CN109888303A - A kind of high catalytic activity Direct Carbon Fuel Cells anode material catalytic performance improved method - Google Patents
A kind of high catalytic activity Direct Carbon Fuel Cells anode material catalytic performance improved method Download PDFInfo
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Abstract
The present invention relates to a kind of high catalytic activity Direct Carbon Fuel Cells anode material catalytic performance improved methods, in particular to a kind of Direct Carbon Fuel Cells anode material and its anode pattern improved method with high stability and catalytic activity, it realizes the high output performance of Direct Carbon Fuel Cells, belongs to clean energy technology field.New material synthesized by the present invention (PrBa)0.95Fe2‑x‑ yCuxNbyO5+δ(PBFCN) it is used as the direct carbon solid oxide fuel cell anode material of mixed type, wherein the Cu content x numerical value is 0.1~0.4, and the Nb content y value is 0.1~0.4.Regulated and controled by anode pattern of the water droplet template to battery, improve catalytic performance, substantially increase the output performance of battery, under 800 DEG C of operating temperature, the single battery peak power output after improving anode pattern is up to 790mW/cm2, performance raising nearly 60%.
Description
Technical field
The present invention relates to a kind of high catalytic activity Direct Carbon Fuel Cells anode material catalytic performance improved methods, especially relate to
And a kind of Direct Carbon Fuel Cells anode material and its anode pattern improved method with high stability and catalytic activity, come real
The high output performance of existing Direct Carbon Fuel Cells, belongs to clean energy technology field.
Background technique
The fast development of world economy causes demand for energy to be continuously improved, country of the China as current high speed development,
Demand to the energy is equally growing day by day, and ring is both constantly polluted in the thermal power generation of the traditional energy utilization patterns such as coal in China
Border is also unable to satisfy current higher and higher energy demand, therefore needs to compel further to the efficient, clean utilization mode of the energy
It cuts.Direct carbon fuel cell of solid oxide (Solid Oxide Direct Carbon Fuel Cell, SO-DCFC) due to
The advantages that raw material sources of its carbon fuel are wide, generating efficiency is high, operation pollution is small, highly-safe be considered as it is a kind of have very much it is latent
Power replaces the new technology of traditional coal fuel firepower Land use systems.
Direct carbon fuel cell of solid oxide is commercialized at present there are still bigger difficulty, because it uses all solid state knot
Structure, thus limit it develop main problem be exactly solid carbon particle it is larger, size be much larger than gas molecule, lead to fuel
Seldom with the contact site of anode, electrolyte, electrochemical reaction active site quantity is extremely limited, causes direct carbon fuel electricity
The output power in pond is generally relatively low.In existing solution, increase anode and solid carbon including using melting Sb anode
Contact area increases reactivity region, and to improve battery performance, but the corrosivity of molten metal Sb is stronger, and chemistry
Stability is poor, and lower as the Direct Carbon Fuel Cells open-circuit voltage of anode using Sb, Constant current output stability is poor.And it is other
The method such as method of electrostatic spinning, infusion process etc. for improving anode pattern improves although the anode pattern of battery has certain optimization
The output performance of battery, but be still limited by the partial size of solid carbon fuel used, can not effectively regulate and control anode surface pattern into
Row matching is to realize optimal output performance.
Existing patent of invention (103972526 B of publication number CN 107539142 A and publication number CN) proposes use
Liquid metal anode solves the problems, such as to contact deficiency between solid carbon fuel and solid-state anode, but uses liquid metal anode
Open-circuit voltage it is relatively low, cause the output power of battery lower, and long-time stability are poor, thereby increases and it is possible to make to electrolyte
At corrosion failure battery structure, therefore also shortcoming can effectively improve direct carbon fuel cell of solid oxide anode shape at present
Looks are come the method that improves output performance.
