CN112980247A - High-stability ink-jet printing ink for fuel cell and preparation and application thereof - Google Patents
High-stability ink-jet printing ink for fuel cell and preparation and application thereof Download PDFInfo
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- CN112980247A CN112980247A CN201911287550.5A CN201911287550A CN112980247A CN 112980247 A CN112980247 A CN 112980247A CN 201911287550 A CN201911287550 A CN 201911287550A CN 112980247 A CN112980247 A CN 112980247A
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- ink
- jet printing
- catalyst
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- chelating agent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention provides high-stability ink-jet printing ink for a fuel cell and preparation and application thereof. The ink-jet printing ink consists of a catalyst, a solvent, an adhesive, a chelating agent and a resin solution, wherein the mass ratio of the catalyst to the solvent to the adhesive to the chelating agent to the resin solution is 1:15-1:40,1:10-1:30,1:10-1:20 and 1:1.8-1:12.6 respectively; the catalyst is a platinum-based catalyst; the solvent is one or more of isopropanol, ethanol or water; the adhesive is one or two of ethylene glycol or glycerol; the chelating agent is butyl acetate; the mass fraction of the resin solution is 1-10%; compared with the prior art, the ink-jet printing ink for the fuel cell has high stability, is simple in preparation method and is convenient for realizing industrialization; the membrane electrode prepared by printing the ink on a proton exchange membrane through ink jet is soaked and dried by deionized water, so that the battery performance is good and is superior to that of the traditional ink without the chelating agent.
Description
Technical Field
The invention belongs to the field of fuel cells, and particularly relates to high-stability ink-jet printing ink as well as preparation and application thereof.
Background
The proton exchange membrane fuel cell has the characteristics of environmental friendliness, high energy conversion rate, low-temperature quick start and the like, and has a very wide development prospect in the fields of transportation, portable power supplies and aerospace. However, how to perform mass production of fuel cells and increase the power density of fuel cells are key issues that restrict further development of fuel cells.
The ink-jet printing technology, as one of the current popular preparation technologies, has the advantages of wide application range, simple operation, low cost, capability of realizing rapid batch preparation and the like. At present, the technology can be conveniently applied to the fields of wide process preparation and scientific research such as solar cells, Organic Light Emitting Diodes (OLEDs), high-molecular light emitting diodes, functional material printers, printing electronics and the like, and has great development potential in the field of fuel cell preparation. The introduction of ink-jet printing technology into the membrane electrode preparation field has many advantages: firstly, the content of a noble metal catalyst in a catalytic layer and the thickness of the catalytic layer can be well controlled by the ink-jet printing technology, so that the preparation of the low-platinum, ultra-low platinum-loading and ultra-thin catalytic layer is convenient, and compared with other preparation technologies, the flatness of the catalytic layer is higher; secondly, the ink-jet printing technology can realize synchronous high-precision printing of various materials, and the establishment of functional structures such as a gas channel, a water drainage channel and the like in a catalytic layer can be realized through the technology, so that the gas mass transfer is promoted, the flooding phenomenon is slowed down, the consumption of a noble metal catalyst is reduced, and a functionally-ordered electrode is prepared; and thirdly, the ink-jet printing technology has very wide application prospect in the aspect of large-scale mass production of the membrane electrode, can realize the rapid and large-scale continuous preparation of the membrane electrode, synchronously complete the membrane electrode sealing step, simplify the process flow and improve the production efficiency.
