CN102517602A - Gelatin hole forming method for gas diffusion electrodes - Google Patents
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Abstract
A gelatin hole forming method for gas diffusion electrodes belongs to the field of energy. The gelatin hole forming method includes steps of firstly coating Triton water solution with concentration of 4%, isopropanol, hydrophobic carbon black, 1% to 2% of gelatin water solution and 60% of PTFE (poly tetra fluoro ethylene) emulsion to foaming nickel so as to prepare a diffusion layer; coating 4% of Triton water solution, the isopropanol, 1% to 2% of gelatin water solution, 60% of PTFE emulsion, hydrophilic carbon black and silver/carbon catalyst onto the diffusion layer to form a catalyzing layer; heating gelatin to be carbonized and decomposed to form holes after one-hour heat treatment at the temperature ranging from 200 DEG C to 300 DEG C, and finally forming the electrodes in a hot pressing manner at the temperature of 360 DEG C. Electrode holes formed by the method are uniform in structural distribution and high in hole rate, the average radius of the electrode holes ranges from 20nm to 30nm, the electrodes are stable in structures and performance thereof is improved evidently.
Description
Technical field
The present invention relates to a kind of method of in gas diffusion electrode, carrying out pore-creating, belong to energy field through the gelatin thermolysis.
Background technology
Along with Economic development, energy problem becomes increasingly conspicuous, and the efficient that therefore improves energy utilization is particularly important.Wherein oxygen cathode as a kind of be a kind ofly oxygen to be reduced generate water or electrode hydroxy in the electrode catalyst responding layer with oxygen as the gas diffusion electrode of cathode active material.The cathode for hydrogen evolution that adopts with respect to traditional chloric alkali electrolysis industry is because the hydrogen reduction current potential than hydrogen-evolution overpotential just, if thereby replace traditional hydrogen-precipitating electrode with oxygen cathode then can reduce bath voltage and save electric energy.
At present, in the preparation process of kind electrode,, lack the problem of gas diffusion paths, cause the diffusion process of oxygen in electrode to form certain resistance, thereby make cathodic reaction process oxygen supply not enough, cause polarization of electrode owing to exist void content lower.In order to reduce the diffusional resistance of cathode gas in electrode, can improve the porosity of electrode through the method for adding an amount of pore-forming material in electrode diffusion layer and Catalytic Layer, improve the gas permeation passage.At present the pore-forming material of existing report has ammonium salt class material such as bicarbonate of ammonia, volatile salt, ammonium oxalate, an ammonium nitrate etc., also has small molecules inorganic salt such as Quilonum Retard, sodium-chlor, sodium sulfate etc.But still there is certain defective in above-mentioned pore-forming material in the pore-creating process of electrode; For example the decomposition temperature of ammonium salt is lower; In the early stage of electrode drying course, will most ofly decompose volatilization, can't be in the electrode continued pore-creating of colding pressing, thus cause the porosity of electrode not enough.For general extracting process that adopts heated and boiled zero(ppm) water backflow dissolve inorganic salts such as the difficult inorganic salt that decompose of heating; This method complex process; Length consuming time, and pyritous zero(ppm) water can destroy the internal structure of gas diffusion electrode in extraction process, thus the performance and the life-span of infringement electrode.Therefore seek suitable pore-forming material and pore forming method is most important for the gas diffusion electrode for preparing excellent performance.
Based on above reason, thereby adopt the method counter electrode of gelatin pore-creating to carry out the performance that classification pore-creating improves electrode in the present invention.
Summary of the invention
The present invention is on the basis of existing technology, improves to the defective that exists in the gas diffusion electrode pore-creating process, and a kind of method of carrying out pore-creating through the gelatin thermolysis is provided, thereby effectively improves the pore structure and the electrocatalysis characteristic that improves electrode of electrode.Thermal-decomposing pore-forming method provided by the present invention is in the diffusion layer of gas diffusion electrode and Catalytic Layer, to add the gelatin pore-forming material; Through the pore-creating in the diffusion layer of electrode and Catalytic Layer of pore-creating process, its pore-creating process is to make the gelatin charing be decomposed to form secondary pore structure 200～300 ℃ of following thermal treatments.