Summary of the invention
The purpose of the present invention is for direct carbon fuel cell of solid oxide Anodic to the catalytic activity of solid carbon compared with
Difference, solid carbon fuel grain diameter is larger, causes fuel and the contact site of anode, electrolyte seldom, electrochemical reaction activity
Bit number of points are extremely limited, caused by Direct Carbon Fuel Cells the universal relatively low problem of output power, a kind of high catalysis is provided
Active Direct Carbon Fuel Cells anode material catalytic performance improved method, this method is by improving anode pattern, Lai Gaishan anode
Contact situation with solid carbon to achieve the purpose that improve cell output, and will not influence the job stability of battery.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of high catalytic activity Direct Carbon Fuel Cells anode material catalytic performance improved method, the specific steps are as follows:
(1) liquid phase carrier of water droplet template is configured.
Styrene-isoprene-styrene triblock copolymer is dissolved in chloroform, being configured to concentration is 10~40mg/
The solution of ml, and being sealed in the place of being protected from light and saving is sufficiently spread out the strand of copolymer.
(2) PBFCN anode material is added in the solution of step (1) and is uniformly mixed, the PBFCN anode material adds
Dosage is 0.2~0.5g/ml, and electrode slurry is made；
(3) electrode slurry made from step (2) is added dropwise in LSGM (La0.9Sr0.1Ga0.8Mg0.2O3-δ) on electrolyte, dry
It is re-sintered after dry to get the improved Direct Carbon Fuel Cells anode of pattern is arrived.
PBFCN is used to prepare direct carbon fuel SOFC as anode material: with La0.9Sr0.1Ga0.8Mg0.2O3-δFor electrolysis
The anode of battery is made using PBFCN as anode material by pattern improved method for matter, and with commercialized
La0.6Sr0.4Co0.2Fe0.8O3(LSCF) it is used as cathode material, the yin of Direct Carbon Fuel Cells is made by way of silk-screen printing
Single battery is made in pole after sintering, using activated carbon and carbonate mixture as fuel, and be passed through 10ml/min to anode-side and carry
Gas；The mass ratio of the activated carbon and carbonate is 1~4:1；The carbonate is one in lithium carbonate, potassium carbonate and sodium carbonate
Kind substance or a variety of mixtures.
The carrier gas is N2、Ar、He、CO2Or one of vapor.
The PBFCN anode material, specific molecular formula are (PrBa)0.95Fe2-x-yCuxNbyO5+δ, the Cu content x numerical value
It is 0.1~0.4, the Nb content y value is 0.1~0.4.
Any one or two kinds in the cathode layer and anode layer of the Direct Carbon Fuel Cells with a thickness of 10~30 μ
m；
The preparation method of the PBFCN anode material include: method of electrostatic spinning, solid phase method, combustion method, sol-gel method,
Hydro-thermal method or solvent-thermal method.
The synthetic method of the PBFCN anode is sol-gel method, specific steps are as follows: metal salt and citric acid are added
It is uniformly mixed in water；Water-bath heating stirring is to gel state at 60~90 DEG C, and drying obtains presoma at 150~250 DEG C, then
By presoma, 950~1100 DEG C of roasting 6h obtain PBFCN anode material under air atmosphere；
The molar ratio of the metal ion of the citric acid and metal salt is 1.5~2:1；The metal salt includes praseodymium salt, barium
Salt, molysite, mantoquita and niobium salt, wherein the molar ratio of metal ion be 0.95:0.95:1.2~1.8:0.1~0.4:0.1~
0.4。
The praseodymium salt includes praseodymium nitrate, acetic acid praseodymium, praseodymium oxalate.
The barium salt includes barium nitrate, barium acetate, barium oxalate.
The molysite includes ferric nitrate, ferric oxalate.
The mantoquita includes copper nitrate, copper acetate, cupric oxalate.
The niobium salt is niobium oxalate.
Beneficial effect
1, a kind of SO-DCFC anode material (PrBa) with high stability and catalytic activity disclosed by the invention0.95Fe2-x-yCuxNbyO5+δ(PBFCN), the Ca-Ti ore type under carbonate and reducing atmosphere with stable laminated structure has been obtained
Material.Regulated and controled by the doping of Cu, improves material to the absorption of CO, catalytic oxidation activity in anode chamber, improve battery
Output performance, peak power output can achieve 500mW/cm under 800 DEG C of operating temperature2, and can with steady operation 20h with
On.