However, the application of ink-jet printing technology in the field of fuel cell preparation has many difficulties, especially in the preparation of high-stability ink-jet printing ink. Due to the characteristics of the fuel cell electrode, the traditional ink required by the current electrode prepared by ink-jet printing only contains a catalyst, an adhesive, a solvent and a resin solution, the obtained traditional ink is a suspension, a dispersion system is unstable, the particle size of the catalyst is large, and the problems of ink sedimentation, nozzle blockage and the like are easily caused. Therefore, improving the stability of the ink-jet printing ink for the fuel cell is crucial to the application of the ink-jet printing technology in the field of fuel cell preparation, and is a key to solving the problem of mass production of the fuel cell.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides high-stability ink-jet printing ink for a fuel cell, and preparation and application thereof. Compared with the prior art, the ink-jet printing ink for the fuel cell has high stability, does not have the phenomenon of sedimentation after standing for 24 hours at room temperature, has simple preparation method and is convenient to realize industrialization; the membrane electrode prepared by printing the ink on a proton exchange membrane through ink jet is soaked and dried by deionized water, so that the battery performance is good and is superior to that of the traditional ink without the chelating agent.
The technical scheme of the invention is as follows:
in a first aspect, the present invention provides an ink-jet printing ink for a fuel cell, the ink consisting of a catalyst, a solvent, a binder, a chelating agent, and a resin solution;
the mass ratio of the catalyst to the solvent, the adhesive, the chelating agent and the resin solution is 1:15-1:40,1:10-1:30,1:10-1:20 and 1:1.8-1:12.6 respectively;
the catalyst is a platinum-based catalyst; the solvent is one or more of isopropanol, ethanol or water; the adhesive is one or two of ethylene glycol or glycerol; the chelating agent is butyl acetate; the mass fraction of the resin solution is 1-10%.
Preferably, the platinum-based catalyst is one or more of platinum black, carbon-supported platinum, a platinum alloy, a core-shell structure platinum-based catalyst, a nanowire structure platinum-based catalyst or a monoatomic layer platinum-based catalyst; the resin is perfluorosulfonic acid resin.
In a second aspect, the present invention provides a method for preparing an ink for inkjet printing, the method comprising:
weighing the catalyst, the solvent, the adhesive, the chelating agent and the resin solution according to the mass ratio;
mixing a catalyst, an adhesive and a solvent, performing water bath ultrasound at 0-25 ℃ for 0.5-3h, and dropwise adding a resin solution in the water bath ultrasound process to obtain a mixed solution;
and after the water bath ultrasound is finished, adding the mixed solution into a chelating agent in the water bath ultrasound at the speed of 1-2ml/min, continuing the water bath ultrasound for 10-30min, and then performing probe ultrasound for 15-60min under an ice water bath to obtain the high-stability ink-jet printing ink.
Preferably, the power of the probe ultrasound is 10% -50% of the rated power, and the rated power is 200-400W.
The high-stability ink-jet printing ink does not generate a sedimentation phenomenon after standing for 24 hours under room temperature natural light; the viscosity is 1-50 mPas, and the surface tension is 50-150 mN/m.
In a third aspect, the present invention provides a membrane electrode prepared from the above ink-jet printing ink by an ink-jet printing method.
In a fourth aspect, the present invention provides a method for preparing a membrane electrode, the method comprising: and ink-jet printing the ink-jet printing ink on one side or both sides of a proton exchange membrane, soaking the proton exchange membrane in deionized water at 0-25 ℃ for 0.5-5h, heating the proton exchange membrane in air to 60-100 ℃, and carrying out heat treatment for 1-5h to obtain the membrane electrode.
In a fifth aspect, the invention provides the use of a membrane electrode in the field of fuel cells.
Advantageous effects
1. The chelating agent is introduced into the composition of the ink-jet printing ink for the fuel cell for the first time, so that the state of the ink is adjusted from a suspension state to a colloidal state, the addition of the chelating agent has no influence on the activity of a catalyst, the stability of the ink-jet printing ink is improved, and the ink-jet printing ink does not generate a sedimentation phenomenon after standing for 24 hours at room temperature, but generates sedimentation after standing for more than 5 hours.
2. The high-stability ink-jet printing ink for the fuel cell, prepared by the invention, has the viscosity of 1-50mPa & s and the surface tension of 50-150mN/m, is wide and adjustable in viscosity and surface tension range and wide in application range, and is suitable for various ink-jet printing nozzles and ink-jet printing modes.
