CN109888317B - Direct methanol fuel cell catalyst and preparation method thereof - Google Patents
Direct methanol fuel cell catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention provides a direct methanol fuel cell catalyst and a preparation method thereof, the catalyst is activated carbon loaded with platinum and indium, wherein the BET surface area of an activated carbon carrier is 800-1000m2The load rate on the active carbon carrier is 1.8-4.2 wt%, the mass ratio of the loaded platinum to the loaded indium is 1.3-2.8:1, the invention adopts platinum and indium as main catalytic noble metals, takes active carbon particles as the carrier, and effectively improves the load rate and adhesiveness of the catalytic active ingredients by reasonably regulating and controlling the types, addition ratio and process parameters of the noble metals, the structural function stability is good, and the comprehensive catalytic efficiency is obviously improved.
Description
Technical Field
The invention relates to the technical field of methanol fuel cells, in particular to a direct methanol fuel cell catalyst and a preparation method thereof.
Background
The fuel cell is used as an efficient and environment-friendly power generation device, and has wide application prospect in the aspects of base station power supplies, medium and small power stations, electric vehicles, standby power supplies, portable power supplies and the like. Fuel cells can be classified into proton exchange membrane fuel cells, direct methanol fuel cells, alkaline fuel cells, solid oxide fuel cells, molten salt fuel cells, microbial fuel cells, biofuel cells, and the like.
A Direct Methanol Fuel Cell (DMFC) is a power generation device that uses methanol as a fuel, and converts chemical energy stored in the fuel into electric energy under the action of an electrocatalyst to work externally. The device has the advantages of high theoretical specific energy density, compact structure, simple system and large miniaturization potential; rich fuel source, low cost, environment friendship, etc. Compared with the hydrogen-oxygen fuel cell, the direct alcohol fuel cell has no safety problem in hydrogen storage and transportation, and can more effectively realize the miniaturization design and application of the fuel cell. Therefore, the DMFC is a preferred portable power supply for powering micro electronic devices, and has a wide commercial prospect.
The fuel cell mainly comprises an end plate, a collector plate, a bipolar plate, a membrane electrode and the like, wherein the membrane electrode is a core component of the fuel cell, and a catalyst is a heart part of the membrane electrode. At present, the mature catalyst mainly uses carbon powder as a carrier to load metal platinum, but the carbon powder is used as the carrier and has the following defects:
(1) the adhesion force of the metal platinum particles and the carbon carrier is reduced along with the use of the battery, and finally the catalyst agglomeration phenomenon is caused, so that the service life of the membrane electrode is reduced;
(2) the electrochemical corrosion resistance of the carbon carrier is weaker along with the use of the battery, and finally, the carbon carrier is corroded electrochemically to cause the collapse of the catalyst layer, so that the performance of the membrane electrode is reduced;
(3) the surface area of the carbon carrier is small, so that the rate of gas-liquid-solid reactions is influenced, the contact surface of platinum atoms of the catalyst and hydrogen is reduced, the catalytic efficiency of metal platinum cannot be improved, and the waste of noble metal platinum is caused to a certain extent;
(4) because the efficiency of the catalyst is low, in order to achieve the required power density, the dosage of the catalyst is increased, the thickness of the catalyst layer is further increased, the internal resistance of the membrane electrode is increased, the performance of the membrane electrode is reduced, and the output power of the galvanic pile is reduced.
Therefore, in order to meet the evolving performance requirements of fuel cells, further development of highly efficient and highly stable catalysts is required.
Disclosure of Invention
Aiming at the problems, the invention provides a direct methanol fuel cell catalyst and a preparation method thereof, which adopts platinum and indium as main catalytic precious metals, takes activated carbon particles as a carrier, and effectively improves the loading rate and the adhesiveness of catalytic active ingredients by reasonably regulating and controlling the types, the addition proportion and the process parameters of the catalytic metals, and has good structural function stability and remarkably improved comprehensive catalytic efficiency.
In order to achieve the above object, the present invention adopts the following technical solutions:
a direct methanol fuel cell catalyst is active carbon loaded by platinum and indium, wherein the BET surface area of the active carbon carrier is 800-1000m2The load rate on the active carbon carrier is 1.8-4.2 wt%, and the mass ratio of the loaded platinum to the loaded indium is 1.3-2.8: 1.
Preferably, the platinum and the indium are selected from platinum-indium alloy, and the platinum-indium alloy further contains 0-5 wt% of La and Sr, and the molar ratio of the La to the Sr is 1-3: 1.