2, the anode pattern for improving Direct Carbon Fuel Cells using water droplet template is prepared by regulating and controlling temperature humidity and is had
There is the SO-DCFC anode of different duct patterns, and regulates and controls the anode surface duct to match with solid carbon fuel partial size used and come
It is effective to increase chemical reactivity site, electrochemical reaction activity is improved, so as to greatly improve Direct Carbon Fuel Cells
Output power.Battery of the single battery compared to traditional silk screen print method preparation of anode is prepared using water droplet template,
Cell output significantly improves, and the maximum power output of battery is up to 790mW/cm at 800 DEG C2, performance raising nearly 60%.
Detailed description of the invention
Fig. 1 is the XRD diagram of the PBFCN anode material with high stability and catalytic activity；
Fig. 2 is that the TEM of the PBFCN anode material with high stability and catalytic activity schemes；
Fig. 3 is that the CO-TPD of 1 synthetic material of embodiment schemes；
Fig. 4 is the anode surface pattern of battery prepared by embodiment 1；
Fig. 5 is the discharge curve of battery prepared by embodiment 1；
Fig. 6 is the discharge curve of battery prepared by embodiment 2；
Fig. 7 is the discharge curve of battery prepared by embodiment 3；
Fig. 8 is the anode surface pattern of battery prepared by embodiment 3；
Fig. 9 is the discharge curve of battery prepared by embodiment 4；
Figure 10 is the anode surface pattern of battery prepared by embodiment 4.
Specific embodiment
Embodiment 1
A kind of direct carbon fuel SOFC anode material with high stability and catalytic activity, specific molecular formula are
(PrBa)0.95Fe1.4Cu0.4Nb0.2O5+δ。
Material preparation method is as follows:
Take six nitric hydrate praseodymium of 4.1326g, 2.4827g barium nitrate, 5.656g Fe(NO3)39H2O, the hydration of 0.9664g tri-
16.3909g citric acid is added in 500ml deionized water in copper nitrate, 1.0761g niobium oxalate, and 80 DEG C of heating water baths stir, directly
To rufous clear gel is formed, drying obtains brown presoma at 250 DEG C, after presoma is ground carefully under air atmosphere
950 DEG C of roasting 6h obtain (PrBa) with Perovskite Phase structure0.95Fe1.4Cu0.4Nb0.2O5+δAnode material, XRD analysis show
Prepared oxide corresponds to the base peak of perovskite, and the anode material of preparation is mixed with activated carbon, 800 under argon atmosphere
DEG C heat preservation 10h after, XRD analysis shows that material remains the stabilization of phase structure, as shown in Figure 1, TEM photo also indicates that material has
Laminated perovskite structure, as shown in Figure 2.
The anode material of synthesis is subjected to CO-TPD test, method particularly includes: the powder of 150mg synthesis is weighed, grinding is equal
After even, it is down to room temperature after 300 DEG C of pre-burning 30min under helium atmosphere, then be passed through 10%CO/Ar, by the absorption of two hours
Helium atmosphere is switched to after process, by adsorption instrument temperature programming to 1000 DEG C, and records CO desorption curve, as shown in figure 3,
800-1000 DEG C of desorption peaks illustrate that material has good CO adsorption activity at 700-800 DEG C of DCFC operating temperature.
