CN111554946B - Pt alloy with high HOR catalytic activity and preparation method and application thereof - Google Patents

Pt alloy with high HOR catalytic activity and preparation method and application thereof Download PDF

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CN111554946B
CN111554946B CN202010327965.7A CN202010327965A CN111554946B CN 111554946 B CN111554946 B CN 111554946B CN 202010327965 A CN202010327965 A CN 202010327965A CN 111554946 B CN111554946 B CN 111554946B
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达斯汀.威廉.班哈姆
彭晔
崔自然
白金勇
张翼
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Guangdong Taiji Power Technology Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/90—Selection of catalytic material
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    • H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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Abstract

The invention discloses a Pt alloy with high HOR catalytic activity, a preparation method and application thereof, wherein the specific surface area of the Pt alloy is not less than 30m2The grain diameter is 3-9 nm, and the alloy is Pt-Ir alloy, Pt-Au alloy or Pt-Ag alloy. The Pt alloy has better HOR catalytic activity, can reduce the consumption of PGM under the condition of ensuring that the performance of the anode is not influenced when being applied to the MEA anode of the PEMFC, and is beneficial to reducing the cost of the PEMFC.

Description

Pt alloy with high HOR catalytic activity and preparation method and application thereof
Technical Field
The invention relates to the field of fuel cells, in particular to a fuel cell catalyst and a preparation method and application thereof.
Background
Proton Exchange Membrane Fuel Cells (PEMFCs) are used in an increasing number of fields with the ultimate goal of being used as a power source, including those for buses, trucks, and general passenger vehicles. The MEA is the core of the PEMFC and consists of a membrane sandwiched between two electrodes (anode and cathode) which are themselves sandwiched between two gas diffusion layers.
In the prior art, commercial MEA usually contains PGM of platinum group metals in an amount of about 0.25 to 0.3mg/cm2The consumption of the fuel cell passenger car is about 25-35 g in conversion, which is 4-6 times of the consumption of PGM in the traditional fuel car catalytic converter. PGM is relatively expensive and limited in production, and the amount of PGM degrading used has the property of PEMFCOf great significance.
The loading target for PGM in the PEMFCs MEA was about 0.125mg/cm2. MEA in which 80% of PGM is supported on the cathode and about 0.125mg/cm2The PGM supporting amount of (A) means that the supporting amount of the PGM of the cathode is about 0.10mg/cm2The loading of PGM on the anode was about 0.025mg/cm2. In the conventional MEA, the PGM loading amount on the anode is 0.05-0.10 mg/cm2. This places higher demands on the catalytic activity of the PGM on the anode.
Studies have shown that the Pt loading on the anode of the MEA is from 0.10mg/cm2Reduced to 0.05mg/cm2The MEA performance is not substantially affected. In view of this fact, the load on the anode of the existing MEA exceeds 0.05mg/cm2The only motivation for Pt is to provide a performance margin against CO or H in the combustion gas2S contamination leads to loss of catalytic performance, degradation of the anode by "reverse" reactions. The load amount of Pt on the MEA anode is 0.05-0.10 mg/cm2The reason why the performance does not decrease is a sharp change in the HOR (hydrogen oxidation reaction) power curve. But when the Pt loading is less than 0.05mg/cm2When the HOR curve of PEMFC is no longer constant, a significant performance drop can be observed (fig. 1). Apparently, although Pt is the most promising HOR catalyst, it cannot be at about 0.025mg/cm2At a loading level to provide sufficient catalytic performance. To further reduce the Pt loading in the anode, the only viable approach is to increase the HOR performance of the catalyst on which it is supported.
Disclosure of Invention
It is an object of the present invention to overcome at least one of the disadvantages of the prior art and to provide a Pt alloy with a higher HOR catalytic activity and its use.
