CN109192995A - A kind of method of ink-jet 3D printing manufacture solid oxide fuel cell electrode - Google Patents
A kind of method of ink-jet 3D printing manufacture solid oxide fuel cell electrode Download PDFInfo
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- CN109192995A CN109192995A CN201811038102.7A CN201811038102A CN109192995A CN 109192995 A CN109192995 A CN 109192995A CN 201811038102 A CN201811038102 A CN 201811038102A CN 109192995 A CN109192995 A CN 109192995A
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- ink
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- fuel cell
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
- H01M4/8832—Ink jet printing
-
- 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
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M2008/1293—Fuel cells with solid oxide electrolytes
-
- 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
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fuel Cell (AREA)
- Inert Electrodes (AREA)
Abstract
The invention discloses a kind of methods of ink-jet 3D printing manufacture solid oxide fuel cell electrode, which comprises mixed solution is made as the electrode ink of ink-jet 3D printing in electrode powder, surfactant, dispersing agent, volatilization inhibitor, acid-base modifier and solvent according to predetermined quality percentage；Print routine is formulated according to electrode structure to be prepared, and is input in ink-jet 3D printer；The print parameters of ink-jet 3D printer are set, comprising: impulse waveform, crest voltage, pulse frequency, substrate temperature, the printing number of plies and single layer interval；According to the print routine and print parameters of setting, using electrolyte layer well prepared in advance as printing substrate, ink-jet 3D printing is carried out using the electrode ink, electrode precursor is obtained, is placed in baking oven and is dried；Electrode precursor after drying and processing is sintered, solid oxide fuel cell electrode is obtained.
Description
Technical field
The present invention relates to solid oxide fuel cell technical fields more particularly to a kind of ink-jet 3D printing to manufacture solid oxygen
The method of compound fuel cell electrode.
Background technique
Solid oxide fuel cell is a kind of chemical energy being directly stored in fuel and oxidant under high temperature
Efficiently, be environmentally friendly converted to all solid state chemical generated device of electric energy, have high efficiency, pollution-free, structure of whole solid state with
And the advantages that fuel selection and mobile flexibility, there is broad prospect of application in fixed and mobile power source field.
Electrolyte is all solid state compact texture in solid oxide fuel cell, and anode and cathode then all has porous micro- knot
Structure, reasonable micro-structure are effective transmission, interfacial reaction and the diffusion realized electricity/ion in different materials and provide structure branch
The guarantee of support, so the manufacture means of electrode are also most important for the improvement of battery and electrode performance, it is in addition to material itself
In addition, another key factor solid oxide fuel cell reliability and durability regulated and controled.
However there are still some problems during its functionization needs to solve for solid oxide fuel cell, traditional system
The acquisitions such as Preparation Method such as silk-screen printing be uncontrollable, repeatable difference micro-structure, can not accurately control with balancing machine and
Chemical property；The thickness of single-layer electrodes is often thicker in traditional preparation method, is unfavorable for according to solid oxide fuel electricity
Regulation of the real work demand in pond to its different spatial electrode component.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
The technical problem to be solved in the present invention is that in view of the drawbacks of the prior art, the present invention provides a kind of ink-jet 3D and beats
The method for making solid oxide fuel cell electrode is printed, gives full play to ink-jet 3D printing technique to realize that electrode thin layer is controllably changed
The advantage of manufacture, the effective means as the innovation for solving the problems, such as solid-oxide fuel battery performance regulation.
The technical proposal for solving the technical problem of the invention is as follows:
A kind of method of ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the ink-jet 3D printing manufacture is solid
The method of oxide body fuel cell electrode includes:
According to predetermined quality percentage by electrode powder, surfactant, dispersing agent, volatilization inhibitor, acid-base modifier and molten
Electrode ink of the mixed solution as ink-jet 3D printing is made in agent；
Print routine is formulated according to the structure of solid oxide fuel cell electrode to be prepared, and is input to ink-jet 3D printer
In；
The print parameters of ink-jet 3D printer are set, and the print parameters include impulse waveform, crest voltage, pulse frequency, base
Plate temperature, the printing number of plies and single layer interval；
According to the print routine and print parameters of setting, using electrolyte layer well prepared in advance as printing substrate, using described
Electrode ink carries out ink-jet 3D printing in the printing substrate and obtains electrode precursor, is placed in baking oven and is dried；
Electrode precursor after drying and processing is sintered, solid oxide fuel cell electrode is obtained.