Using the material of synthesis as anode material, the anode of Direct Carbon Fuel Cells is prepared by water droplet template, specific side
Method are as follows: (1) weigh 35mg styrene-isoprene-styrene triblock copolymer and the sample bottle for filling 1ml chloroformic solution is added
In, and seal and be placed in shady place storage 72h, make that copolymer is completely dissolved and strand is sufficiently spread out；(2) 0.25g system is weighed
Standby anode material is mixed into the solution that step (1) obtains, and ultrasonic 10min obtains finely dispersed anode slurry；(3) liquid relief is used
Rifle weighs the anode slurry that 20 microlitres of steps (2) obtain and is added dropwise in La0.9Sr0.1Ga0.8Mg0.2O3-δ(LSGM) on electrolyte, transfer
It is 50 DEG C to temperature, in the climatic chamber that relative humidity is 60%, drying 10min makes chloroform evaporating completely, obtains direct carbon combustion
Expect the anode layer of battery.The method brush La of silk-screen printing is used in the other side of electrolyte0.6Sr0.4Co0.2Fe0.8O3(LSCF) make
For cathode, monocell, anode table prepared by water droplet template after sintering is made in 1100 DEG C of sintering 2h of temperature programming in air
Face pore size is about 35-50 μm, with a thickness of 25 μm, by 400 mesh activated carbon (average grain diameter is 37 μm) and carbonate (lithium carbonate
It is 62:38 with the molar ratio of potassium carbonate) 4:1 in mass ratio mixes as in anode chamber, using 10ml/min Ar gas as carrier gas,
Using still air as oxidant, the operating temperature of battery is 800 DEG C, and battery peak power output density is 787mW/cm2, phase
60% is improved than improving preceding peak power output in pattern, the SEM figure of anode pattern such as attached drawing 4, the output power of battery is such as
Attached drawing 5.
Embodiment 2
A kind of direct carbon fuel SOFC anode material with high stability and catalytic activity, specific molecular formula are
(PrBa)0.95Fe1.7Cu0.1Nb0.2O5+δ。
It is prepared using solid phase method, the specific method is as follows:
Weigh 1.6173g praseodymium oxide (Pr6O11), 1.8747g barium carbonate, 1.36g di-iron trioxide, 0.0795g copper oxide,
0.2658g niobium pentaoxide is placed in ball mill with the speed ball milling of 400 revolution per seconds for 24 hours, by the powder after ball milling in air atmosphere
It encloses lower 1100 DEG C of roastings 10h and obtains (PrBa) with Perovskite Phase structure0.95Fe1.7Cu0.1Nb0.2O5+δAnode material.
Using the material of preparation as anode material, with La0.6Sr0.4Co0.2Fe0.8O3It (LSCF) is cathode material, with
La0.9Sr0.1Ga0.8Mg0.2O3-δ(LSGM) electrolyte two sides, every side brush are printed on by way of silk-screen printing as electrolyte
Twice, obtain single battery after being sintered under air, electrode layer with a thickness of 30 μm, by 400 mesh activated carbon (average grain diameters 37
μm) mixed with carbonate (lithium carbonate with the molar ratio of potassium carbonate be 62:38) 4:1 in mass ratio as in anode chamber, with 10ml/
Min Ar gas is as carrier gas, and using still air as oxidant, at 800 DEG C of operating temperature, peak power output is battery
278mW/cm2For as shown in Figure 6.
Embodiment 3
A kind of direct carbon fuel SOFC anode material with high stability and catalytic activity, specific molecular formula are
(PrBa)0.95Fe1.5Cu0.3Nb0.2O5+δ。
Material preparation method is as follows:
Take six nitric hydrate praseodymium of 4.1326g, 2.4827g barium nitrate, 6.06g Fe(NO3)39H2O, the hydration nitre of 0.7248g tri-
16.3909g citric acid is added in 500ml deionized water in sour copper, 1.0761g niobium oxalate, and 80 DEG C of heating water baths stir, until
Rufous clear gel is formed, drying obtains brown presoma at 250 DEG C, after presoma is ground carefully under air atmosphere