3. The membrane electrode prepared by the high-stability ink-jet printing ink for the fuel cell provided by the invention has good performance, and is superior to the membrane electrode prepared by the traditional ink-jet printing without adding a chelating agent.
4. In traditional ink, the active component accounts for the mass ratio of carrier and is not higher than 20% usually in the catalyst, otherwise can lead to the catalyst granule bigger, deposit more easily, this application has improved the stability of ink-jet printing ink through introducing the chelating agent, in the ink-jet printing ink that this application provided, the active component accounts for the mass ratio of carrier can reach 70% in the catalyst, and 24h does not have the settlement phenomenon and produces.
Drawings
Fig. 1 is a graph showing a comparison of the ink states of the high-stability ink-jet printing ink for a fuel cell of example 1 of the present invention (left side, 1) and the conventional ink-jet printing ink for a fuel cell of comparative example 1 (right side, 2) after being left standing at room temperature for 24 hours.
Fig. 2 is a graph comparing polarization curves of membrane electrodes prepared from the high stability ink-jet printing ink for fuel cells of example 1 of the present invention and the conventional ink-jet printing ink for fuel cells.
Detailed Description
The catalyst, solvent, binder, chelating agent and resin solution used in the examples of the present invention are all commercially available products.
Comparative example 1
A conventional ink jet printing ink for a fuel cell, said ink comprising: according to the mass ratio of 20 wt% of catalyst Pt/C62.5 mg to solvent isopropanol, adhesive glycerol and resin solution 5% of perfluorinated sulfonic acid resin (Nafion) solution, respectively, 1:25,1:13.67 and 1: 7.
The preparation method of the ink comprises the following steps:
dissolving 20 wt% of Pt/C in isopropanol according to the proportion, adding glycerol, carrying out water bath ultrasonic treatment for 30min at 5 ℃, dropwise adding 5% of Nafion solution in the water bath ultrasonic process, carrying out probe ultrasonic treatment for 30min under the condition that the power is 50%, wherein the rated power of a probe ultrasonic instrument is 300W, and obtaining the traditional ink-jet printing ink for the fuel cell of the comparative example, wherein the viscosity is 8.7mPa & s, and the surface tension is 90 mN/m.
Printing the high-stability ink-jet printing ink for the fuel cell of the comparative example on one side of a Nafion-211 membrane, soaking the printed electrode in deionized water for 5 hours at 25 ℃, then heating the electrode to 80 ℃ in air, and carrying out heat treatment for 3 hours to prepare a membrane electrode of the fuel cell, wherein the membrane electrode is used as a cathode, and the platinum loading capacity of the cathode is 0.05mg cm-2The anode is prepared by a spraying method, and the platinum loading capacity is 0.2mg cm-2. The testing conditions of the membrane electrode are as follows: the effective area of the battery is 5cm2The testing temperature is 60 ℃, the humidification is 100 percent, the cathode and anode reaction gases are oxygen and hydrogen, and the gas pressure of the cathode and anode of the battery is 0.5 bar.
Example 1
A high stability ink jet printing ink for fuel cells, said ink comprising: according to the mass ratio of 50 wt% of catalyst Pt/C25 mg to solvent isopropanol, adhesive glycerol, chelating agent butyl acetate and resin solution 5% Nafion solution, respectively, 1:25,1:13.67,1:11.79 and 1: 7.
The preparation method of the ink comprises the following steps:
dissolving 50 wt% of Pt/C in isopropanol according to the proportion, adding glycerol, performing water bath ultrasonic treatment at 5 ℃ for 30min, and dropwise adding a 5% Nafion solution in the water bath ultrasonic process; slowly adding the mixed solution obtained in the above process into butyl acetate in a water bath ultrasonic state at the speed of 1.5ml/min, performing water bath ultrasonic treatment for 10min, uniformly mixing, performing probe ultrasonic treatment for 30min under the condition that the power is 40% and the rated power of a probe ultrasonic instrument is 300W to obtain the high-stability ink-jet printing ink for the fuel cell, wherein the viscosity of the ink-jet printing ink is 9.96mPa & s, and the surface tension of the ink-jet printing ink is 98 mN/m.