The method of the ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the electrode powder, table
Face activating agent, dispersing agent, volatilization inhibitor, acid-base modifier and solvent mass ratio be 10%:2%:0.5%:5%:10%:
72.5%。
The method of the described ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the electrode powder is
Fuel battery negative pole perovskite material, the fuel battery negative pole perovskite material include lanthanum-strontium-cobalt-oxygen body, lanthanum-strontium Conjugate ferrite
With one of lanthanum-strontium cobalt manganese oxysome or a variety of.
The method of the ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the surfactant
For the Aqueous Solutions of Polyethylene Glycol of 20% concentration.
The method of the ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the dispersing agent is three
Ethanol amine.
The method of the ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the volatilization inhibitor
For glycerine.
The method of the ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the acid-base modifier
The HCL aqueous solution for being 1mol/L for hydrogen ion concentration.
The method of the described ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the solvent be go from
Sub- water.
The method of the described ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein described according to setting
Print routine and print parameters, using electrolyte layer well prepared in advance as printing substrate, using the electrode ink described
Ink-jet 3D printing is carried out in printing substrate and obtains electrode precursor, is placed in be dried in baking oven and is specifically included:
The cerium oxide of solid-oxide fuel battery electrolyte material Gd2 O3 is subjected to compressing tablet process, quality 5g, tabletting carries
Lotus is 15MPa, and load time is 20 seconds, is then sintered 2 hours under the conditions of 1200 DEG C, obtains solid oxide fuel cell
Dense electrolyte layer；
Electrode ink is laid in the dense electrolyte by the planform continuous spray being pre-designed by ink-jet 3D printing
On layer, and the thickness of be layering printing to less than 100 μm, printing is completed to be placed on electric drying oven with forced convection, at 50 DEG C
Lower progress drying in 24 hours.
The method of the ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the sintering processes tool
Body includes:
1000 DEG C first are warming up to 5 DEG C/min of speed, then keeps the temperature 240 minutes, finally room is down in furnace cooling in air
Temperature.
The invention discloses a kind of method of ink-jet 3D printing manufacture solid oxide fuel cell electrode, the method packets
It includes: according to predetermined quality percentage by electrode powder, surfactant, dispersing agent, volatilization inhibitor, acid-base modifier and solvent
Electrode ink of the mixed solution as ink-jet 3D printing is made；According to the structure of solid oxide fuel cell electrode to be prepared
Print routine is formulated, and is input in ink-jet 3D printer；The print parameters of ink-jet 3D printer, the print parameters packet are set
Include impulse waveform, crest voltage, pulse frequency, substrate temperature, the printing number of plies and single layer interval；According to setting print routine and
Print parameters, using electrolyte layer well prepared in advance as printing substrate, using the electrode ink in the printing substrate
It carries out ink-jet 3D printing and obtains electrode precursor, be placed in baking oven and be dried；Electrode precursor after drying and processing is burnt
Knot processing, obtains solid oxide fuel cell electrode.The present invention gives full play to ink-jet 3D printing technique to realize that micro-structure can
The advantage of controlization manufacture solves the problems, such as solid-oxide fuel battery performance regulation, is solid oxide fuel cell electrode
Manufacture bring a kind of new scheme.
Detailed description of the invention
Fig. 1 is the stream of the preferred embodiment of the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode of the present invention
Cheng Tu；
Fig. 2 is the structural schematic diagram of solid oxide fuel cell electrode prepared by the present invention, in figure: 1-LSCF(lanthanum-strontium cobalt
Ferrite) cathode layer；The cerium oxide of 2-GDC(Gd2 O3) electrolyte layer；
Fig. 3 is the impulse waveform used in ink-jet 3D printing process of solid oxide fuel cell electrode prepared by the present invention
Figure；
Fig. 4 is the sintering curre figure that solid oxide fuel cell electrode prepared by the present invention uses during the sintering process.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer and more explicit, right as follows in conjunction with drawings and embodiments
The present invention is further described.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
It is of the invention in limiting.