The technical scheme adopted by the invention is as follows:
in a first aspect of the present invention, there is provided:
a Pt alloy having a specific surface area of not less than 30m2The grain diameter is 3-9 nm, and the Pt alloy is selected from the following components:
the Pt-Ir alloy comprises 45 to 55 percent of Ir in molar percentage and the balance of Pt; or
The alloy comprises Pt-Au, wherein the mole percentage of Au is 5-15%, and the balance is Pt; or
The Pt-Ag alloy comprises 5-15% of Ag in mole percentage and the balance of Pt.
In some examples, the molar percentage of Ir in the Pt-Ir alloy is 48 to 55%, preferably 50 to 55%, and more preferably 52 to 55%.
In some examples, the molar percentage of Au in the Pt-Au alloy is 9 to 13%, preferably 11 to 13%.
In some examples, the molar percentage of Ag in the Pt-Ag alloy is 8-15%, preferably 8-12%, and more preferably 10-12%.
In some examples, the molar percentage of Ir in the Pt-Ir alloy is 52%.
In some examples, the mole percentage of Au in the Pt-Au alloy is 11%.
In some examples, the mole percent of Ag in the Pt-Ag alloy is 10%.
In a second aspect of the present invention, there is provided:
use of a Pt alloy as described in the first aspect of the invention in the manufacture of a catalyst for the anode of a fuel cell MEA.
In some examples, the Pt alloy is loaded at the anode of the MEA at 0.01-0.05 mg/cm2，0.01～0.04mg/cm2，0.01～0.03mg/cm2。
In a third aspect of the present invention, there is provided:
an MEA comprising an anode carrying the Pt alloy of the first aspect of the present invention.
In some examples, the Pt alloy is loaded at the anode of the MEA at a load of 0.01-0.05 mg/cm2，0.01～0.04mg/cm2，0.01～0.03mg/cm2。
In a fourth aspect of the present invention, there is provided:
a proton exchange membrane fuel cell, wherein the anode uses a catalyst comprising the Pt alloy of the first aspect of the present invention; or with an MEA according to the third aspect of the invention.
In a fifth aspect of the present invention, there is provided:
the method for producing a Pt alloy according to the first aspect of the present invention includes:
s1) dissolving a water-soluble Pt salt and another water-soluble alloy element salt in a polar solvent;
s2), adding a reducing agent, and reacting to obtain the Pt alloy.
In some examples, the Pt alloy is a Pt-Ir alloy, and the method of making comprises:
s1) dissolving a Pt salt and an Ir salt in 1, 2-propylene glycol, and fully carrying out solvothermal reaction at 130-180 ℃ in a pressure container;
s2) after the solvothermal reaction is finished, cooling, adding a non-polar solution of octane thiol, and fully mixing;
s3), adding water, mixing uniformly, separating liquid, collecting a non-polar solvent phase, and removing the non-polar solvent to obtain the Pt-Ir alloy.
In some examples, the Pt alloy is a Pt-Au alloy, and the method of making comprises:
s1) dripping the Pt salt solution and the Au salt solution into the citric acid solution, and fully and uniformly mixing;
s2) adding NaBH4Fully and uniformly mixing the solution;
s3), adding 2-propanol, and fully and uniformly mixing for reaction;
s4), collecting a solid phase product after the reaction is finished, washing and drying to obtain the Pt-Au alloy.
In some examples, the Pt alloy is a Pt-Ag alloy, and the method of making comprises:
s1) mixing the Pt salt solution, the Ag salt solution, the poly (N-isopropyl acrylamide) water solution and water evenly;
s2), adding a formaldehyde solution, uniformly dispersing, transferring into a hydrothermal reaction kettle, and reacting at 120-160 ℃;
s3), collecting a solid-phase product after the reaction is finished, washing and drying to obtain the Pt-Ag alloy.