The gelatin pore forming method of a kind of gas diffusion electrode provided by the present invention; It is characterized in that; In the diffusion layer of gas diffusion electrode and Catalytic Layer, add the gelatin pore-forming material,, specifically comprise the steps: through the secondary pore-creating in the diffusion layer of electrode and Catalytic Layer of pore-creating process
(1) preparation of diffusion layer: the aqueous gelatin solution that in container, adds earlier the Triton aqueous solution, Virahol, hydrophobic carbon black and the massfraction 1-2% of mass concentration 4% successively; Ultra-sonic dispersion mixes then; Add massfraction then and be 60% PTFE emulsion; Shear to disperse 0.5～1 hour with refiner, form uniform slurry with cell pulverization machine ultra-sonic dispersion again, the gained slurry is coated on the nickel foam to cold pressing after drying by the fire 0.5 hour down at 60～80 ℃ obtains diffusion layer; The Triton aqueous solution wherein: PTFE emulsion: aqueous gelatin solution: the volume ratio of Virahol is 20～45: 2～3: 1～5: 20～70; The volume of the Triton aqueous solution and hydrophobic sooty mass ratio are 20～45mL: 2～4g;
(2) preparation of Catalytic Layer: the aqueous gelatin solution that in container, adds earlier 4% the Triton aqueous solution, Virahol and massfraction 1-2% successively; Ultra-sonic dispersion mixes the three then; Add massfraction then and be 60% PTFE emulsion, hydrophilic fumed silica, silver/Pd/carbon catalyst; Shear dispersion 0.5 hour with refiner, use cell pulverization machine ultra-sonic dispersion again, ultra-sonic dispersion obtains uniform Catalytic Layer slurry; Gained Catalytic Layer slurry is coated onto on step (1) diffusion layer forms Catalytic Layer, put into 60～80 ℃ of baking ovens then and carry out coldmoulding after dry 0.5 hour, form gas diffusion electrode;
Wherein the volume ratio of the Triton aqueous solution, PTFE emulsion, aqueous gelatin solution and Virahol is 10～20: 0.4～0.6: 0.5～2: 20～25, and Triton aqueous solution volume: the quality of hydrophilic fumed silica: the quality of silver/Pd/carbon catalyst is 10～20mL: 1～1.5g: 0.8～1.5g;
(3) thermal treatment and hot pressing: made the charing of being heated of diffusion layer and the gelatin in the Catalytic Layer of gas diffusion electrode decompose pore-creating in 1 hour 200～300 ℃ of following thermal treatments the above-mentioned gas diffusion electrode for preparing, at last that electrode is hot-forming down at 360 ℃.
The quality of the gelatin that in the electrode slurry process for preparation, is added in the step (2) is 1～3% with respect to the sooty quality optimization.
Gelatin pore-creating process is under 15 ℃ of/minute heating rate conditions in the step (3), is warming up to 200～300 ℃, is incubated after 1 hour, and the gelatin charing is decomposed, and electrode is hot-forming under 360 ℃, and air cooling is to room temperature then.
Advantage of the present invention is when adopting gelatin to be pore-forming material; Gelatin can play influence of surfactant in the slurry layoutprocedure; The flowability and the leveling characteristics of slurry have been improved; Help being uniformly dispersed of slurry, and gelatin can persist in the electrode and can not decompose in electrode early stage drying course, electrode in 200～300 ℃ of following heat treatment processes gelatin gradually charing decompose in electrode interior and form the duct.The electrode hole structure distribution that adopts this programme to prepare is even, and porosity is big, and the electrode average pore radius that obtains is at 20～30nm, and electrode structure is stable, and performance is significantly improved.