Printing the high-stability ink-jet printing ink for the fuel cell on one side of a Nafion-211 membrane, soaking the printed electrode in deionized water at 25 ℃ for 5 hours, heating the electrode in air to 80 ℃, and carrying out heat treatment for 3 hours to prepare a membrane electrode of the fuel cell, wherein the membrane electrode is used as a cathode, the platinum loading capacity of the cathode is 0.05mg cm-2The anode is prepared by a spraying method, and the platinum loading capacity is 0.2mg cm-2. The testing conditions of the membrane electrode are as follows: the effective area of the battery is 5cm2The testing temperature is 60 ℃, the humidification is 100 percent, the cathode and anode reaction gases are oxygen and hydrogen, and the gas pressure of the cathode and anode of the battery is 0.5 bar.
The polarization curve of the membrane electrode thus obtained is shown in FIG. 2. From FIG. 2, the maximum working current density of the membrane electrode prepared by the conventional ink under the same test conditions is 3A cm-2The maximum power density is 1.028 W.cm-2(ii) a The maximum working current density of the membrane electrode prepared by the high-stability ink can reach 3.2A cm-2The highest power density can reach 1.305W cm-2And the performance of the membrane electrode prepared by the high-stability ink is superior to that of the membrane electrode prepared by the traditional ink.
The high stability ink-jet printing ink for fuel cell of example 1 (left side, 1) and the conventional ink-jet printing ink for fuel cell of comparative example 1 (right side, 2) were left to stand at room temperature for 24 hours, and then the ink states were compared, as shown in fig. 1. After standing for 24 hours, the traditional ink-jet printing ink has obvious sedimentation phenomenon, the high-stability ink does not sediment, the catalyst used in the high-stability ink is 50 wt% Pt/C, and compared with the catalyst used in the traditional ink which is 20 wt% Pt/C, the catalyst has larger particles and is easier to sediment, so that in the high-stability ink, the addition of the chelating agent is not only beneficial to the improvement of the stability of the ink, but also is beneficial to the expansion of the use ratio of active components in the catalyst.
Example 2
A high stability ink jet printing ink for fuel cells, said ink comprising: the mass ratios of 20 wt% of catalyst Pt/C to isopropanol, adhesive glycerol, chelating agent butyl acetate and 5% of resin solution Nafion solution are 1:30,1:19.78,1:15 and 1:7 respectively.
The preparation method of the ink comprises the following steps:
dissolving 20 wt% of Pt/C in isopropanol according to the proportion, adding glycerol, performing water bath ultrasonic treatment at 5 ℃ for 30min, and dropwise adding a 5% Nafion solution in the water bath ultrasonic process; and slowly adding the mixed solution obtained in the process into butyl acetate in a water bath ultrasonic state, performing water bath ultrasonic treatment for 10min, uniformly mixing, performing probe ultrasonic treatment for 15min under the condition that the power is 30% and the rated power of a probe ultrasonic instrument is 300W to obtain the high-stability ink-jet printing ink for the fuel cell, wherein the viscosity of the ink-jet printing ink is 11.6mPa & s, and the surface tension of the ink-jet printing ink is 103 mN/m.
Example 3
A high stability ink jet printing ink for fuel cells, said ink comprising: the mass ratios of 10 wt% of catalyst Pt/C to isopropanol, adhesive glycerol, chelating agent butyl acetate and 5% of resin solution Nafion solution are 1:15,1:10,1:10 and 1:1.8 respectively.