Preferably, the direct methanol fuel cell catalyst is prepared by the following steps: sputtering an alloy metal layer on the active carbon carrier by adopting vacuum magnetron sputtering and taking platinum-indium alloy as a target material; then drying for 20-60min at the temperature of 150-; taking out, grinding into particles loaded with carbon by ball milling, then sending into a carbonization furnace, and carrying out carbonization treatment for 20-60min at the high temperature of 800-1000 ℃ under inert atmosphere to obtain the carbon-loaded carbon particles.
Preferably, the thickness of the alloy metal layer is 2-4nm, and the inert atmosphere is argon or nitrogen.
Preferably, the supported carbon particles have a particle size of 4 to 5 μm and a BET surface area of 1200-1700m2And/g, the inert atmosphere is argon or nitrogen.
Preferably, the preparation method of the platinum-indium alloy target material comprises the following steps: taking platinum-indium alloy, crushing and ball-milling the platinum-indium alloy to be nano-scale, then adding the platinum-indium alloy into nano-silica aqueous solution for blending, carrying out normal-temperature ultrasonic treatment for 5-15min, filtering and drying the mixture, adding the mixture into PTFE emulsion, stirring and mixing the mixture at 80-120 ℃ to prepare slurry, then sending the slurry into a mold for extrusion forming to obtain a block product, heating the block product at the temperature of 650-800 ℃ for 10-15min under inert atmosphere, then heating the block product at the temperature of 1000-1200 ℃ for 10-30min, taking out the block product and cooling the block product to obtain the platinum-indium alloy.
Preferably, the platinum-indium alloy is ball-milled to 8-10nm, and the mass ratio of the platinum-indium alloy to the nano silicon dioxide aqueous solution to the PTFE emulsion is 1: 8-12: 4-7.
Preferably, the specification of the block product is 4X 8X 1 cm-5X 10X 2cm, and the inert atmosphere is argon or nitrogen.
Due to the adoption of the technical scheme, the invention has the beneficial effects that: according to the invention, platinum and indium are used as main catalytic precious metals, activated carbon particles are used as carriers, the types, addition ratios and process parameters of the precious metals are reasonably regulated, the loading rate and adhesiveness of catalytic active ingredients are effectively improved, the structural function stability is good, and the comprehensive catalytic efficiency is remarkably improved.
In the preparation process of the platinum-indium alloy target material, the platinum-indium alloy is sequentially mixed with silicon dioxideThe blending treatment of PTFE emulsion, the progressive adsorption of platinum and indium elements, the embedding and coating of the platinum and indium elements on silicon dioxide in PTFE, and the two-stage heating sintering effectively ensure the activity of the effective components of platinum and indium, and effectively improve the BET specific surface area (A)>500m2(g), has a good effect of promoting adsorption and adhesion of the activated carbon carrier. In the preparation process of the catalyst, technological parameters and carrier particle size are reasonably regulated and controlled, the target material receiving binding degree is high, the load uniformity and the binding force are obviously improved, the content of effective components of the catalyst is greatly improved, the effective service life is long, the comprehensive contact reaction specific surface area is high, and the catalytic efficiency is obviously improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Example 1:
a direct methanol fuel cell catalyst is active carbon loaded by platinum and indium, wherein the BET surface area of the active carbon carrier is 800-2The loading rate on the activated carbon carrier is 3.6 wt%, and the mass ratio of the loaded platinum to the loaded indium is 1.7: 1.
The preparation method of the direct methanol fuel cell catalyst comprises the following steps: sputtering an alloy metal layer on the active carbon carrier by adopting vacuum magnetron sputtering and taking platinum-indium alloy as a target material, wherein the thickness is 2-4 nm; then drying at 200 deg.C under inert atmosphere (argon or nitrogen, the same below) for 30 min; taking out, grinding into load carbon particles with particle size of 4-5 μm and BET surface area of 1200-1700m2And/g, then sending the mixture into a carbonization furnace, and carbonizing the mixture for 50min at the high temperature of 1000 ℃ under the inert atmosphere to obtain the carbon fiber.