The method that ink-jet 3D printing described in present pre-ferred embodiments manufactures solid oxide fuel cell electrode is such as schemed
Shown in 1, a kind of method of ink-jet 3D printing manufacture solid oxide fuel cell electrode, wherein the ink-jet 3D printing manufacture
The method of solid oxide fuel cell electrode the following steps are included:
Step S10, according to predetermined quality percentage by electrode powder, surfactant, dispersing agent, volatilization inhibitor, soda acid tune
Electrode ink of the mixed solution as ink-jet 3D printing is made in section agent and solvent.
Specifically, the matter of the electrode powder, surfactant, dispersing agent, volatilization inhibitor, acid-base modifier and solvent
Amount is than being 10%:2%:0.5%:5%:10%:72.5%.
Wherein, the electrode powder is fuel battery negative pole perovskite material, the fuel battery negative pole perovskite material
Including lanthanum-strontium-cobalt-oxygen body (LSC), lanthanum-strontium Conjugate ferrite (LSCF), lanthanum-strontium cobalt manganese oxysome (LSM) etc. and their composite powder
(i.e. one or more kinds of).Such as LSCF has high oxonium ion-electronics mixed conductivity and better oxygen catalytic activity, in
LSCF cathode catalysis performance can also have the substance of oxygen-ion conductive, such as GDC or SDC to mention by adding under low temperature
It is high；The surfactant is polyethylene glycol (PEG-4000) aqueous solution of 20% concentration (mass percentage concentration), is had good
Water solubility, and have good intermiscibility with many organic matter components, there is excellent lubricity, moisture retention, dispersibility, bonding
Agent, antistatic agent and softening agent etc.；The dispersing agent is triethanolamine (TEA), similar to other aminated compounds, due to nitrogen original
There are lone pair electrons on son, triethanolamine has alkalescent, can generate salt with inorganic acid or organic acid reaction；The evaporation retardation
Agent is glycerine, is commonly called as glycerol, and moisture can be absorbed from air, can also absorb hydrogen sulfide, hydrogen cyanide and sulfur dioxide；The acid
Alkali regulator is the HCL aqueous solution that hydrogen ion concentration is 1mol/L；The solvent is deionized water, and deionized water, which refers to, to be eliminated
In the pure water after ionic species impurity, rather than common water or organic solvent.
Step S20, print routine is formulated according to the structure of solid oxide fuel cell electrode to be prepared, and be input to
In ink-jet 3D printer.
Specifically, the print routine made is input in ink-jet 3D printer, to the electrode of printing in print routine
Laminate structure outer profile size requires, this outer profile is traditionally arranged to be circle, a diameter of D, by formulaInto
Row calculates, and unit is μm；P is resolution ratio (ink droplet number in single size), and unit is a；E is ink droplet spacing, and unit is μm.
Step S30, be arranged ink-jet 3D printer print parameters, the print parameters include impulse waveform, crest voltage,
Pulse frequency, substrate temperature, the printing number of plies and single layer interval.
Step S40, according to the print routine of setting and print parameters, using electrolyte layer well prepared in advance as printing base
Body is carried out ink-jet 3D printing in the printing substrate using the electrode ink and obtains electrode precursor, be placed in baking oven into
Row drying.
Specifically, tabletting is carried out to solid-oxide fuel battery electrolyte material GDC powder (cerium oxide of Gd2 O3)
Processing, powder quality 5g, tabletting load are 15MPa, and load time is 20 seconds, are then sintered 2 hours under the conditions of 1200 DEG C,
Obtain the dense electrolyte layer thin rounded flakes of solid oxide fuel cell；Then electrode ink is pressed by ink-jet 3D printing pre-
The planform continuous spray first designed is laid in the dense electrolyte layer, and carries out be layering printing to less than 100 μ
The thickness of m, printing are completed to be placed on electric drying oven with forced convection, and drying in 24 hours is carried out at 50 DEG C.It step S50, will be at drying
Electrode precursor after reason is sintered, and obtains solid oxide fuel cell electrode.