The preparation method of the ink comprises the following steps:
dissolving 10 wt% of Pt/C in isopropanol according to the proportion, adding glycerol, performing water bath ultrasonic treatment at 5 ℃ for 30min, and dropwise adding a 5% Nafion solution in the water bath ultrasonic process; and slowly adding the mixed solution obtained in the process into butyl acetate in a water bath ultrasonic state, carrying out water bath ultrasonic treatment for 10min, uniformly mixing, then carrying out probe ultrasonic treatment for 15min under the condition that the power is 100% and the rated power of a probe ultrasonic instrument is 300W to obtain the high-stability ink-jet printing ink for the fuel cell, wherein the viscosity of the ink-jet printing ink is 10.8mPa & s, and the surface tension of the ink-jet printing ink is 101 mN/m.
Example 4
A high stability ink jet printing ink for fuel cells, said ink comprising: the mass ratios of the catalyst 70 wt% Pt/C to the solvent isopropanol, the adhesive glycerol, the chelating agent butyl acetate and the resin solution 5% Nafion solution are 1:40,1:30,1:20 and 1:12.6 respectively.
The preparation method of the ink comprises the following steps:
dissolving 70 wt% of Pt/C in isopropanol according to the proportion, adding glycerol, performing water bath ultrasonic treatment at 5 ℃ for 30min, and dropwise adding a 5% Nafion solution in the water bath ultrasonic process; and slowly adding the mixed solution obtained in the process into butyl acetate in a water bath ultrasonic state, performing water bath ultrasonic treatment for 30min, uniformly mixing, performing probe ultrasonic treatment for 60min under the condition that the power is 50% and the rated power of a probe ultrasonic instrument is 300W to obtain the high-stability ink-jet printing ink for the fuel cell, wherein the viscosity of the ink-jet printing ink is 12.9mPa & s, and the surface tension of the ink-jet printing ink is 123 mN/m.
Claims (7)
1. An ink-jet printing ink for a fuel cell, characterized in that the ink is composed of a catalyst, a solvent, a binder, a chelating agent, and a resin solution;
the mass ratio of the catalyst to the solvent, the adhesive, the chelating agent and the resin solution is 1:15-1:40,1:10-1:30,1:10-1:20 and 1:1.8-1:12.6 respectively;
the catalyst is a platinum-based catalyst;
the solvent is one or more of isopropanol, ethanol or water;
the adhesive is one or two of ethylene glycol or glycerol;
the chelating agent is butyl acetate;
the mass fraction of the resin solution is 1-10%.
2. The inkjet printing ink of claim 1, wherein the platinum-based catalyst is one or more of platinum black, platinum on carbon, a platinum alloy, a core-shell platinum-based catalyst, a nanowire-structured platinum-based catalyst, or a monoatomic layer platinum-based catalyst; the resin is perfluorosulfonic acid resin.
3. A method of preparing an ink-jet printing ink as defined in claim 1, wherein the method comprises:
weighing the catalyst, the solvent, the adhesive, the chelating agent and the resin solution according to the mass ratio of the catalyst to the solvent to the chelating agent to be weighed in the claim 1;
mixing a catalyst, an adhesive and a solvent, performing water bath ultrasound at 0-25 ℃ for 0.5-3h, and dropwise adding a resin solution in the water bath ultrasound process to obtain a mixed solution;
and after the water bath ultrasound is finished, adding the mixed solution into a chelating agent in the water bath ultrasound at the speed of 1-2ml/min, continuing the water bath ultrasound for 10-30min, and then performing probe ultrasound for 15-60min under an ice water bath to obtain the high-stability ink-jet printing ink.
4. The preparation method according to claim 3, wherein the power of the probe ultrasound is 10% -50% of the rated power, and the rated power is 200-400W.
5. A fuel cell membrane electrode assembly prepared by an ink jet printing process from the ink jet printing ink of claim 1.
6. A preparation method of a fuel cell membrane electrode is characterized by comprising the following steps: the ink-jet printing ink of claim 1 is ink-jet printed on one side or both sides of a proton exchange membrane, soaked in deionized water at 0-25 ℃ for 0.5-5h, then heated to 60-100 ℃ in air, and thermally treated for 1-5h to obtain a membrane electrode.
7. Use of a fuel cell membrane electrode, characterized in that a membrane electrode according to claim 5 is used in the fuel cell field.
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