The preparation method of the platinum-indium alloy target material comprises the following steps: taking platinum-indium alloy, crushing and ball-milling the platinum-indium alloy to a nano level (8-10nm), adding the platinum-indium alloy into a nano silicon dioxide aqueous solution for blending, carrying out normal temperature ultrasonic treatment (20 ℃, 25-28KHz) for 5-15min, filtering, drying, adding the obtained product into PTFE emulsion, stirring and mixing the obtained product at 100 ℃ to prepare slurry, then sending the slurry into a die for extrusion forming to obtain a blocky product (the specification is 4 multiplied by 8 multiplied by 1cm-5 multiplied by 10 multiplied by 2cm), heating the blocky product at 650 ℃ for 15min under an inert atmosphere, then heating the blocky product to 1200 ℃ for 30min, taking out and cooling the blocky product to obtain the platinum-indium alloy. Wherein: the mass ratio of the platinum-indium alloy to the nano silicon dioxide aqueous solution to the PTFE emulsion is 1: 10: 5.
example 2:
a direct methanol fuel cell catalyst is active carbon loaded by platinum and indium, wherein the BET surface area of the active carbon carrier is 800-2The loading rate on the activated carbon carrier is 2.2 wt%, and the mass ratio of the loaded platinum to the loaded indium is 2.1: 1.
The platinum and the indium are selected from platinum-indium alloy, and the platinum-indium alloy also contains 3 wt% of La and Sr, and the molar ratio of the La to the Sr is 3: 1.
The preparation method of the direct methanol fuel cell catalyst comprises the following steps: sputtering an alloy metal layer on the active carbon carrier by adopting vacuum magnetron sputtering and taking platinum-indium alloy as a target material, wherein the thickness is 2-4 nm; then drying at 200 deg.C under inert atmosphere (argon or nitrogen, the same below) for 20 min; taking out, grinding into load carbon particles with particle size of 4-5 μm and BET surface area of 1200-1700m2And/g, then sending the mixture into a carbonization furnace, and carbonizing the mixture for 30min at the high temperature of 1000 ℃ under the inert atmosphere to obtain the carbon fiber.
The preparation method of the platinum-indium alloy target comprises the following steps: taking platinum-indium alloy, crushing and ball-milling the platinum-indium alloy to a nano level (8-10nm), adding the platinum-indium alloy into a nano silicon dioxide aqueous solution for blending, carrying out ultrasonic treatment at normal temperature for 5-15min, filtering, drying, adding the platinum-indium alloy into PTFE emulsion, stirring and mixing at 120 ℃ to prepare slurry, then sending the slurry into a die for extrusion forming to obtain a block product (the specification is 4 multiplied by 8 multiplied by 1cm-5 multiplied by 10 multiplied by 2cm), heating the block product at 800 ℃ for 15min under an inert atmosphere, then heating to 1200 ℃ for 10min, taking out, and cooling to obtain the platinum-indium alloy. Wherein: the mass ratio of the platinum-indium alloy to the nano silicon dioxide aqueous solution to the PTFE emulsion is 1: 10: 4.
example 3:
a direct methanol fuel cell catalyst is active carbon loaded by platinum and indium, wherein the BET surface area of the active carbon carrier is 800-2The loading rate on the activated carbon carrier is 4.2 wt%, and the mass ratio of the loaded platinum to the loaded indium is 2.6: 1.
The platinum and the indium are selected from platinum-indium alloy, 5 wt% of La and Sr are further contained in the platinum-indium alloy, and the molar ratio of the La to the Sr is 1: 1.
The preparation method of the direct methanol fuel cell catalyst comprises the following steps: sputtering an alloy metal layer on the active carbon carrier by adopting vacuum magnetron sputtering and taking platinum-indium alloy as a target material, wherein the thickness is 2-4 nm; then drying at 150 deg.C under inert atmosphere (argon or nitrogen, the same below) for 60 min; taking out, grinding into load carbon particles by ball milling, wherein the particle size is 4-5 mu m, the BET surface area is 1200-1700m2And/g, then sending the mixture into a carbonization furnace, and carbonizing the mixture at a high temperature of 800 ℃ for 60min under an inert atmosphere to obtain the carbon fiber.
The preparation method of the platinum-indium alloy target material comprises the following steps: taking platinum-indium alloy, crushing and ball-milling the platinum-indium alloy to a nano level (8-10nm), adding the platinum-indium alloy into a nano silicon dioxide aqueous solution for blending, carrying out ultrasonic treatment at normal temperature for 5-15min, filtering, drying, adding the platinum-indium alloy into PTFE emulsion, stirring and mixing the mixture at 80 ℃ to prepare slurry, then sending the slurry into a die for extrusion forming to obtain a blocky product (the specification is 4 multiplied by 8 multiplied by 1cm-5 multiplied by 10 multiplied by 2cm), heating the blocky product at 700 ℃ for 15min under an inert atmosphere, then heating the blocky product to 1000 ℃ for 30min, taking out the blocky product, and cooling the blocky product to obtain the platinum-indium alloy. Wherein: the mass ratio of the platinum-indium alloy to the nano silicon dioxide aqueous solution to the PTFE emulsion is 1: 12: 5.
example 4:
a direct methanol fuel cell catalyst is active carbon loaded by platinum and indium, wherein the BET surface area of the active carbon carrier is 800-2The loading rate on the activated carbon carrier is 3.5 wt%, and the mass ratio of the loaded platinum to the loaded indium is 1.3: 1.
