CN108336384A - A kind of the niobium modification doping barium cerate electrolyte and preparation method of fuel cell - Google Patents
A kind of the niobium modification doping barium cerate electrolyte and preparation method of fuel cell Download PDFInfo
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- CN108336384A CN108336384A CN201810095436.1A CN201810095436A CN108336384A CN 108336384 A CN108336384 A CN 108336384A CN 201810095436 A CN201810095436 A CN 201810095436A CN 108336384 A CN108336384 A CN 108336384A
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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
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
- H01M2300/0071—Oxides
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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
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Abstract
A kind of the niobium modification doping barium cerate electrolyte and preparation method of fuel cell, stoichiometrically barium source, cerium source, doped metal salt, dispersant, bonding agent are mixed, ball milling is carried out using water as medium 1~12 hour, and drying is ground up, sieved to obtain porous doping barium cerate electrolyte precursor；Then addition niobium source uniformly mixes, and in 200~600 DEG C of pre-burnings 1~5 hour, then grinds 1~3 hour, obtains niobium doping barium cerate electrolyte precursor powder；Finally add sintering aid, it is ground to homogeneous mixture, then it fills this blend into mold and is pressed into sheet, pressure is 20~150MPa, keeps 150~300MPa static pressures 1~4 hour, is sintered 1~12 hour in 600~1000 DEG C of air atmospheres, then cooled to room temperature, originally water washing, it is dry, obtain BaCe0.8M0.2‑xNbxO3Perovskite type electrolyte film.The present invention passes through Nb3+Displacement doped metal salt to doping barium cerate be modified, prevent its at high temperature with water vapour and CO2React decomposition, improves the stability of electrolyte.
Description
Technical field
The invention belongs to technical field of ceramic material, and in particular to a kind of niobium modification doping barium cerate electrolysis of fuel cell
Matter and preparation method.
Background technology
ABO3The crystal structure of type perovskite is cubic system, in figure larger sphere represent the cation-bit on the positions A in
Cubical vertex, usually by the larger Ba of ionic radius2+、Sr2+And Ca2+Plasma occupies；Smaller sphere represent oxygen from
Son is in the face heart position in each face；Ion on the positions B is typically smaller by ionic radius in cubical body position
Ce4+Or Zr4+Plasma occupies, and is in the interstitial site of oxygen octahedra.
In the positions A of Ca-Ti ore type proton conductor electrolyte, doping is come the method for improving material electric property：A cations
Displacement or offset stoichiometric ratio.
American scholar Shima et al. has studied BaxCeO3±δAnd BaxCe0.85Gd0.15O3–δ(x=0.96,0.99,1.00,
1.01,1.04) material, the results showed that：The increase of Ba contents can improve conductivity and the material for having Gd to adulterate can be by mistake
The Ba solid solutions of amount enter in perovskite crystal structure.British scholar Barison et al. is with Ba1+xCe0.65Zr0.20Y0.15O3–δ(x=0,
0.05,0.10) it is research object, finds the content of A Ba to conductivity and in CO2In stability all have an impact；When x=
When 0.05, conductivity highest.
Number of patent application CN201110359568.9 discloses Yb and Y co-doped zirconium barium cerate multiphase structure proton conductors
Material and preparation method thereof, the Ba prepared by high temperature solid-state methodxCe0.50Yb0.40Y0.10O3–δ(x=0.95,0.97,1.00,
1.03,1.05) in system material, the content increase of Ba can improve conductivity and chemical stability.
Number of patent application CN201210003413.6 discloses Yt doped zirconium barium cerate _ inorganic salts multiphase structure proton conductor
Material and preparation method thereof is doped with K in the positions A of zirconium barium cerate2CO3, the results showed that in A doping K appropriate2CO3It can carry
The conductivity of high material.
But since barium cerate is easy and the vapor and CO in environment under the conditions of high temperature2It reacts, generates carbonic acid
The substances such as barium and barium hydroxide, chemical stability are poor.Therefore, it is carried out in the positions B of Ca-Ti ore type proton conductor electrolyte low
The doping of valence cation can largely improve the conductivity of material so that this electrolyte can be adapted for middle height
The application performance of the SOFCs of warm range.