Description of drawings
The pressure mercury test result of the gas diffusion electrode for preparing among Fig. 1: the embodiment 1;
Fig. 2: gas diffusion electrode of the present invention is the instant potential curve in 30% the NaOH solution at massfraction.
Embodiment
Comparative Examples 1:
Do not add gelatin and prepare process:
(1) preparation of diffusion layer: the Triton aqueous solution, 20mL Virahol, the hydrophobic carbon black of 2g that in beaker, add 20mL mass concentration 4% successively; Ultra-sonic dispersion mixes the three; The PTFE emulsion that adds 2mL 60% then; Shear to disperse 0.5h with refiner, form uniform slurry with cell pulverization machine ultra-sonic dispersion 10min again, the gained slurry is coated on the nickel foam to cold pressing after drying by the fire 0.5 hour down at 60～80 ℃ obtains diffusion layer;
(2) preparation of Catalytic Layer: the Triton aqueous solution, the 20mL Virahol that in container, add earlier 10mL 4% successively; Ultra-sonic dispersion mixes the three; Add 1g hydrophilic fumed silica, 0.8g silver/Pd/carbon catalyst then; 0.4mL massfraction is 60% PTFE emulsion, shears with refiner and disperses 0.5 hour, obtains uniform Catalytic Layer slurry with cell pulverization machine ultra-sonic dispersion again; Gained Catalytic Layer slurry is coated onto on step (1) diffusion layer forms Catalytic Layer, put into 60～80 ℃ of baking ovens then and carry out coldmoulding after dry 0.5 hour, form gas diffusion electrode;
(3) thermal treatment and hot pressing: made the charing of being heated of diffusion layer and the gelatin in the Catalytic Layer of gas diffusion electrode decompose pore-creating in 1 hour 200 ℃ of following thermal treatments the above-mentioned gas diffusion electrode for preparing; At last that electrode is hot-forming under 360 ℃, the electrode average pore radius that obtains is at 19nm.
Embodiment 1:
Add gelatin and prepare process, wherein gelatin and carbon black mass ratio is 1% in the electrode component:
(1) preparation of diffusion layer: the Triton aqueous solution, the aqueous gelatin solution of 1mL massfraction 2%, 20mL Virahol, the hydrophobic carbon black of 2g that in beaker, add 20mL mass concentration 4% successively; Ultra-sonic dispersion mixes the three; The PTFE emulsion that adds 2mL 60% then; Shear to disperse 0.5h with refiner, form uniform slurry with cell pulverization machine ultra-sonic dispersion 10min again, the gained slurry is coated on the nickel foam to cold pressing after drying by the fire 0.5 hour down at 60～80 ℃ obtains diffusion layer;
(2) preparation of Catalytic Layer: in container, add earlier the Triton aqueous solution of 10mL 4%, the aqueous gelatin solution of 0.5mL massfraction 2% successively; The 20mL Virahol; Ultra-sonic dispersion mixes the three; Add 1g hydrophilic fumed silica, 0.8g silver/Pd/carbon catalyst then, the 0.4mL massfraction is that 60% PTFE emulsion is sheared with refiner and disperseed 0.5 hour, obtains uniform Catalytic Layer slurry with cell pulverization machine ultra-sonic dispersion again; Gained Catalytic Layer slurry is coated onto on step (1) diffusion layer forms Catalytic Layer, put into 60～80 ℃ of baking ovens then and carry out coldmoulding after dry 0.5 hour, form gas diffusion electrode;
(3) thermal treatment and hot pressing: made the charing of being heated of diffusion layer and the gelatin in the Catalytic Layer of gas diffusion electrode decompose pore-creating in 1 hour 200 ℃ of following thermal treatments the above-mentioned gas diffusion electrode for preparing; At last that electrode is hot-forming under 360 ℃, the electrode average pore radius that obtains is at 22nm.