In some examples, the Pt salt is selected from H2PtCl6The Ir salt is selected from IrCl3The Au salt is selected from HAuCl4、Ag salt is selected from AgNO3。
In some examples, the method of making the Pt-Ir alloy includes:
S1)0.27mmol IrCl3and 0.25mmol of PtCl2Dissolving in 100mL of 1, 2-propylene glycol, reacting at 165 ℃ for 15min, and vigorously stirring until the solution becomes dark brown to obtain a colloidal solution;
s2) cooling the colloidal solution to room temperature, adding a mixed solution of 20mL of toluene and 0.3g of octane thiol, and stirring overnight;
s3) adding 20mL of deionized water, separating, collecting a toluene phase, and distilling under reduced pressure to obtain the product.
In some examples, the method of making the Pt-Au alloy includes:
s1) dissolving 1.5mL of 0.1 mM sodium citrate solution in 400mL of water, stirring vigorously for 10min, and adding 1mL of 9.1mg Pt/mL H dropwise2PtCl6And 0.25mL4.46 mg Au/mL HAuCl4Stirring the solution vigorously for 10 min;
s2) adding fresh NaBH in one portion4Solution, stirring vigorously for 5min, the NaBH4The solution was composed of 22.5mg NaBH4Dissolved in a solution of 3.5mL of water and 1.5mL of 0.1M sodium citrate;
s3) adding 10mL of 2-propanol, and stirring for 4 h;
s4), centrifugally collecting the product, washing the product by deionized water until no chloride ions exist, and drying the product to obtain the Pt-Au alloy.
In some examples, the method of preparing the Pt-Ag alloy includes:
S1)0.21mL50 mM AgNO3aqueous solution, 1.25mL50 mM H2PtCl6The solution, 5.0mL of 50 mM Mw. ═ 2500 poly (N-isopropylacrylamide) solution, and 35mL were mixed well;
s2), dropwise adding 2.5mL of 40 wt.% formaldehyde solution, performing ultrasonic treatment for 5min, transferring the solution into a 100mL hydrothermal reaction kettle, sealing, and keeping the temperature at 140 ℃ for 6 hours;
s3), cooling to room temperature after the reaction is finished, centrifugally collecting the product, washing for 3 times by deionized water and acetone, and drying to obtain the Pt-Ag alloy.
The invention has the beneficial effects that:
the Pt alloy has better HOR catalytic activity, can reduce the consumption of PGM under the condition of ensuring that the performance of the anode is not influenced when being applied to the MEA anode of the PEMFC, and is beneficial to reducing the cost of the PEMFC.
Drawings
FIG. 1 is the effect of anode Pt loading on HOR;
FIG. 2 is a graph of the effect of increased HOR catalytic activity on the overall performance of the MEA.
Detailed Description
A representative Pt alloy was prepared as follows:
the preparation method of the Pt-Ir alloy comprises the following steps:
S1)0.27mmol IrCl3and 0.25mmol of PtCl2Dissolving in 100mL of 1, 2-propylene glycol, reacting at 165 ℃ for 15min, and vigorously stirring until the solution becomes dark brown to obtain a colloidal solution;
s2) cooling the colloidal solution to room temperature, adding a mixed solution of 20mL of toluene and 0.3g of octane thiol, and stirring overnight;
s3) adding 20mL of deionized water, separating, collecting a toluene phase, and distilling under reduced pressure to obtain the product.
The preparation method of the Pt-Au alloy comprises the following steps:
s1) dissolving 1.5mL of 0.1 mM sodium citrate solution in 400mL of water, stirring vigorously for 10min, and adding 1mL of 9.1mg Pt/mL H dropwise2PtCl6And 0.25mL4.46 mg Au/mL HAuCl4Stirring the solution vigorously for 10 min;
s2) adding fresh NaBH in one portion4Solution, stirring vigorously for 5min, the NaBH4The solution was composed of 22.5mg NaBH4Dissolved in a solution of 3.5mL of water and 1.5mL of 0.1M sodium citrate;
s3) adding 10mL of 2-propanol, and stirring for 4 h;
s4), centrifugally collecting the product, washing the product by deionized water until no chloride ions exist, and drying the product to obtain the Pt-Au alloy.