Invention content
For the problem of hot conditions stability inferior difference existing for above-mentioned Ca-Ti ore type proton conductor electrolyte, the present invention carries
The niobium for going out a kind of fuel cell is modified doping barium cerate electrolyte and preparation method, the present invention are achieved through the following technical solutions
's.
A kind of niobium modification doping barium cerate electrolyte preparation method of fuel cell, which is characterized in that preparation process packet
Include following steps：
（1）Stoichiometrically barium source, cerium source, doped metal salt, dispersant, bonding agent are mixed, ball is carried out by medium of water
Then mill 1~12 hour is dried, is ground up, sieved to obtain porous doping barium cerate electrolyte precursor；Wherein barium source, cerium source, mix
Miscellaneous metal salt is by mol：Ba：Ce：M is 1:0.8:0.2-x, wherein x=0.1-0.15, M are doping metals salt ion；
（2）Niobium source is added in porous doping barium cerate electrolyte precursor, is uniformly mixed, it is small in 200~600 DEG C of pre-burnings 1~5
When, it then grinds 1~3 hour, obtains niobium doping barium cerate electrolyte precursor powder；Wherein the addition in niobium source according to mole
Count Ba：Ce：M：Nb is 1:0.8:0.2-x：X, wherein x=0.1-0.15；
（3）Sintering aid is added in niobium doping barium cerate electrolyte precursor powder, is ground to homogeneous mixture, it then will mixing
Object is packed into mold and is pressed into sheet, and pressure is 20~150MPa, 150~300MPa static pressures is kept 1~4 hour, 600~1000
It is sintered 1~12 hour in DEG C air atmosphere, then cooled to room temperature, originally water washing, dry, obtains BaCe0.8M0.2- xNbxO3Perovskite type electrolyte film.
The mass ratio in the barium source and cerium source, the gross mass of doped metal salt and dispersant, bonding agent is 1:（0.05~
0.2）:（0.05~0.2）.
The barium source is BaCO3；The cerium source is CeO2Or one in the non-sulfuric acid salt inorganic acid compound of cerium
Kind；The doped metal salt is yttrium salt, one kind of vanadic salts, scandium salts；The dispersant be triethanolamine, citric acid one
Kind；The bonding agent is one kind in methylcellulose, polyvinyl alcohol, acrylate, polyvinyl butyral.
The valence state in the niobium source, niobium is ﹢ trivalents.
The sintering aid is nickel protoxide, and dosage is the 3-5% of electrolyte precursor powder quality.
A kind of niobium for the fuel cell being prepared by the above method is modified doping barium cerate electrolyte.
A kind of niobium of fuel cell of the present invention is modified doping barium cerate electrolyte and preparation method, and prior art ratio,
Significant advantage is：
1, pass through Nb3+Displacement doped metal salt to doping barium cerate be modified, prevent its at high temperature with water vapour and CO2Hair
Raw reaction is decomposed, and the stability of electrolyte is improved.The atom of trace doping simultaneously can enhance the adsorption capacity of Hydrogen Proton.
2, the present invention is sintered by high-pressure static pressure, is made stably-doped fusion, is further strengthened the thermal stability of barium cerate.
3, preparation process of the present invention is brief, and technique is easy to control, and is suitble to stablize large-scale production.