The platinum and the indium are selected from platinum-indium alloy, and the platinum-indium alloy also contains 4 wt% of La and Sr, and the molar ratio of the La to the Sr is 2: 1.
Direct methanol fuel cell catalyst and preparation method thereofThe method comprises the following steps: sputtering an alloy metal layer on the active carbon carrier by adopting vacuum magnetron sputtering and taking platinum-indium alloy as a target material, wherein the thickness is 2-4 nm; then drying at 200 deg.C under inert atmosphere (argon or nitrogen, the same below) for 20 min; taking out, grinding into load carbon particles with particle size of 4-5 μm and BET surface area of 1200-1700m2And/g, then sending the mixture into a carbonization furnace, and carbonizing the mixture at the high temperature of 900 ℃ for 60min under the inert atmosphere to obtain the carbon fiber.
The preparation method of the platinum-indium alloy target material comprises the following steps: taking platinum-indium alloy, crushing and ball-milling the platinum-indium alloy to a nano level (8-10nm), adding the platinum-indium alloy into a nano silicon dioxide aqueous solution for blending, carrying out ultrasonic treatment at normal temperature for 5-15min, filtering, drying, adding the platinum-indium alloy into PTFE emulsion, stirring and mixing the mixture at 80 ℃ to prepare slurry, then sending the slurry into a mould for extrusion forming to obtain a block product (the specification is 4 multiplied by 8 multiplied by 1cm-5 multiplied by 10 multiplied by 2cm), heating the block product at 800 ℃ for 15min under an inert atmosphere, then heating the block product to 1100 ℃ for 30min, taking out the block product, and cooling the block product to obtain the platinum-indium alloy. Wherein: the mass ratio of the platinum-indium alloy to the nano silicon dioxide aqueous solution to the PTFE emulsion is 1: 8: 4.
example 5:
a direct methanol fuel cell catalyst is active carbon loaded by platinum and indium, wherein the BET surface area of the active carbon carrier is 800-2The loading rate on the activated carbon carrier is 2.8 wt%, and the mass ratio of the loaded platinum to the loaded indium is 2.2: 1.
The preparation method of the direct methanol fuel cell catalyst comprises the following steps: sputtering an alloy metal layer on the active carbon carrier by adopting vacuum magnetron sputtering and taking platinum-indium alloy as a target material, wherein the thickness is 2-4 nm; then drying at 200 deg.C under inert atmosphere (argon or nitrogen, the same below) for 40 min; taking out, grinding into load carbon particles with particle size of 4-5 μm and BET surface area of 1200-1700m2And/g, then sending the mixture into a carbonization furnace, and carbonizing the mixture at a high temperature of 800 ℃ for 40min under an inert atmosphere to obtain the carbon fiber.
The preparation method of the platinum-indium alloy target material comprises the following steps: taking platinum-indium alloy, crushing and ball-milling the platinum-indium alloy to a nano level (8-10nm), adding the platinum-indium alloy into a nano silicon dioxide aqueous solution for blending, carrying out ultrasonic treatment at normal temperature for 5-15min, filtering, drying, adding the platinum-indium alloy into PTFE emulsion, stirring and mixing the mixture at 100 ℃ to prepare slurry, then sending the slurry into a die for extrusion forming to obtain a block product (the specification is 4 multiplied by 8 multiplied by 1cm-5 multiplied by 10 multiplied by 2cm), heating the block product for 15min at 650 ℃ in an inert atmosphere, then heating the block product for 30min at 1000 ℃, taking out the block product and cooling the block product to obtain the platinum-indium alloy. Wherein: the mass ratio of the platinum-indium alloy to the nano silicon dioxide aqueous solution to the PTFE emulsion is 1: 10: 7.
example 6:
a direct methanol fuel cell catalyst is active carbon loaded by platinum and indium, wherein the BET surface area of the active carbon carrier is 800-2The loading rate on the activated carbon carrier is 2.0 wt%, and the mass ratio of the loaded platinum to the loaded indium is 2.5: 1.