1000 DEG C of roasting 6h obtain (PrBa) with Perovskite Phase structure0.95Fe1.5Cu0.3Nb0.2O5+δAnode material.
Using the material of synthesis as anode material, the anode of Direct Carbon Fuel Cells is prepared by water droplet template, specific side
Method are as follows: (1) weigh 30mg styrene-isoprene-styrene triblock copolymer and the sample bottle for filling 1ml chloroformic solution is added
In, and seal and be placed in shady place storage 72h, make that copolymer is completely dissolved and strand is sufficiently spread out；(2) 0.2g preparation is weighed
Anode material be mixed into the solution that step (1) obtains, ultrasonic 10min obtains finely dispersed anode slurry；(3) liquid-transfering gun is used
The anode slurry that 20 microlitres of steps (2) obtain is weighed to be added dropwise in La0.9Sr0.1Ga0.8Mg0.2O3-δ(LSGM) it on electrolyte, is transferred to
Temperature is 35 DEG C, and in the climatic chamber that relative humidity is 80%, drying 10min makes chloroform evaporating completely, obtains direct carbon fuel
The anode layer of battery.The method brush La of silk-screen printing is used in the other side of electrolyte0.6Sr0.4Co0.2Fe0.8O3(LSCF) conduct
Cathode, monocell, anode surface prepared by water droplet template after sintering is made in 1100 DEG C of sintering 2h of temperature programming in air
Pore size is about 20-35 μm, with a thickness of 25 μm, by 400 mesh activated carbon (average grain diameter be 37 μm) and carbonate (lithium carbonate with
The molar ratio of potassium carbonate is 62:38) mixing of 4:1 in mass ratio is as in anode chamber, using 10ml/min Ar gas as carrier gas, with
Still air is 800 DEG C as oxidant, the operating temperature of battery, and battery peak power output density is 511mW/cm2, compare
Peak power output improves 35.5% before pattern improves, the output power of battery such as attached drawing 7, the anode pattern of monocell
SEM figure such as attached drawing 8.
Embodiment 4
A kind of direct carbon fuel SOFC anode material with high stability and catalytic activity, specific molecular formula are
(PrBa)0.95Fe1.6Cu0.2Nb0.2O5+δ。
It is specific the preparation method is as follows:
Take six nitric hydrate praseodymium of 4.1326g, 2.4827g barium nitrate, 6.464g Fe(NO3)39H2O, the hydration of 0.4832g tri-
16.3909g citric acid is added in 500ml deionized water in copper nitrate, 1.0761g niobium oxalate, and 80 DEG C of heating water baths stir, directly
To rufous clear gel is formed, drying obtains brown presoma at 250 DEG C, after presoma is ground carefully under air atmosphere
1000 DEG C of roasting 6h obtain (PrBa) with Perovskite Phase structure0.95Fe1.6Cu0.2Nb0.2O5+δAnode material.
Using the material of synthesis as anode material, the anode of Direct Carbon Fuel Cells is prepared by water droplet template, specific side
Method are as follows: (1) weigh 36mg styrene-isoprene-styrene triblock copolymer and the sample bottle for filling 1ml chloroformic solution is added
In, and seal and be placed in shady place storage 72h, make that copolymer is completely dissolved and strand is sufficiently spread out；(2) 0.25g system is weighed
Standby anode material is mixed into the solution that step (1) obtains, and ultrasonic 10min obtains finely dispersed anode slurry；(3) liquid relief is used
Rifle weighs the anode slurry that 20 microlitres of steps (2) obtain and is added dropwise in La0.9Sr0.1Ga0.8Mg0.2O3-δ(LSGM) on electrolyte, transfer
It is 35 DEG C to temperature, in the climatic chamber that relative humidity is 60%, drying 10min makes chloroform evaporating completely, obtains direct carbon combustion
Expect the anode layer of battery.The method brush La of silk-screen printing is used in the other side of electrolyte0.6Sr0.4Co0.2Fe0.8O3(LSCF) make
For cathode, monocell, anode table prepared by water droplet template after sintering is made in 1100 DEG C of sintering 2h of temperature programming in air
Face pore size is about 5-20 μm, with a thickness of 25 μm, by 400 mesh activated carbon (average grain diameter is 37 μm) and carbonate (lithium carbonate
It is 62:38 with the molar ratio of potassium carbonate) 4:1 in mass ratio mixes as in anode chamber, using 10ml/min Ar gas as carrier gas,
Using still air as oxidant, the operating temperature of battery is 800 DEG C, and battery peak power output density is 433mW/cm2, phase
Than before pattern improves peak power output improve 38.3%, the output power of battery such as attached drawing 9, the anode pattern of monocell
SEM figure such as attached drawing 10.