Description of the drawings
Fig. 1 is perovskite type electrolyte prepared by embodiment 1,3, and the electrolyte that niobium is seldom adulterated with comparative example 1 exists respectively
5%H2O-H2Under obtain Arrhenius figure.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
（1）Stoichiometrically by barium source BaCO3, cerium source CeO2, yttrium salt, dispersant triethanolamine, bonding agent it is PVA mixed
It closes, carries out ball milling 1 hour using water as medium, then dry, be ground up, sieved to obtain porous doping barium cerate electrolyte precursor；
Wherein barium source, cerium source, doped metal salt be by mol：Ba：Ce：Y is 1:0.8:0.1；Total matter of the barium source and cerium source, yttrium salt
The mass ratio of amount and dispersant, bonding agent is 1:0.05:0.05；
（2）Niobium source is added in porous doping barium cerate electrolyte precursor, is uniformly mixed, in 300 DEG C of pre-burnings 1 hour, then
Grinding 1 hour obtains niobium doping barium cerate electrolyte precursor powder；Wherein the addition in niobium source is according to a mole meter Ba：Ce：Y：
Nb is 1:0.8:0.1：0.1；
（3）Sintering aid is added in niobium doping barium cerate electrolyte precursor powder, is ground to homogeneous mixture, it then will mixing
Object is packed into mold and is pressed into sheet, and pressure 20MPa keeps 150MPa static pressures 1 hour, and it is small that 1 is sintered in 600 DEG C of air atmospheres
When, then cooled to room temperature, originally water washing, drying obtains BaCe0.8Y0.1Nb0.1O3Perovskite type electrolyte film.Institute
The sintering aid stated is nickel protoxide, and dosage is the 3% of electrolyte precursor powder quality.
Embodiment 2
（1）Stoichiometrically by barium source BaCO3, cerium source CeO2, vanadic salts, dispersant triethanolamine, bonding agent it is PVA mixed
It closes, carries out ball milling 1 hour using water as medium, then dry, be ground up, sieved to obtain porous doping barium cerate electrolyte precursor；
Wherein barium source, cerium source, doped metal salt be by mol：Ba：Ce：V is 1:0.8:0.1；Total matter of the barium source and cerium source, yttrium salt
The mass ratio of amount and dispersant, bonding agent is 1:0.05:0.2；
（2）Niobium source is added in porous doping barium cerate electrolyte precursor, is uniformly mixed, in 300 DEG C of pre-burnings 1 hour, then
Grinding 1 hour obtains niobium doping barium cerate electrolyte precursor powder；Wherein the addition in niobium source is according to a mole meter Ba：Ce：V：
Nb is 1:0.8:0.1：0.1；
（3）Sintering aid is added in niobium doping barium cerate electrolyte precursor powder, is ground to homogeneous mixture, it then will mixing
Object is packed into mold and is pressed into sheet, and pressure 50MPa keeps 150MPa static pressures 1 hour, and it is small that 1 is sintered in 800 DEG C of air atmospheres
When, then cooled to room temperature, originally water washing, drying obtains BaCe0.8V0.1Nb0.1O3Perovskite type electrolyte film.Institute
The sintering aid stated is nickel protoxide, and dosage is the 4% of electrolyte precursor powder quality.
Embodiment 3
（1）Stoichiometrically by barium source BaCO3, cerium source CeO2, vanadic salts, dispersant triethanolamine, bonding agent it is acrylic ester mixed
It closes, carries out ball milling 2 hours using water as medium, then dry, be ground up, sieved to obtain porous doping barium cerate electrolyte precursor；
Wherein barium source, cerium source, doped metal salt be by mol：Ba：Ce：V is 1:0.8:0.05；The barium source and cerium source, yttrium salt it is total
The mass ratio of quality and dispersant, bonding agent is 1:0.1:0.2；
（2）Niobium source is added in porous doping barium cerate electrolyte precursor, is uniformly mixed, in 300 DEG C of pre-burnings 1 hour, then
Grinding 1 hour obtains niobium doping barium cerate electrolyte precursor powder；Wherein the addition in niobium source is according to a mole meter Ba：Ce：V：
Nb is 1:0.8:0.05：0.15；
（3）Sintering aid is added in niobium doping barium cerate electrolyte precursor powder, is ground to homogeneous mixture, it then will mixing
Object is packed into mold and is pressed into sheet, and pressure 50MPa keeps 150MPa static pressures 1 hour, and it is small that 1 is sintered in 800 DEG C of air atmospheres
When, then cooled to room temperature, originally water washing, drying obtains BaCe0.8V0.05Nb0.15O3Perovskite type electrolyte film.Institute
The sintering aid stated is nickel protoxide, and dosage is the 4% of electrolyte precursor powder quality.