The platinum and the indium are selected from platinum-indium alloy, and the platinum-indium alloy also contains 3 wt% of La and Sr, and the molar ratio of the La to the Sr is 2: 1.
The preparation method of the direct methanol fuel cell catalyst comprises the following steps: sputtering an alloy metal layer on the active carbon carrier by adopting vacuum magnetron sputtering and taking platinum-indium alloy as a target material, wherein the thickness is 2-4 nm; then drying at 200 deg.C under inert atmosphere (argon or nitrogen, the same below) for 20 min; taking out, grinding into load carbon particles with particle size of 4-5 μm and BET surface area of 1200-1700m2And/g, then sending the mixture into a carbonization furnace, and carbonizing the mixture for 20min at the high temperature of 1000 ℃ under the inert atmosphere to obtain the carbon fiber.
The preparation method of the platinum-indium alloy target material comprises the following steps: taking platinum-indium alloy, crushing and ball-milling the platinum-indium alloy to be nano-scale (8-10nm), adding the platinum-indium alloy into a nano-silica aqueous solution for blending, carrying out ultrasonic treatment at normal temperature for 5-15min, filtering, drying, adding the platinum-indium alloy into PTFE emulsion, stirring and mixing at 100 ℃ to prepare slurry, then sending the slurry into a die for extrusion forming to obtain a block product (the specification is 4 multiplied by 8 multiplied by 1cm-5 multiplied by 10 multiplied by 2cm), heating the block product at 700 ℃ for 10min under an inert atmosphere, then heating to 1100 ℃ for 10min, taking out, and cooling to obtain the platinum-indium alloy. Wherein: the mass ratio of the platinum-indium alloy, the nano silicon dioxide aqueous solution and the PTFE emulsion is 1: 10: 6.
the performance of the catalyst prepared by the invention is compared with the performance of the commercial PtC catalyst and the commercial CoMoC catalyst, and the data is as follows:
the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (4)
1. A direct methanol fuel cell catalyst, characterized by: the catalyst is activated carbon loaded with platinum and indium, wherein the BET surface area of an activated carbon carrier is 800-2The load rate on the active carbon carrier is 1.8-4.2 wt%, and the mass ratio of the loaded platinum to the loaded indium is 1.3-2.8: 1;
the preparation method of the catalyst comprises the following steps: sputtering an alloy metal layer on the active carbon carrier by adopting vacuum magnetron sputtering and taking platinum-indium alloy as a target material; then drying for 20-60min at the temperature of 150-200 ℃ and under the inert atmosphere; taking out, grinding into particles loaded with carbon by ball milling, and then sending into a carbonization furnace for carbonization treatment at the high temperature of 800-1000 ℃ for 20-60min under inert atmosphere to obtain the carbon particles;
the preparation method of the platinum-indium alloy target material comprises the following steps: taking platinum-indium alloy, crushing and ball-milling the platinum-indium alloy to a nanometer level, adding the platinum-indium alloy into a nano silicon dioxide aqueous solution for blending, carrying out ultrasonic treatment at normal temperature for 5-15min, filtering, drying, adding the platinum-indium alloy into PTFE emulsion, stirring and mixing at 80-120 ℃ to prepare slurry, then sending the slurry into a mold for extrusion molding to obtain a blocky product, heating the blocky product for 10-15min at the temperature of 650-800 ℃ in an inert atmosphere, then heating the blocky product for 10-30min at the temperature of 1000-1200 ℃, taking out and cooling to obtain the platinum-indium alloy;
the thickness of the alloy metal layer is 2-4nm, and the inert atmosphere is argon or nitrogen;
the particle diameter of the loaded carbon particle is 4-5 μm, and the BET surface area is 1200-1700m2And/g, the inert atmosphere is argon or nitrogen.
2. The direct methanol fuel cell catalyst as claimed in claim 1, wherein: the platinum and the indium are selected from platinum-indium alloy, and the platinum-indium alloy also contains 0-5 wt% of La and Sr, and the molar ratio of the La to the Sr is 1-3: 1.
3. The direct methanol fuel cell catalyst as claimed in claim 1, wherein: the platinum-indium alloy is ball-milled to 8-10nm, and the mass ratio of the platinum-indium alloy to the nano silicon dioxide aqueous solution to the PTFE emulsion is 1: 8-12: 4-7.
4. The direct methanol fuel cell catalyst as claimed in claim 1, wherein: the specification of the block product is 4 multiplied by 8 multiplied by 1cm-5 multiplied by 10 multiplied by 2cm, and the inert atmosphere is argon or nitrogen.
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