more of them.
6. The method of claim 1, wherein the method comprises the steps of: the solvent A, the solvent B and the solvent C are respectively one or more of deionized water, ethanol, ethylene glycol, isopropanol and n-butanol.
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