Embodiment 2:
Add gelatin and prepare process, wherein gelatin and carbon black mass ratio is 2% in the electrode component:
(1) preparation of diffusion layer: the Triton aqueous solution, the aqueous gelatin solution of 2mL massfraction 1%, 20mL Virahol, the hydrophobic carbon black of 2g that in beaker, add 20mL mass concentration 4% successively; Ultra-sonic dispersion mixes the three; The PTFE emulsion that adds 2mL 60% then; Shear to disperse 0.5h with refiner, form uniform slurry with cell pulverization machine ultra-sonic dispersion 10min again, the gained slurry is coated on the nickel foam to cold pressing after drying by the fire 0.5 hour down at 60～80 ℃ obtains diffusion layer;
(2) preparation of Catalytic Layer: in container, add earlier the Triton aqueous solution of 10mL 4%, the aqueous gelatin solution of 1mL massfraction 1% successively; The 20mL Virahol; Ultra-sonic dispersion mixes the three; Add 1g hydrophilic fumed silica, 0.8g silver/Pd/carbon catalyst then, the 0.4mL massfraction is that 60% PTFE emulsion is sheared with refiner and disperseed 0.5 hour, obtains uniform Catalytic Layer slurry with cell pulverization machine ultra-sonic dispersion again; Gained Catalytic Layer slurry is coated onto on step (1) diffusion layer forms Catalytic Layer, put into 60～80 ℃ of baking ovens then and carry out coldmoulding after dry 0.5 hour, form gas diffusion electrode;
(3) thermal treatment and hot pressing: the above-mentioned gas diffusion electrode for preparing is warming up to 240 ℃ of following thermal treatments made the charing of being heated of diffusion layer and the gelatin in the Catalytic Layer of gas diffusion electrode decompose pore-creating in 1 hour under 15 ℃ of/minute heating rate conditions; At last that electrode is hot-forming down at 360 ℃; Air cooling is to room temperature then, and the electrode average pore radius that obtains is at 23nm.
Embodiment 3:
Add gelatin and prepare process, wherein gelatin and carbon black mass ratio is 3% in the electrode component:
(1) preparation of diffusion layer: the Triton aqueous solution, the aqueous gelatin solution of 3mL massfraction 2%, 20mL Virahol, the hydrophobic carbon black of 2g that in beaker, add 20mL mass concentration 4% successively; Ultra-sonic dispersion mixes the three; The PTFE emulsion that adds 2mL 60% then; Shear to disperse 0.5h with refiner, form uniform slurry with cell pulverization machine ultra-sonic dispersion 10min again, the gained slurry is coated on the nickel foam to cold pressing after drying by the fire 0.5 hour down at 60～80 ℃ obtains diffusion layer;
(2) preparation of Catalytic Layer: in container, add earlier the Triton aqueous solution of 10mL 4%, the aqueous gelatin solution of 1.5mL massfraction 2% successively; The 20mL Virahol; Ultra-sonic dispersion mixes the three; Add 1g hydrophilic fumed silica, 0.8g silver/Pd/carbon catalyst then, the 0.4mL massfraction is that 60% PTFE emulsion is sheared with refiner and disperseed 0.5 hour, obtains uniform Catalytic Layer slurry with cell pulverization machine ultra-sonic dispersion again; Gained Catalytic Layer slurry is coated onto on step (1) diffusion layer forms Catalytic Layer, put into 60～80 ℃ of baking ovens then and carry out coldmoulding after dry 0.5 hour, form gas diffusion electrode;
(3) thermal treatment and hot pressing: made the charing of being heated of diffusion layer and the gelatin in the Catalytic Layer of gas diffusion electrode decompose pore-creating in 1 hour 300 ℃ of following thermal treatments the above-mentioned gas diffusion electrode for preparing; At last that electrode is hot-forming under 360 ℃, the electrode average pore radius that obtains is at 25nm.