Embodiment 4
1）Stoichiometrically by barium source BaCO3, cerium source CeO2, scandium salts, dispersant citric acid, bonding agent polyvinyl butyral
Mixing carries out ball milling 2 hours using water as medium, then dries, is ground up, sieved to obtain porous doping barium cerate electrolyte precursor
Body；Wherein barium source, cerium source, doping metals scandium salts be by mol：Ba：Ce：Sc is 1:0.8:0.05；The barium source and cerium source, yttrium
The mass ratio of the gross mass of salt and dispersant, bonding agent is 1:0.1:0.05；
（2）Niobium source is added in porous doping barium cerate electrolyte precursor, is uniformly mixed, in 300 DEG C of pre-burnings 1 hour, then
Grinding 1 hour obtains niobium doping barium cerate electrolyte precursor powder；Wherein the addition in niobium source is according to a mole meter Ba：Ce：
Sc：Nb is 1:0.8:0.05：0.15；
（3）Sintering aid is added in niobium doping barium cerate electrolyte precursor powder, is ground to homogeneous mixture, it then will mixing
Object is packed into mold and is pressed into sheet, and pressure 120MPa keeps 150MPa static pressures 3 hours, is sintered in `1000 DEG C of air atmosphere
1 hour, then cooled to room temperature, originally water washing, drying obtained BaCe0.8Sc0.05Nb0.15O3Perovskite type electrolyte
Film.The sintering aid is nickel protoxide, and dosage is the 5% of electrolyte precursor powder quality.
Comparative example 1
1）Stoichiometrically by barium source BaCO3, cerium source CeO2, scandium salts, dispersant citric acid, bonding agent polyvinyl butyral
Mixing carries out ball milling 2 hours using water as medium, then dries, is ground up, sieved to obtain porous doping barium cerate electrolyte precursor
Body；Wherein barium source, cerium source, doping metals scandium salts be by mol：Ba：Ce：Sc is 1:0.8:0.05；The barium source and cerium source, yttrium
The mass ratio of the gross mass of salt and dispersant, bonding agent is 1:0.1:0.05；
（2）Niobium source is added in porous doping barium cerate electrolyte precursor, is uniformly mixed, in 300 DEG C of pre-burnings 1 hour, then
Grinding 1 hour obtains niobium doping barium cerate electrolyte precursor powder；Wherein the addition in niobium source is according to a mole meter Ba：Ce：
Sc：Nb is 1:0.8:0.18：0.02；
（3）Sintering aid is added in niobium doping barium cerate electrolyte precursor powder, is ground to homogeneous mixture, it then will mixing
Object is packed into mold and is pressed into sheet, and pressure 120MPa keeps 150MPa static pressures 3 hours, is sintered in `1000 DEG C of air atmosphere
1 hour, then cooled to room temperature, originally water washing, drying obtained BaCe0.8Sc0.18Nb0.02O3Perovskite type electrolyte
Film.The sintering aid is nickel protoxide, and dosage is the 5% of electrolyte precursor powder quality.
The perovskite type electrolyte prepared by embodiment 1,3 seldom adulterates the electrolytic condenser of niobium with comparative example 1 compared with general
Electrolyte is respectively in 5%H2O-H2Arrhenius figure.It can be seen from the figure that perovskite type electrolyte is in air with 5%
H2O-H2In have preferable conducting power, when increase Nb3+Molar ratio, the conductivity of material can be improved, material is made to exist
Still there is preferable electric conductivity under higher temperature.Such as attached drawing 1.