Specifically, the sintering schedule of sintering processes is as follows: being warming up to 1000 DEG C first with 5 DEG C/min of speed, then protects
Temperature 240 minutes, finally room temperature is down in furnace cooling in air.
To manufacture solid oxide fuel cell electrode by ink-jet 3D printing as cathode electricity using a specific embodiment below
(as shown in Figure 2) is illustrated for pole, specifically includes the following steps:
LSCF(lanthanum-strontium Conjugate ferrite is weighed respectively by the mass percent of 10:2.0:0.5:5.0:10:72.5) it is powder 50g, dense
Spending polyethylene glycol (PEG-4000) the aqueous solution 10g for 20%, triethanolamine (TEA) 2.5g, glycerine 25g, hydrogen ion concentration is
The HCL aqueous solution 50g and deionized water 362.5g of 1mol/L prepares the electrode ink that quality amounts to 500g；
Above-mentioned electrode ink is placed in grinding pot, and the zirconium oxide bead that gross mass is 1000g φ 0.1mm is added and carries out cathode slurry
The grinding of material is prepared, and grinding rate is 2700r/ minutes, is ground duration 8 hours；
Above-mentioned electrode ink is collected after grinding, and is placed it in stand-by in closed receiving flask；
Print routine is formulated according to the macrostructure of cathode of solid oxide fuel cell electrode, by dimension of picture calculation formula, the graphics resolution p being arranged in print routine is 600, ink droplet spacing e is 25 μm, and program is input to ink-jet
In 3D printer；
Electrode ink is put into printer ink cartridge, and print cartridge is fixed on ink-jet 3D printer corresponding position；
Ink-jet 3D printer print parameters are set, impulse waveform (referring to Fig. 3), 19.0 ~ 24.5mV of crest voltage section, arteries and veins are set
Rush that frequency is 2kHz, substrate temperature is 50 DEG C, the printing number of plies is to be divided between 15, single layer 30 seconds；
To the cerium oxide of solid-oxide fuel battery electrolyte material GDC(Gd2 O3) carry out compressing tablet process, quality 5g, pressure
Piece load is 15MPa, and load time is 20 seconds, is sintered 2 hours under the conditions of 1200 DEG C after the completion of tabletting, obtains soild oxide
Fuel cell electrolyte；
It is fixed on stamp pad using surface treated above-mentioned GDC electrolyte sheet as printing substrate, and in ink-jet 3D printing
Setting printing height and printing coordinate origin, start to print in machine；
It is taken out from ink-jet 3D printer after to electrode printing, is placed in electric drying oven with forced convection, at 50 DEG C into
Row drying in 24 hours；
The dry solid oxide fuel cell electrode precursor finished is taken out, is placed in high temperature box furnace and is sintered,
Described in sintering schedule (referring to fig. 4) it is as follows: be warming up to 1000 DEG C first with 5 DEG C/min of speed, then keep the temperature 240 minutes,
Finally room temperature is down in furnace cooling in air, and the solid oxide fuel cell electrode can be obtained.
The present invention also provides a kind of solid oxide fuel cell electrode, the solid oxide fuel cell electrode passes through
The method of ink-jet 3D printing manufacture solid oxide fuel cell electrode as described above is made.