The pressure mercury test result of the gas diffusion electrode for preparing among the embodiment 1-3, wherein average pore radius can be referring to Fig. 1 about 22-25nm.The gas diffusion electrode that the present invention prepares is the instant potential curve in 30% the NaOH solution at massfraction, and wherein cathodic current is 300mA/cm
2As can be seen from Figure 2 do not add cathodic polarization potential that the electrode pair of gelatin answers at-0.70V, add cathodic polarization potential that the electrode pair of 1% gelatin answers, explain and to play the effect that reduces cathode overpotential after adding gelatin at-0.59V.
Claims (3)
1. the gelatin pore forming method of a gas diffusion electrode is characterized in that, in the diffusion layer of gas diffusion electrode and Catalytic Layer, adds the gelatin pore-forming material, through the secondary pore-creating in the diffusion layer of electrode and Catalytic Layer of pore-creating process, specifically comprises the steps:
(1) preparation of diffusion layer: the aqueous gelatin solution that in container, adds earlier the Triton aqueous solution, Virahol, hydrophobic carbon black and the massfraction 1-2% of mass concentration 4% successively; Ultra-sonic dispersion mixes then; Add massfraction then and be 60% PTFE emulsion; Shear to disperse 0.5～1 hour with refiner, form uniform slurry with cell pulverization machine ultra-sonic dispersion again, the gained slurry is coated on the nickel foam to cold pressing after drying by the fire 0.5 hour down at 60～80 ℃ obtains diffusion layer; The Triton aqueous solution wherein: PTFE emulsion: aqueous gelatin solution: the volume ratio of Virahol is 20～45: 2～3: 1～5: 20～70; The volume of the Triton aqueous solution and hydrophobic sooty mass ratio are 20～45mL: 2～4g;
(2) preparation of Catalytic Layer: the aqueous gelatin solution that in container, adds earlier 4% the Triton aqueous solution, Virahol and massfraction 1-2% successively; Ultra-sonic dispersion mixes the three then; Add massfraction then and be 60% PTFE emulsion, hydrophilic fumed silica, silver/Pd/carbon catalyst; Shear dispersion 0.5 hour with refiner, use cell pulverization machine ultra-sonic dispersion again, ultra-sonic dispersion obtains uniform Catalytic Layer slurry; Gained Catalytic Layer slurry is coated onto on step (1) diffusion layer forms Catalytic Layer, put into 60～80 ℃ of baking ovens then and carry out coldmoulding after dry 0.5 hour, form gas diffusion electrode;
Wherein the volume ratio of the Triton aqueous solution, PTFE emulsion, aqueous gelatin solution and Virahol is 10～20: 0.4～0.6: 0.5～2: 20～25, and Triton aqueous solution volume: the quality of hydrophilic fumed silica: the quality of silver/Pd/carbon catalyst is 10～20mL: 1～1.5g: 0.8～1.5g;
(3) thermal treatment and hot pressing: made the charing of being heated of diffusion layer and the gelatin in the Catalytic Layer of gas diffusion electrode decompose pore-creating in 1 hour 200～300 ℃ of following thermal treatments the above-mentioned gas diffusion electrode for preparing, at last that electrode is hot-forming down at 360 ℃.
2. according to the method for claim 1, it is characterized in that the quality of the gelatin that in the electrode slurry process for preparation, is added in the step (2) is 1～3% with respect to the sooty quality optimization.
3. according to the method for claim 1, it is characterized in that gelatin pore-creating process is under 15 ℃ of/minute heating rate conditions in the step (3); Be warming up to 200～300 ℃, be incubated after 1 hour, the gelatin charing is decomposed; Electrode is hot-forming under 360 ℃, and air cooling is to room temperature then.
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| CN114717587A (en) * | 2022-05-12 | 2022-07-08 | 清华大学 | Diffusion layer, preparation method thereof and proton exchange membrane electrolytic cell |
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