The preparation method of the Pt-Ag alloy comprises the following steps:
S1)0.21mL50 mM AgNO3aqueous solution, 1.25mL50 mM H2PtCl6The solution, 5.0mL of 50 mM Mw. ═ 2500 poly (N-isopropylacrylamide) solution, and 35mL were mixed well;
s2), dropwise adding 2.5mL of 40 wt.% formaldehyde solution, performing ultrasonic treatment for 5min, transferring the solution into a 100mL hydrothermal reaction kettle, sealing, and keeping the temperature at 140 ℃ for 6 hours;
s3), cooling to room temperature after the reaction is finished, centrifugally collecting the product, washing for 3 times by deionized water and acetone, and drying to obtain the Pt-Ag alloy.
S4) by adjusting the proportion of the water-soluble metal salt, Pt alloys with different proportions can be obtained.
The detection result shows that the specific surface area of the Pt alloy particles obtained by the solution reaction is not less than 30m2(iii) per gram, the particle size is between 3 and 9 nm.
Other methods can also be used for reference to prepare the Pt alloy.
HOR catalytic Activity comparison of different Pt alloys
Taking the prepared specific surface area not less than 30m2(g) Pt alloy particles with different molar compositions and particle diameters of 3-9 nm (the specific surface area, the particle diameters and the like have no obvious difference compared), and the loading capacity (0.005-0.070 mg/cm) of the Pt alloy particles at different anodes is respectively tested2) Anode over-potentials (performance losses) were calculated and the HOR catalytic activity was calculated under different conditions, and the results are shown in table 1.
TABLE 1 Effect of different treatments on anodic overpotential (HOR activity)
Figure BDA0002463898300000051
Figure BDA0002463898300000061
As is clear from table 1, there is a narrower range of alloy compositions for the PtIr, PtAu and PtAg alloys, within which Pt alloys unexpectedly have better HOR catalytic activity (manifested as a significant drop in anode overpotential) than Pt, thereby improving the performance of the MEA as a whole.
0.025mg/cm respectively loaded on the anode2Pt or Pt alloy (Pt)52Ir48) MEAs were fabricated and tested for polarization curves under different conditions, with the results shown in figure 2. The results show that the cell voltage increased by about 25mV for the Pt alloy at 75 ℃, 136kPa, 100% RH compared to the conventional anode HOR catalyst Pt/C due to the increase in HOR catalytic activity (resulting in a decrease in anode overpotential).

Claims (8)

  1. The application of the Pt alloy in preparing the catalyst for the anode of the fuel cell MEA (membrane electrode assembly), which is characterized in that the loading amount of the Pt alloy is 0.01-0.05 mg/cm2The specific surface area of the Pt alloy is not less than 30m2The particle size is 3-9 nm, and the Pt alloy is selected from the following components:
    the Pt-Ir alloy comprises 45 to 55 percent of Ir in molar percentage and the balance of Pt; or
    The alloy comprises Pt-Au, wherein the mol percent of Au is 11-13%, and the balance is Pt; or
    The Pt-Ag alloy comprises 8-12% of Ag in mole percentage and the balance of Pt.
  2. 2. Use according to claim 1, characterized in that:
    the mole percentage of Ir in the Pt-Ir alloy is 48-55%.
  3. 3. Use according to claim 2, characterized in that:
    the mole percentage of Ir in the Pt-Ir alloy is 50-55%.
  4. 4. Use according to claim 3, characterized in that:
    the molar percentage of Ir in the Pt-Ir alloy is 52-55%.
  5. 5. Use according to claim 1, characterized in that: the preparation method of the Pt alloy comprises the following steps:
    dissolving a water-soluble Pt salt and another water-soluble alloy element salt in a polar solvent;
    adding a reducing agent, and reacting to obtain the Pt alloy.