Claims (6)
1. the niobium of fuel cell a kind of is modified doping barium cerate electrolyte preparation method, which is characterized in that preparation process includes
Following steps：
（1）Stoichiometrically barium source, cerium source, doped metal salt, dispersant, bonding agent are mixed, ball is carried out by medium of water
Then mill 1~12 hour is dried, is ground up, sieved to obtain porous doping barium cerate electrolyte precursor；Wherein barium source, cerium source, mix
Miscellaneous metal salt is by mol：Ba：Ce：M is 1:0.8:0.2-x, wherein x=0.1-0.15, M are doping metals salt ion；
（2）Niobium source is added in porous doping barium cerate electrolyte precursor, is uniformly mixed, it is small in 200~600 DEG C of pre-burnings 1~5
When, it then grinds 1~3 hour, obtains niobium doping barium cerate electrolyte precursor powder；Wherein the addition in niobium source according to mole
Count Ba：Ce：M：Nb is 1:0.8:0.2-x：X, wherein x=0.1-0.15；
（3）Sintering aid is added in niobium doping barium cerate electrolyte precursor powder, is ground to homogeneous mixture, it then will mixing
Object is packed into mold and is pressed into sheet, and pressure is 20~150MPa, 150~300MPa static pressures is kept 1~4 hour, 600~1000
It is sintered 1~12 hour in DEG C air atmosphere, then cooled to room temperature, originally water washing, dry, obtains BaCe0.8M0.2- xNbxO3Perovskite type electrolyte film.
2. a kind of niobium of fuel cell according to claim 1 is modified doping barium cerate electrolyte preparation method, special
Sign is that the mass ratio in barium source and cerium source, the gross mass of doped metal salt and dispersant, bonding agent is 1:（0.05~0.2）:
（0.05~0.2）.
3. a kind of niobium of fuel cell according to claim 1 is modified doping barium cerate electrolyte preparation method, special
Sign is that the barium source is BaCO3；The cerium source is CeO2Or middle one kind of the non-sulfuric acid salt inorganic acid compound of cerium；
The doped metal salt is yttrium salt, one kind of vanadic salts, scandium salts；The dispersant is one kind of triethanolamine, citric acid；Institute
The bonding agent stated is one kind in methylcellulose, polyvinyl alcohol, acrylate, polyvinyl butyral.
4. a kind of niobium of fuel cell according to claim 1 is modified doping barium cerate electrolyte preparation method, special
Sign is that the valence state in the niobium source, niobium is ﹢ trivalents.
5. a kind of niobium of fuel cell according to claim 1 is modified doping barium cerate electrolyte preparation method, special
Sign is that the sintering aid is nickel protoxide, and dosage is the 3-5% of electrolyte precursor powder quality.
6. a kind of niobium for fuel cell that any one of claim 1-5 the methods are prepared is modified doping barium cerate electrolysis
Matter.
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| CN201810095436.1A CN108336384A (en) | 2018-01-31 | 2018-01-31 | A kind of the niobium modification doping barium cerate electrolyte and preparation method of fuel cell |
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| CN201810095436.1A CN108336384A (en) | 2018-01-31 | 2018-01-31 | A kind of the niobium modification doping barium cerate electrolyte and preparation method of fuel cell |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112062567A (en) * | 2020-09-17 | 2020-12-11 | 中国科学院上海应用物理研究所 | Method for preparing zirconium-yttrium-doped barium cerate powder by using molten salt and powder obtained by method |
| WO2022245710A3 (en) * | 2021-05-17 | 2023-01-05 | Phillips 66 Company | Enhanced proton conduction and steam tolerance of a donor doped electrolyte for solid oxide electrolysis cells |
-
2018
- 2018-01-31 CN CN201810095436.1A patent/CN108336384A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112062567A (en) * | 2020-09-17 | 2020-12-11 | 中国科学院上海应用物理研究所 | Method for preparing zirconium-yttrium-doped barium cerate powder by using molten salt and powder obtained by method |
| WO2022245710A3 (en) * | 2021-05-17 | 2023-01-05 | Phillips 66 Company | Enhanced proton conduction and steam tolerance of a donor doped electrolyte for solid oxide electrolysis cells |
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