Above-described specific descriptions have carried out further specifically the purpose of invention, technical scheme and beneficial effects
It is bright, it should be understood that the above is only a specific embodiment of the present invention, the protection model being not intended to limit the present invention
It encloses, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection scope within.
Claims (9)
1. a kind of high catalytic activity Direct Carbon Fuel Cells anode material catalytic performance improved method, it is characterised in that: specific step
It is rapid as follows:
(1) liquid phase carrier of water droplet template is configured；
Styrene-isoprene-styrene triblock copolymer is dissolved in chloroform, being configured to concentration is 10~40mg/ml's
Solution, and being sealed in the place of being protected from light and saving is sufficiently spread out the strand of copolymer；
(2) PBFCN anode material is added in the solution of step (1) and is uniformly mixed, the additive amount of the PBFCN anode material
For 0.2~0.5g/ml, electrode slurry is made；
(3) electrode slurry made from step (2) is added dropwise in LSGM (La0.9Sr0.1Ga0.8Mg0.2O3-δ) on electrolyte, after drying
It re-sinters to get the improved Direct Carbon Fuel Cells anode catalyst layer of pattern is arrived.
2. preparing anode using method as described in claim 1 to assemble Direct Carbon Fuel Cells, it is characterised in that: use
PBFCN prepares direct carbon fuel SOFC anode as anode material, with La0.9Sr0.1Ga0.8Mg0.2O3-δFor electrolyte, and with quotient
The La of industry0.6Sr0.4Co0.2Fe0.8O3(LSCF) it is used as cathode material, cathode is made by way of silk-screen printing, after sintering
Single battery is made, using activated carbon and carbonate mixture as fuel, and is passed through 10ml/min carrier gas to anode-side；The work
Property carbon and carbonate mass ratio be 1~4:1.
3. battery as claimed in claim 2, it is characterised in that: the PBFCN anode material, specific molecular formula are (PrBa)0.95Fe2-x-yCuxNbyO5+δ, the Cu content x numerical value is 0.1~0.4, and the Nb content y value is 0.1~0.4.
4. battery as claimed in claim 2, it is characterised in that: the carbonate is one in lithium carbonate, potassium carbonate and sodium carbonate
Kind substance or a variety of mixtures；The carrier gas is N2、Ar、He、CO2Or one of vapor.
5. battery as claimed in claim 2, it is characterised in that: appointing in the cathode layer and anode layer of the Direct Carbon Fuel Cells
It anticipates one or two kinds of with a thickness of 10~30 μm.
6. battery as claimed in claim 2, it is characterised in that: the preparation method of the PBFCN anode material includes: electrostatic spinning
Method, solid phase method, combustion method, sol-gel method, hydro-thermal method or solvent-thermal method.
7. using the method for sol-gel method preparation PBFCN anode material as described in Claims 2 or 3, it is characterised in that: tool
Body step are as follows: be added to the water metal salt and citric acid uniformly mixed；Water-bath heating stirring is to gel state at 60~90 DEG C,
Drying obtains presoma at 150~250 DEG C, then 950~1100 DEG C of roasting 6h obtain PBFCN sun under air atmosphere by presoma
The molar ratio of the metal ion of pole material, the citric acid and metal salt is 1.5~2:1.
8. the method for claim 7, it is characterised in that: the metal salt be praseodymium salt, barium salt, molysite, mantoquita and niobium salt,
Wherein the molar ratio of metal ion is 0.95:0.95:1.2~1.8:0.1~0.4:0.1~0.4.
9. method according to claim 8, it is characterised in that: the praseodymium salt includes praseodymium nitrate, acetic acid praseodymium or praseodymium oxalate；It is described
Barium salt includes barium nitrate, barium acetate or barium oxalate；The molysite includes ferric nitrate or ferric oxalate；The mantoquita include copper nitrate,
Copper acetate or cupric oxalate；The niobium salt is niobium oxalate.
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| CN111330583A (en) * | 2020-03-03 | 2020-06-26 | 黑龙江大学 | Catalyst for electrochemical water decomposition reaction and preparation method thereof |
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