In conclusion the present invention provides a kind of method of ink-jet 3D printing manufacture solid oxide fuel cell electrode, institute
The method of stating includes: according to predetermined quality percentage by electrode powder, surfactant, dispersing agent, volatilization inhibitor, acid-base accommodation
Electrode ink of the mixed solution as ink-jet 3D printing is made in agent and solvent；According to solid oxide fuel cell electricity to be prepared
The structure of pole formulates print routine, and is input in ink-jet 3D printer；The print parameters of ink-jet 3D printer are set, it is described to beat
Print parameter includes impulse waveform, crest voltage, pulse frequency, substrate temperature, the printing number of plies and single layer interval；According to beating for setting
Print program and print parameters are beaten using the electrode ink described using electrolyte layer well prepared in advance as printing substrate
Ink-jet 3D printing is carried out on print matrix and obtains electrode precursor, is placed in baking oven and is dried；Before the electrode after drying and processing
Body is sintered, and obtains solid oxide fuel cell electrode.The present invention gives full play to ink-jet 3D printing technique to realize
Micro-structure controllably changes the advantage of manufacture, solves the problems, such as solid-oxide fuel battery performance regulation, is solid oxide fuel
The manufacture of battery electrode brings a kind of new scheme.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of method of ink-jet 3D printing manufacture solid oxide fuel cell electrode, which is characterized in that the ink-jet 3D is beaten
Printing the method for making solid oxide fuel cell electrode includes:
According to predetermined quality percentage by electrode powder, surfactant, dispersing agent, volatilization inhibitor, acid-base modifier and molten
Electrode ink of the mixed solution as ink-jet 3D printing is made in agent；
Print routine is formulated according to the structure of solid oxide fuel cell electrode to be prepared, and is input to ink-jet 3D printer
In；
The print parameters of ink-jet 3D printer are set, and the print parameters include impulse waveform, crest voltage, pulse frequency, base
Plate temperature, the printing number of plies and single layer interval；
According to the print routine and print parameters of setting, using electrolyte layer well prepared in advance as printing substrate, using described
Electrode ink carries out ink-jet 3D printing in the printing substrate and obtains electrode precursor, is placed in baking oven and is dried；
Electrode precursor after drying and processing is sintered, solid oxide fuel cell electrode is obtained.
2. the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode according to claim 1, feature exist
In the mass ratio of, the electrode powder, surfactant, dispersing agent, volatilization inhibitor, acid-base modifier and solvent be 10%:
2%:0.5%:5%:10%:72.5%。
3. the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode according to claim 1, feature exist
In the electrode powder is fuel battery negative pole perovskite material, and the fuel battery negative pole perovskite material includes lanthanum-strontium cobalt
One of oxysome, lanthanum-strontium Conjugate ferrite and lanthanum-strontium cobalt manganese oxysome are a variety of.
4. the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode according to claim 1, feature exist
In the surfactant is the Aqueous Solutions of Polyethylene Glycol of 20% concentration.
5. the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode according to claim 1, feature exist
In the dispersing agent is triethanolamine.
6. the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode according to claim 1, feature exist
In the volatilization inhibitor is glycerine.
7. the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode according to claim 1, feature exist
In the acid-base modifier is the HCL aqueous solution that hydrogen ion concentration is 1mol/L.
8. the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode according to claim 1, feature exist
In the solvent is deionized water.
9. the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode according to claim 1, feature exist
In the print routine and print parameters according to setting uses institute using electrolyte layer well prepared in advance as printing substrate
State electrode ink and carry out ink-jet 3D printing in the printing substrate and obtain electrode precursor, be placed in baking oven be dried it is specific
Include:
The cerium oxide of solid-oxide fuel battery electrolyte material Gd2 O3 is subjected to compressing tablet process, quality 5g, tabletting carries
Lotus is 15MPa, and load time is 20 seconds, is then sintered 2 hours under the conditions of 1200 DEG C, obtains solid oxide fuel cell
Dense electrolyte layer；
Electrode ink is laid in the dense electrolyte by the planform continuous spray being pre-designed by ink-jet 3D printing
On layer, and the thickness of be layering printing to less than 100 μm, printing is completed to be placed on electric drying oven with forced convection, at 50 DEG C
Lower progress drying in 24 hours.
10. the method for ink-jet 3D printing manufacture solid oxide fuel cell electrode according to claim 1, feature exist
In the sintering processes specifically include:
1000 DEG C first are warming up to 5 DEG C/min of speed, then keeps the temperature 240 minutes, finally room is down in furnace cooling in air
Temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112048213A (en) * | 2019-06-05 | 2020-12-08 | 上海大学 | Ink-jet 3D printing material, ink and preparation method thereof |
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