  6. 6. Use according to claim 5, characterized in that:
    the Pt alloy is a Pt-Ir alloy, and the preparation method comprises the following steps:
    s1) dissolving a Pt salt and an Ir salt in 1, 2-propylene glycol, and fully carrying out solvothermal reaction at 130-180 ℃ in a pressure container;
    s2) after the solvothermal reaction is finished, cooling, adding a non-polar solution of octane thiol, and fully mixing;
    s3), adding water, uniformly mixing, separating liquid, collecting a non-polar solvent phase, and removing the non-polar solvent to obtain a Pt-Ir alloy;
    the Pt alloy is a Pt-Au alloy, and the preparation method comprises the following steps:
    s1) dripping the Pt salt solution and the Au salt solution into the citric acid solution, and fully and uniformly mixing;
    s2) adding NaBH4Fully and uniformly mixing the solution;
    s3), adding 2-propanol, and fully and uniformly mixing for reaction;
    s4), collecting a solid-phase product after the reaction is finished, washing and drying to obtain a Pt-Au alloy;
    the Pt alloy is a Pt-Ag alloy, and the preparation method comprises the following steps:
    s1) mixing the Pt salt solution, the Ag salt solution, the poly (N-isopropyl acrylamide) water solution and water evenly;
    s2), adding a formaldehyde solution, uniformly dispersing, transferring into a hydrothermal reaction kettle, and reacting at 120-160 ℃;
    s3), collecting a solid-phase product after the reaction is finished, washing and drying to obtain the Pt-Ag alloy.
  7. 7. Use according to claim 6, characterized in that: the Pt salt is selected from H2PtCl6The Ir salt is selected from IrCl3The Au salt is selected from HAuCl4The Ag salt is AgNO3。
  8. 8. Use according to claim 7, characterized in that:
    the preparation method of the Pt-Ir alloy comprises the following steps:
    S1)0.27 mmol IrCl3and 0.25mmol of PtCl2Dissolving in 100mL of 1, 2-propylene glycol, reacting at 165 ℃ for 15min, and vigorously stirring until the solution becomes dark brown to obtain a colloidal solution;
    s2) cooling the colloidal solution to room temperature, adding a mixed solution of 20mL of toluene and 0.3g of octane thiol, and stirring overnight;
    s3), adding 20mL of deionized water, separating liquid, collecting a toluene phase, and distilling under reduced pressure to obtain a product;
    the preparation method of the Pt-Au alloy comprises the following steps:
    s1)1.5mL of 0.1 mM sodium citrate solution was dissolved in 400mL of water, vigorously stirred for 10min, and 1mL of 9.1mg Pt/mL H was added dropwise2PtCl6And 0.25mL4.46 mg Au/mL HAuCl4Stirring the solution vigorously for 10 min;
    s2) adding fresh NaBH in one portion4Solution, stirring vigorously for 5min, the NaBH4The solution was composed of 22.5mg NaBH4Dissolved in a solution of 3.5mL of water and 1.5mL of 0.1M sodium citrate;
    s3) adding 10mL of 2-propanol, and stirring for 4 h;
    s4), centrifugally collecting a product, washing the product by using deionized water until no chloride ion exists, and drying the product to obtain a Pt-Au alloy;
    the preparation method of the Pt-Ag alloy comprises the following steps:
    S1)0.21 mL50 mM AgNO3aqueous solution, 1.25mL50 mM H2PtCl6The solution, 5.0mL of 50 mM Mw =2500 poly (N-isopropylacrylamide) solution was mixed well with 35 mL;
    s2), dropwise adding 2.5mL of 40 wt.% formaldehyde solution, performing ultrasonic treatment for 5min, transferring the solution into a 100mL hydrothermal reaction kettle, sealing, and keeping the temperature at 140 ℃ for 6 hours;
    s3), cooling to room temperature after the reaction is finished, centrifugally collecting the product, washing for 3 times by deionized water and acetone, and drying to obtain the Pt-Ag alloy.
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